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METHOD FOR COATING TEXTILE MATERIALS

20240218588 ยท 2024-07-04

Assignee

Inventors

Cpc classification

International classification

Abstract

The invention relates to a method for coating a textile material, said method comprising the following steps: a) at least one cycle of impregnating the textile material with a sol-gel adhesion formulation, said sol-gel adhesion formulation being free of polycarboxylic acid; b) at least one cycle of drying the impregnated textile material obtained in step a); c) at least one cycle of impregnating the dried textile material obtained in step b) with an omniphobic or hydrophobic sol-gel formulation comprising sulphamic acid, said omniphobic or hydrophobic sol-gel formulation being different from the sol-gel adhesion formulation; d) at least one cycle of drying the impregnated textile material obtained in step c).

Claims

1-29. (canceled)

30. A process for coating a textile material, said process comprising the following steps: a) at least one cycle of impregnating the textile material with a sol-gel bonding formulation, said sol-gel bonding formulation being free of polycarboxylic acid; b) at least one cycle of drying the impregnated textile material obtained in step a); c) at least one cycle of impregnating the dried textile material obtained in step b) with an omniphobic or hydrophobic sol-gel formulation comprising sulfamic acid, said omniphobic or hydrophobic sol-gel formulation being different from the sol-gel bonding formulation; d) at least one cycle of drying the impregnated textile material obtained in step c).

31. The process as claimed in claim 30, wherein at least one drying cycle is followed by a step d) of maturing the material obtained in step d) by storage at room temperature under a humid atmosphere with a relative humidity of 50% for at least 16H to 18H.

32. The process as claimed in claim 30, comprising the following additional steps: e) washing the impregnated textile material obtained in step d) with a neutralizing aqueous solution. f) drying the material obtained in step e).

33. The process as claimed in claim 32, wherein the step of drying the material obtained in step e) is followed by a step f) of maturing the material obtained in step f) by storage at room temperature under a humid atmosphere with a relative humidity of 50% for at least 16H to 18H.

34. The process as claimed in claim 30, wherein each of the impregnation steps is independently performed by padding or spraying.

35. The process as claimed in claim 30, comprising at least two successive cycles, a) and b), of impregnating the textile material with a sol-gel bonding formulation, said sol-gel bonding formulation being free of polycarboxylic acid, and of drying the impregnated textile material.

36. The process as claimed in claim 30, wherein step a) comprises a squeezing step under pressure after the or each impregnation cycle and/or step c) comprises a squeezing step under pressure after the or each impregnation cycle.

37. The process as claimed in claim 30, wherein the sol-gel bonding formulation comprises at least two silylated precursors.

38. The process as claimed claim 30, wherein the sol-gel bonding formulation comprises an acid chosen from sulfamic acid, hydrochloric acid, sulfuric acid, nitric acid and para-toluenesulfonic acid.

39. The process as claimed in claim 30, wherein the sol-gel bonding formulation is free of zirconium alkoxide and/or sodium hypophosphite.

40. The process as claimed in claim 30, wherein the omniphobic sol-gel formulation comprises at least one silylated precursor, chosen from 1H,1H,2H,2H-perfluorodecyltriethoxysilane (17FTEOS), 1H,1H,2H,2H-perfluorooctyltriethoxysilane (13FTEOS), 1H,1H,2H,2H-perfluorooctyltrimethoxysilane (13FTMOS), 1H,1H,2H,2H-perfluorodecyltrimethoxysilane (17FTMOS), or a mixture of one or more of these precursors with tetraethoxysilane (TEOS).

41. The process as claimed in claim 30, wherein the hydrophobic sol-gel formulation comprises at least one silylated precursor chosen from hexadecyltriethoxysilane (HDTEOS), n-octadecyltriethoxysilane (ODTEOS), n-decyltriethoxysilane (DTEOS) and dodecyltriethoxysilane (DDTEOS), or a mixture of one or more of these precursors with tetraethoxysilane (TEOS).

42. The process as claimed in claim 30, wherein the sol-gel bonding, omniphobic and/or hydrophobic formulation is an aqueous formulation and optionally comprises one or more C1 to C4 aliphatic alcohols.

43. A sol-gel bonding formulation comprising at least two silylated precursors, a first precursor being chosen from tetramethoxysilane (TMOS), tetraethoxysilane (TEOS), and a second precursor chosen from (3-glycidyloxypropyl)trimethoxysilane (GPTMOS), (3-glycidyloxypropyl)triethoxysilane (GPTEOS) and aminopropyltriethoxysilane, optionally, the combination of TMOS/GPTMOS precursors being excluded, and comprising an acid chosen from sulfamic acid, hydrochloric acid, sulfuric acid, nitric acid and para-toluenesulfonic acid, said sol-gel formulation being free of polycarboxylic acid.

44. An omniphobic sol-gel formulation comprising at least one silylated precursor chosen from 1H,1H,2H,2H-perfluorodecyltriethoxysilane (17FTEOS), 1H,H,H,H-perfluorooctyltriethoxysilane (13FTEOS), 1H,1H,2H,2H-perfluorooctyltrimethoxysilane (13FTMOS) and 1H,1H,2H,2H-perfluorodecyltrimethoxysilane (17FTMOS), or a mixture of one or more of these precursors with tetraethoxysilane (TEOS), and comprising sulfamic acid.

45. \A hydrophobic sol-gel formulation comprising at least one silylated precursor chosen from hexadecyltriethoxysilane (HDTEOS), n-octadecyltriethoxysilane (ODTEOS), n-decyltriethoxysilane (DTEOS) and dodecyltriethoxysilane (DDTEOS), or a mixture of one or more of these precursors with tetraethoxysilane (TEOS), and comprising sulfamic acid.

46. An impregnated textile material comprising at least a first bonding layer obtained by application of a sol-gel bonding formulation as claimed in claim 43 and at least a second omniphobic or hydrophobic layer over the bonding layer.

47. An impregnated textile material obtained via the coating process as claimed in claim 30.

48. A personal protective equipment comprising the impregnated textile material as claimed in claim 46.

Description

BRIEF DESCRIPTION OF THE DRAWINGS

[0146] FIG. 1 shows a photograph of a laboratory scarf.

[0147] FIG. 2 shows a photo of a laboratory spray system placed in an extractor hood, seen in profile.

[0148] FIG. 3 shows an example of grading for oleophobicity tests according to the standard ISO14419. The attributed grades range from A to D for drop shape, with A=pass, well rounded drop, B=partial pass with round drop with partial darkening, C=fail, visible wicking effect or complete wetting, and D=fail, complete wetting. The oleophobicity index n of the coating is that of the alkane (n) for which the drop shape is rated A.

[0149] FIG. 4 shows drop shapes of water and alkanes (50 ?L) deposited on a freshly coated fabric according to the P(3).sub.F process. From left to right: water, hexadecane (index 3), dodecane (index 5), decane (index 6), octane (index 7).

[0150] FIG. 5 shows photos of the contact angles of drops of water and decane (10 ?L) on a fabric coated according to the P(15).sub.F process at new (0 w) and washed 30 times (30 w).

[0151] FIG. 6 shows an SEM image of untreated K5204 fabric (Kermel?/Lenzing FR? 50/50). At 500? magnification.

[0152] FIG. 7 shows an SEM image of the K5204 fabric (Kermel?/Lenzing FR? 50/50) shown in FIG. 6, coated according to the P(3).sub.F process, at 500? magnification.

[0153] FIG. 8 shows an SEM image of the K5204 fabric (Kermel?/Lenzing FR? 50/50) shown in FIG. 6, coated via the P(3).sub.F process, at 1000? magnification.

[0154] FIG. 9 shows an example of light transmission analysis of sol(6).sub.omniP with the Turbiscan lab apparatus at different temperatures (30? C., 35? C., 40? C.). When the sol is homogeneous and clear, the % transmission of the intensity of a light beam passing through the sample is 92?1% here. The loss in transmission over long time indicates either the presence of scattering particles or the demixing of the sol with a change in the refractive index of the liquid.

[0155] FIG. 10 shows the results of the tests of resistance of the omniphobic coating to strong acids and bases. The contact angles of water and n-decane on the surface of sample P(15).sub.F were measured before and after the sample had been soaked for 24 hours in acidic solutions (pH=0) and basic solutions (pH=12 and 14).

EXAMPLES

Chemical Products Used:

[0156] Tetramethoxysilane (CAS No.: 681-84-5) (TMOS, Acros Organics, 99%); [0157] Tetraethoxysilane (CAS No.: 78-10-4) (TEOS, Acros Organics, 98%); [0158] (3-Glycidyloxypropyl)trimethoxysilane (CAS No.: 2530-83-8) (GPTMOS, Sigma-Aldrich, >98%); [0159] (3-Glycidyloxypropyl)triethoxysilane (CAS No. 2602-34-8) (GPTEOS, Gelest); [0160] 1H,H,H,H-Perfluorooctyltriethoxysilane (CAS No.: 51851-37-7) (13FTEOS, Acros Organics, 98%); [0161] 1H,H,H,H-Perfluorodecyltriethoxysilane (CAS No.: 101947-16-4) (17FTEOS, Acros Organics, 97%); [0162] Hexadecyltriethoxysilane (CAS No.: 16415-13-7) (HDTEOS, Gelest, 95%) [0163] Hydrochloric acid (CAS No. 7647-01-0) (HCl, Merck 37%) [0164] Sulfamic acid (CAS No. 5329-14-6) (AcSm, Sigma-Aldrich, >99%) [0165] Sodium hydroxide (CAS No. 1310-73-2) (NaOH, Sigma-Aldrich, >99%) [0166] Ethanol (CAS No.: 64-17-5) (EtOH, Carlo Erba, HPLC-PLUS-Gradient); [0167] Isopropanol (CAS No.: 67-63-0) (iPrOH, Fisher, 99.9%); [0168] demineralized H.sub.2O

Textiles Used:

[0169] Different types of fabric were used to demonstrate the applicability of the omniphobic coating. These were [0170] Kermel?/Lenzing FR? 50/50 (kermel-viscose fabric). The mixed fabric has a mass per unit area of 260 g/m.sup.2 and an air permeability of 57.5 L/m.sup.2.Math.s (average value measured in accordance with the standard ISO 9237 at 100 Pa). Kermel? is a polyamide-imide with flame-retardant and thermostable properties. Lenzing FR? is a flame-retardant viscose (Modal manufacturing process) constituted of cellulose. Thus, the chemical nature of the two fibers is very different. [0171] 100% cotton with a mass per unit area of 180 g/m.sup.2. Cotton is constituted of cellulose and contains hydroxyl functions.

[0172] Tests were performed with A4 (21?30 cm.sup.2) fabric samples or with 100 m of fabric with a 30 cm width. The coatings were performed with various sol-gel formulations, either by padding with a laboratory padding machine, or by spraying with a motorized spraying system. The wet take-up, which represents the amount of sol taken up by the fabric before drying, is of the order of 43?3%.

[0173] The take-up rate is calculated by weighing the textile before and after treatment. The principle is to impregnate the fabric with a bath containing the desired product formulation, and to squeeze it out, i.e. to make the product penetrate and remove the excess bath from the fabric by exerting pressure between two elastomer-covered rollers. This allows the amount of bath deposited to be controlled, known as the squeezing or take-up rate. The material is treated throughout and on both sides, and maintains its textile appearance. The textile is weighed again after the squeezing step, but before the drying step. The ratio [(weight after deposition)?(weight before deposition)]/(weight before deposition) gives the take-up rate.

Example 1: Preparation of the Bonding Formulations (Sol.SUB.ACC.)

Sol(1).SUB.ACC

[0174] 9.1 mL of TMOS, 3.5 mL of GPTMOS and 87.5 mL of ultrapure water are successively added to a hermetically sealed glass flask. The mixture is stirred at room temperature (20-24? C.) at 500 rpm for 1H using an IKA Werke RO10 Power multiple stirrer plate. Sol(1).sub.ACC contains 12.5% v/v of silylated precursors with a TMOS/GPTMOS mole ratio of 4. Sol(1).sub.ACC has a stability of 6H.

Sol(2).SUB.ACC

[0175] 6.0 mL of TMOS, 6.0 mL of GPTMOS and 77.0 mL of ultrapure water are successively added to a hermetically sealed glass flask. The mixture is stirred at room temperature (20-24? C.) at 500 rpm for 1H using an IKA Werke RO10 Power multiple stirrer plate. Sol(2).sub.ACC contains 13.5% v/v of silylated precursors with a TMOS/GPTMOS mole ratio of 1.5. Sol(2).sub.ACC has a stability of 6H.

Sol(3).SUB.ACC

[0176] 6 mL of TMOS, 6 mL of GPTMOS and 77 mL of ultrapure water are successively added to a hermetically sealed glass flask. The mixture is stirred at room temperature (20-24? C.) at 500 rpm for 3 h using an IKA Werke RO10 Power multiple stirrer plate. Sol(3).sub.ACC contains 13.5% v/v of silylated precursors with a TMOS/GPTMOS mole ratio of 1.5. Sol(3).sub.ACC has a stability of 6H.

Sol(4).SUB.ACC

[0177] 6.0 mL of TMOS, 6.0 mL of GPTMOS and 77.0 mL of ultrapure water are successively added to a hermetically sealed glass flask. The mixture is stirred at room temperature (20-24? C.) at 500 rpm for 4H using an IKA Werke RO10 Power multiple stirrer plate. Sol(4).sub.ACC contains 13.5% v/v of silylated precursors with a TMOS/GPTMOS mole ratio of 1.5. Sol(4).sub.ACC has a stability of 6H.

Sol(5).SUB.ACC

[0178] 9.5 mL of TEOS, 8.1 mL of GPTEOS and 82.4 mL of aqueous sulfamic acid solution at 3.2 mmol/L are added successively to a hermetically sealed glass flask. The mixture is stirred at room temperature (20-24? C.) at 500 rpm for 24H using an IKA multiple stirrer plate. Sol(5).sub.ACC contains 17.6% v/v of silylated precursors with a TEOS/GPTEOS mole ratio of 1.5. Sol(5).sub.ACC has a stability time of more than 1 month.

Sol(6).SUB.ACC

[0179] 9.5 mL of TEOS, 8.1 mL of GPTEOS, 10 mL of ethanol and 72.4 mL of aqueous sulfamic acid solution at 3.6 mmol/L are successively added to a hermetically sealed glass flask. The mixture is stirred at room temperature (20-24? C.) at 500 rpm for 3H using an IKA multiple stirrer plate. Sol(6).sub.ACC contains 17.6% v/v of silylated precursors with a TEOS/GPTEOS mole ratio of 1.5 and 10% v/v of ethanol. Sol(6).sub.ACC has a stability time of more than 2 months.

Sol(7).SUB.ACC

[0180] 9.5 mL of TEOS, 8.1 of mL of GPTEOS, 20 mL of ethanol and 62.4 mL of aqueous sulfamic acid solution at 4.2 mmol/L are successively added to a hermetically sealed glass flask. The mixture is stirred at room temperature (20-24? C.) at 500 rpm for 3H using an IKA multiple stirrer plate. Sol(7).sub.ACC contains 17.6% v/v of silylated precursors with a TEOS/GPTEOS mole ratio of 1.5 and 20% v/v of ethanol. Sol(7).sub.ACC has a stability time of more than 1 month.

Sol(8).SUB.ACC

[0181] 9.5 mL of TEOS, 8.1 mL of GPTEOS, 30 mL of ethanol and 52.4 mL of aqueous sulfamic acid solution at 5.0 mmol/L are successively added to a hermetically sealed glass flask. The mixture is stirred at room temperature (20-24? C.) at 500 rpm for 3H using an IKA multiple stirrer plate. Sol(8).sub.ACC contains 17.6% v/v of silylated precursors with a TEOS/GPTEOS mole ratio of 1.5 and 30% v/v of ethanol. Sol(8).sub.ACC has a stability time of more than 1 month.

Example 2: Preparation of the Omniphobic Formulations (Sol.SUB.omniP.)

Sol(1).SUB.omniP

[0182] 12.0 mL of EtOH, 2.0 mL of 17FTEOS and 3.7 mL of aqueous HCl solution at 54.0 mmol/L are added successively to a hermetically sealed glass flask. The mixture is stirred at room temperature (20-24? C.) at 500 rpm for 1H using an IKA Werke RO10 Power multiple stirrer plate. Sol(1).sub.omniP contains 11.3% v/v of silylated precursor and 67.7% v/v of EtOH. Sol(1).sub.omniP has a stability of 3H.

Sol(2).SUB.omniP

[0183] 34.0 mL of EtOH, 10.4 mL of 17FTEOS and 14.7 mL of aqueous HCl solution at 70.0 mmol/L are added successively to a hermetically sealed glass flask. The mixture is stirred at room temperature (20-24? C.) at 500 rpm for 1H using an IKA Werke RO10 Power multiple stirrer plate. Sol(2).sub.omniP contains 17.2% v/v of silylated precursor and 59.1% v/v of EtOH. Sol(2).sub.omniP has a stability of 3H.

Sol(3).SUB.omniP

[0184] 34.0 mL of EtOH, 10.4 mL of 17FTEOS and 5.6 mL of aqueous HCl solution at 184.0 mmol/L are added successively to a hermetically sealed glass flask. The mixture is stirred at room temperature (20-24? C.) at 500 rpm for 1H using an IKA Werke RO10 Power multiple stirrer plate. Sol(3).sub.omniP contains 20.7% v/v of silylated precursor and 68.0% v/v of EtOH. Sol(3).sub.omniP has a stability of 5H.

Sol(4).SUB.omniP

[0185] 24.9 mL of isopropanol, 10.4 mL of 17FTEOS and 14 mL of aqueous HCl solution at 70.0 mmol/L are added successively to a hermetically sealed glass flask. The mixture is stirred at room temperature (20-24? C.) at 500 rpm for 1H using an IKA Werke RO10 Power multiple stirrer plate. Sol(4).sub.omniP contains 20.7% v/v of silylated precursor and 49.8% v/v of isopropanol. Sol(4).sub.omniP has a stability of 6H.

Sol(5).SUB.omniP

[0186] 34.0 mL of EtOH, 10.4 mL of 17FTEOS and 5.6 mL of aqueous AcSm solution at 184.0 mmol/L are added successively to a hermetically sealed glass flask. The mixture is stirred at room temperature (20-24? C.) at 500 rpm for 1H30 (or 3H or 5H) using an IKA Werke RO10 Power multiple stirrer plate. Sol(5).sub.omniP contains 20.7% v/v of silylated precursor and 68.0% v/v of EtOH. Sol(5).sub.omniP has a stability of 22H.

Sol(6).SUB.omniP

[0187] 34.0 mL of EtOH, 10.4 mL of 17FTEOS and 5.6 mL of aqueous AcSm solution at 93.0 mmol/L are added successively to a hermetically sealed glass flask. The mixture is stirred at room temperature (20-24? C.) at 500 rpm for 3 h using an IKA Werke RO10 Power multiple stirrer plate. Sol(6).sub.omniP contains 20.7% v/v of silylated precursor and 68% v/v of EtOH. Sol(6).sub.omniP has a stability of 27H.

Sol(7).SUB.omniP

[0188] 34.0 mL of EtOH, 10.4 mL of 17FTEOS and 5.6 mL of aqueous AcSm solution at 46.0 mmol/L are added successively to a hermetically sealed glass flask. The mixture is stirred at room temperature (20-24? C.) at 500 rpm for 3 h using an IKA Werke RO10 Power multiple stirrer plate. Sol(7).sub.omniP contains 20.7% v/v of silylated precursor and 68% v/v of EtOH. Sol(7).sub.omniP has a stability of 27H.

Sol(8).SUB.omniP

[0189] 34.0 mL of EtOH, 10.4 mL of 17FTEOS and 5.6 mL of aqueous AcSm solution at 23.0 mmol/L are added successively to a hermetically sealed glass flask. The mixture is stirred at room temperature (20-24? C.) at 500 rpm for 3 h using an IKA Werke RO10 Power multiple stirrer plate. Sol(8).sub.omniP contains 20.7% v/v of silylated precursor and 68% v/v of EtOH. Sol(8).sub.omniP has a stability of 48H.

Sol(9).SUB.omniP

[0190] 24.6 mL of EtOH, 30 mL of 17FTEOS and 4 mL of aqueous HCl solution at 0.75 mol/L are added successively to a hermetically sealed glass flask. The mixture is stirred at room temperature (20-24? C.) at 500 rpm for 1H using an IKA Werke RO10 Power multiple stirrer plate. Sol(9).sub.omniP contains 51.1% v/v of silylated precursor and 42.0% v/v of EtOH. Sol(9).sub.omniP has a stability of 2H30.

Sol(10).SUB.omniP

[0191] 15.0 mL of EtOH, 15.0 mL of 17FTEOS and 2.1 mL of aqueous HCl solution at 1.0 mol/L are added successively to a hermetically sealed glass flask. The mixture is stirred at room temperature (20-24? C.) at 500 rpm for 30 min using an IKA Werke RO10 Power multiple stirrer plate (mixture 1). Successively add 3.0 mL of EtOH, 4.0 mL of TEOS and 1.0 mL of water to a separate glass flask, and shake to homogenize (mixture 2). Add mixture 2 to mixture 1 and stir for 30 min using an IKA Werke RO10 Power multiple stirrer plate. Sol(10).sub.omniP contains 48% v/v of silylated precursors with a TEOS/17FTEOS mole ratio of 2.5 and 44.9% v/v of EtOH. Sol(10).sub.omniP has a stability of 2H30.

Sol(11).SUB.omniP

[0192] 10.4 mL of 17FTEOS and 39.6 mL of aqueous AcSm solution at 3.3 mmol/L are added successively to a hermetically sealed glass flask. The mixture is stirred at room temperature (20-24? C.) at 500 rpm for 4H using an IKA Werke RO10 Power multiple stirrer plate. Sol(11).sub.omniP contains 20.7% v/v of silylated precursor.

Sol(12).SUB.omniP

[0193] 34.0 mL of EtOH, 10.4 mL of 13FTEOS and 5.6 mL of aqueous AcSm solution at 23.0 mmol/L are added successively to a hermetically sealed glass flask. The mixture is stirred at room temperature (20-24? C.) at 500 rpm for 3 h using an IKA Werke RO10 Power multiple stirrer plate. Sol(14).sub.omniP contains 20.7% v/v of silylated precursor and 68% v/v of EtOH. Sol(14).sub.omniP has a stability of 89 h.

Sol(13).SUB.omniP

[0194] 29.8 mL of EtOH, 15.3 mL of 13FTEOS and 4.9 mL of aqueous AcSm solution at 26.5 mmol/L are added successively to a hermetically sealed glass flask. The mixture is stirred at room temperature (20-24? C.) at 500 rpm for 3 h using an IKA Werke RO10 Power multiple stirrer plate. Sol(15).sub.omniP contains 30.7% v/v of silylated precursor and 60% v/v of EtOH. Sol(15).sub.omniP has a stability of 78 h.

Example 3: Preparation of Hydrophobic Formulations (Sol.SUB.HYDRO.)

Sol(1).SUB.HYDRO

[0195] 38.8 mL of EtOH, 9.7 mL of HDTEOS and 1.6 mL of aqueous AcSm solution at 83.2 mmol/L are added successively to a hermetically sealed glass flask. The mixture is stirred at room temperature (20-24? C.) at 500 rpm for 3 h using an IKA Werke RO10 Power multiple stirrer plate. Sol(1).sub.HYDRO contains 19.4% v/v of silylated precursor and 77.4% v/v of EtOH. Sol(1).sub.HYDRO has a stability of greater than 4H.

Sol(2).SUB.HYDRO

[0196] 39.1 mL of EtOH, 8.4 mL of HDTEOS, 1.4 mL of TEOS and 1.1 mL of aqueous HCl solution at 117.1 mmol/L are added successively to a hermetically sealed glass flask. The mixture is stirred at room temperature (20-24? C.) at 500 rpm for 3 h using an IKA Werke RO10 Power multiple stirrer plate. Sol(2).sub.HYDRO contains 19.6% v/v of silylated precursor and 78.2% v/v of EtOH. Sol(2).sub.HYDRO has a stability of 4H.

Sol(3).SUB.HYDRO

[0197] 39.1 mL of EtOH, 8.4 mL of HDTEOS, 1.4 mL of TEOS and 1.1 mL of aqueous HCl solution at 117.1 mmol/L are added successively to a hermetically sealed glass flask. The mixture is stirred at room temperature)(20-24? C. at 500 rpm for 5H using an IKA Werke RO10 Power multiple stirrer plate. Sol(3).sub.HYDRO contains 19.6% v/v of silylated precursor and 78.2% v/v of EtOH. Sol(3).sub.HYDRO has a stability of 1 D.

Sol(4).SUB.HYDRO

[0198] 39.1 mL of EtOH, 6.6 mL of HDTEOS, 3.2 mL of TEOS and 1.1 mL of aqueous HCl solution at 117.1 mmol/L are added successively to a hermetically sealed glass flask. The mixture is stirred at room temperature (20-24? C.) at 500 rpm for 5H using an IKA Werke RO10 Power multiple stirrer plate. Sol(4).sub.HYDRO contains 19.6% v/v of silylated precursor and 78.2% v/v of EtOH. Sol(4).sub.HYDRO has a stability of 1 D.

Sol(5).SUB.HYDRO

[0199] 39.1 mL of EtOH, 6.6 mL of HDTEOS, 3.2 mL of TEOS and 1.1 mL of aqueous AcSm solution at 117.1 mmol/L are added successively to a hermetically sealed glass flask. The mixture is stirred at room temperature (20-24? C.) at 500 rpm for 5H using an IKA Werke RO10 Power multiple stirrer plate. Sol(5).sub.HYDRO contains 19.6% v/v of silylated precursor and 78.2% v/v of EtOH. Sol(5).sub.HYDRO has a stability of greater than 6 D.

Sol(6).SUB.HYDRO

[0200] 39.1 mL of EtOH, 4.9 mL of HDTEOS, 4.9 mL of TEOS and 1.1 mL of aqueous HCl solution at 117.1 mmol/L are added successively to a hermetically sealed glass flask. The mixture is stirred at room temperature (20-24? C.) at 500 rpm for 5H using an IKA Werke RO10 Power multiple stirrer plate. Sol(6).sub.HYDRO contains 19.6% v/v of silylated precursor and 78.2% v/v of EtOH. Sol(6).sub.HYDRO has a stability of greater than 6 D.

Sol(7).SUB.HYDRO

[0201] 39.1 mL of EtOH, 4.9 mL of HDTEOS, 4.9 mL of TEOS and 1.1 mL of aqueous AcSm solution at 117.1 mmol/L are added successively to a hermetically sealed glass flask. The mixture is stirred at room temperature (20-24? C.) at 500 rpm for 5H using an IKA Werke RO10 Power multiple stirrer plate. Sol(7).sub.HYDRO contains 19.6% v/v of silylated precursor and 78.2% v/v of EtOH. Sol(7).sub.HYDRO has a stability of greater than 6 D.

Example 4: Preparation of Fabrics Coated by Padding (FIG. 1) According to the Invention

P(1).SUB.F

[0202] Sol(1).sub.ACC is applied to the fabric by padding at a speed of 2 m/min. After squeezing, the fabric is dried for 2 min at 120? C. in an oven. Immediately afterwards, a second deposit of Sol(1).sub.ACC is applied by padding at the same speed, and the fabric is again dried for 2 min at 120? C. in an oven. The fabric is then kept for 18 hours in a desiccator at 50% relative humidity, at room temperature (20-24? C.) and atmospheric pressure. Sol(10).sub.omniP is then applied to the fabric by padding at a speed of 2 m/min. After squeezing, the fabric is dried for 2 min at 120? C. in an oven, then left to cool at room temperature (20-24? C.) and laboratory atmospheric pressure for 10-30 min, before undergoing the final padding/squeezing in a 0.065 mol/L sodium hydroxide solution at a speed of 2 m/min. The fabric is dried for 2 min at 120? C. in an oven, then kept for 16-18 hours in a desiccator at 50% relative humidity, at room temperature (20-24? C.) and atmospheric pressure, before being stored for the washing, hydrophobicity and oleophobicity tests.

P(2).SUB.F

[0203] Sol(1).sub.ACC is applied to the fabric by padding at a speed of 2 m/min. After squeezing, the fabric is dried for 2 min at 120? C. in an oven. Immediately afterwards, a second deposit of Sol(1).sub.ACC is applied by padding at the same speed, and the fabric is again dried for 2 min at 120? C. in an oven. The fabric is then kept for 18 hours in a desiccator at 50% relative humidity, at room temperature)(20-24? C. and atmospheric pressure. Sol(10).sub.omniP is then applied to the fabric by padding at a speed of 2 m/min. After squeezing, the fabric is dried for 40 min at 120? C. in an oven, then left to cool at room temperature (20-24? C.) and laboratory atmospheric pressure for 10-30 min, before undergoing the final padding/squeezing in a 0.065 mol/L sodium hydroxide solution at a speed of 2 m/min. The fabric is dried for 2 min at 120? C. in an oven, then kept for 16-18 hours in a desiccator at 50% relative humidity, at room temperature (20-24? C.) and atmospheric pressure, before being stored for the washing, hydrophobicity and oleophobicity tests.

P(3).SUB.F

[0204] Sol(1).sub.ACC is applied to the fabric by padding at a speed of 2 m/min. After squeezing, the fabric is dried for 2 min at 120? C. in an oven, then left to cool for 30 min to 1 hour in the open air, at room temperature (20-24? C.) and atmospheric pressure. Sol(9).sub.omniP is then applied to the fabric by padding at a speed of 2 m/min. After squeezing, the fabric is dried for 2 min at 120? C. in an oven, then left to cool at room temperature (20-24? C.) and laboratory atmospheric pressure for 10-30 min, before undergoing the final padding/squeezing in a 0.065 mol/L sodium hydroxide solution at a speed of 2 m/min. The fabric is dried for 2 min at 120? C. in an oven, then kept for 16-18 hours in a desiccator at 50% relative humidity, at room temperature (20-24? C.) and atmospheric pressure, before being stored for the washing, hydrophobicity and oleophobicity tests.

P(4).SUB.F

[0205] Sol(1).sub.ACC is applied to the fabric by padding at a speed of 2 m/min. After squeezing, the fabric is dried for 2 min at 120? C. in an oven. Immediately afterwards, a second deposit of Sol(1).sub.ACC is applied by padding at the same speed, and the fabric is again dried for 2 min at 120? C. in an oven. The fabric is then kept for 18 hours in a desiccator at 50% relative humidity, at room temperature (20-24? C.) and atmospheric pressure. Sol(1).sub.omniP is then applied to the fabric by padding at a speed of 2 m/min. After squeezing, the fabric is dried for 2 min at 120? C. in an oven, then left to cool at room temperature (20-24? C.) and laboratory atmospheric pressure for 10-30 min, before undergoing the final padding/squeezing in a 0.065 mol/L sodium hydroxide solution at a speed of 2 m/min. The fabric is dried for 2 min at 120? C. in an oven, then kept for 16-18 hours in a desiccator at 50% relative humidity, at room temperature (20-24? C.) and atmospheric pressure, before being stored for the washing, hydrophobicity and oleophobicity tests.

P(5).SUB.F

[0206] Sol(1).sub.ACC is applied to the fabric by padding at a speed of 2 m/min. After squeezing, the fabric is dried for 2 min at 120? C. in an oven. Immediately afterwards, a second deposit of Sol(1).sub.ACC is applied by padding at the same speed, and the fabric is again dried for 2 min at 120? C. in an oven. The fabric is then kept for 18 hours in a desiccator at 50% relative humidity, at room temperature (20-24? C.) and atmospheric pressure. Sol(9).sub.omniP is then applied to the fabric by padding at a speed of 2 m/min. After squeezing, the fabric is dried for 10 min at 120? C. in an oven, then left to cool at room temperature (20-24? C.) and laboratory atmospheric pressure for 10-30 min, before undergoing the final padding/squeezing in a 0.065 mol/L sodium hydroxide solution at a speed of 2 m/min. The fabric is dried for 2 min at 120? C. in an oven, then kept for 16-18 hours in a desiccator at 50% relative humidity, at room temperature (20-24? C.) and atmospheric pressure, before being stored for the washing, hydrophobicity and oleophobicity tests.

P(6).SUB.F

[0207] Sol(2).sub.ACC is applied to the fabric by padding at a speed of 2 m/min. After squeezing, the fabric is dried for 2 min at 120? C. in an oven, then left to cool for 30 min to 1 hour in the open air, at room temperature (20-24? C.) and atmospheric pressure. Sol(9).sub.omniP is then applied to the fabric by padding at a speed of 2 m/min. After squeezing, the fabric is dried for 10 min at 120? C. in an oven, then left to cool at room temperature (20-24? C.) and laboratory atmospheric pressure for 10-30 min, before undergoing the final padding/squeezing in a 0.065 mol/L sodium hydroxide solution at a speed of 2 m/min. The fabric is dried for 2 min at 120? C. in an oven, then kept for 16-18 hours in a desiccator at 50% relative humidity, at room temperature (20-24? C.) and atmospheric pressure, before being stored for the washing, hydrophobicity and oleophobicity tests.

P(7).SUB.F

[0208] Sol(2).sub.ACC is applied to the fabric by padding at a speed of 2 m/min. After squeezing, the fabric is dried for 2 min at 120? C. in an oven, then left to cool for 30 min to 1 hour in the open air, at room temperature (20-24? C.) and atmospheric pressure. Sol(3).sub.omniP is then applied to the fabric by padding at a speed of 2 m/min. After squeezing, the fabric is dried for 10 min at 120? C. in an oven, then left to cool at room temperature (20-24? C.) and laboratory atmospheric pressure for 10-30 min, before undergoing the final padding/squeezing in a 0.065 mol/L sodium hydroxide solution at a speed of 2 m/min. The fabric is dried for 2 min at 120? C. in an oven, then kept for 16-18 hours in a desiccator at 50% relative humidity, at room temperature (20-24? C.) and atmospheric pressure, before being stored for the washing, hydrophobicity and oleophobicity tests.

P(8).SUB.F

[0209] Sol(3).sub.ACC is applied to the fabric by padding at a speed of 2 m/min. After squeezing, the fabric is dried for 2 min at 120? C. in an oven, then left to cool for 30 min to 1 hour in the open air, at room temperature (20-24? C.) and atmospheric pressure. Sol(3).sub.omniP is then applied to the fabric by padding at a speed of 2 m/min. After squeezing, the fabric is dried for 10 min at 120? C. in an oven, then left to cool at room temperature (20-24? C.) and laboratory atmospheric pressure for 10-30 min, before undergoing the final padding/squeezing in a 0.065 mol/L sodium hydroxide solution at a speed of 2 m/min. The fabric is dried for 2 min at 120? C. in an oven, then kept for 16-18 hours in a desiccator at 50% relative humidity, at room temperature (20-24? C.) and atmospheric pressure, before being stored for the washing, hydrophobicity and oleophobicity tests.

P(9).SUB.F

[0210] Sol(3).sub.ACC is applied to the fabric by padding at a speed of 2 m/min. After squeezing, the fabric is dried for 2 min at 120? C. in an oven, then left to cool for 30 min to 1 hour in the open air, at room temperature (20-24? C.) and atmospheric pressure. Sol(3).sub.omniP is then applied to the fabric by padding at a speed of 2 m/min. After squeezing, the fabric is dried for 10 min at 120? C. in an oven, then left to cool at room temperature (20-24? C.) and laboratory atmospheric pressure for 10-30 min, before undergoing the final padding/squeezing in a 0.065 mol/L sodium hydroxide solution at a speed of 2 m/min. The fabric is dried for 2 min at 120? C. in an oven, then left to cool in the open air at room temperature (20-24? C.) and atmospheric pressure, before being stored for the washing, hydrophobicity and oleophobicity tests.

P(10).SUB.F

[0211] Sol(4).sub.ACC is applied to the fabric by padding at a speed of 2 m/min. After squeezing, the fabric is dried for 2 min at 120? C. in an oven, then left to cool for 30 min to 1 hour in the open air, at room temperature (20-24? C.) and atmospheric pressure. Sol(3).sub.omniP is then applied to the fabric by padding at a speed of 2 m/min. After squeezing, the fabric is dried for 10 min at 120? C. in an oven, then left to cool at room temperature (20-24? C.) and laboratory atmospheric pressure for 10-30 min, before undergoing the final padding/squeezing in a 0.065 mol/L sodium hydroxide solution at a speed of 2 m/min. The fabric is dried for 2 min at 120? C. in an oven, then kept for 16-18 hours in a desiccator at 50% relative humidity, at room temperature (20-24? C.) and atmospheric pressure, before being stored for the washing, hydrophobicity and oleophobicity tests.

P(11).SUB.F

[0212] Sol(2).sub.ACC is applied to the fabric by padding at a speed of 2 m/min. After squeezing, the fabric is dried for 2 min at 120? C. in an oven, then left to cool for 30 min to 1 hour in the open air, at room temperature (20-24? C.) and atmospheric pressure. Sol(2).sub.omniP is then applied to the fabric by padding at a speed of 2 m/min. After squeezing, the fabric is dried for 10 min at 120? C. in an oven, then left to cool at room temperature (20-24? C.) and laboratory atmospheric pressure for 10-30 min, before undergoing the final padding/squeezing in a 0.065 mol/L sodium hydroxide solution at a speed of 2 m/min. The fabric is dried for 2 min at 120? C. in an oven, then kept for 16-18 hours in a desiccator at 50% relative humidity, at room temperature (20-24? C.) and atmospheric pressure, before being stored for the washing, hydrophobicity and oleophobicity tests.

P(12).SUB.F

[0213] Sol(3).sub.ACC is applied to the fabric by padding at a speed of 2 m/min. After squeezing, the fabric is dried for 2 min at 120? C. in an oven, then left to cool for 30 min to 1 hour in the open air, at room temperature (20-24? C.) and atmospheric pressure. Sol(5).sub.omniP is then applied to the fabric by padding at a speed of 2 m/min. After squeezing, the fabric is dried for 10 min at 120? C. in an oven, then left to cool at room temperature (20-24? C.) and laboratory atmospheric pressure for 10-30 min, before undergoing the final padding/squeezing in a 0.065 mol/L sodium hydroxide solution at a speed of 2 m/min. The fabric is dried for 2 min at 120? C. in an oven, then kept for 16-18 hours in a desiccator at 50% relative humidity, at room temperature (20-24? C.) and atmospheric pressure, before being stored for the washing, hydrophobicity and oleophobicity tests.

P(13).SUB.F

[0214] Sol(6).sub.ACC is applied to the fabric by padding at a speed of 2 m/min. After squeezing, the fabric is dried for 2 min at 120? C. in an oven, then left to cool for 30 min to 1 hour in the open air, at room temperature (20-24? C.) and atmospheric pressure. Sol(3).sub.omniP is then applied to the fabric by padding at a speed of 2 m/min. After squeezing, the fabric is dried for 10 min at 120? C. in an oven, then left to cool at room temperature (20-24? C.) and laboratory atmospheric pressure for 10-30 min, before undergoing the final padding/squeezing in a 0.065 mol/L sodium hydroxide solution at a speed of 2 m/min. The fabric is dried for 2 min at 120? C. in an oven, then kept for 16-18 hours in a desiccator at 50% relative humidity, at room temperature (20-24? C.) and atmospheric pressure, before being stored for the washing, hydrophobicity and oleophobicity tests.

P(14).SUB.F

[0215] Sol(6).sub.ACC is applied to the fabric by padding at a speed of 2 m/min. After squeezing, the fabric is dried for 2 min at 120? C. in an oven, then left to cool for 30 min to 1 hour in the open air, at room temperature (20-24? C.) and atmospheric pressure. Sol(5).sub.omniP is then applied to the fabric by padding at a speed of 2 m/min. After squeezing, the fabric is dried for 10 min at 120? C. in an oven, then left to cool at room temperature (20-24? C.) and laboratory atmospheric pressure for 10-30 min, before undergoing the final padding/squeezing in a 0.065 mol/L sodium hydroxide solution at a speed of 2 m/min. The fabric is dried for 2 min at 120? C. in an oven, then kept for 16-18 hours in a desiccator at 50% relative humidity, at room temperature (20-24? C.) and atmospheric pressure, before being stored for the washing, hydrophobicity and oleophobicity tests.

P(15).SUB.F

[0216] Sol(6).sub.ACC is applied to the fabric by padding at a speed of 2 m/min. After squeezing, the fabric is dried for 2 min at 120? C. in an oven, then left to cool for 30 min to 1 hour in the open air, at room temperature (20-24? C.) and atmospheric pressure. Sol(8).sub.omniP is then applied to the fabric by padding at a speed of 2 m/min. After squeezing, the fabric is dried for 10 min at 120? C. in an oven, then left to cool at room temperature (20-24? C.) and laboratory atmospheric pressure for 10-30 min, before undergoing the final padding/squeezing in a 0.065 mol/L sodium hydroxide solution at a speed of 2 m/min. The fabric is dried for 2 min at 120? C. in an oven, then kept for 16-18 hours in a desiccator at 50% relative humidity, at room temperature (20-24? C.) and atmospheric pressure, before being stored for the washing, hydrophobicity and oleophobicity tests.

P(16).SUB.F

[0217] Sol(6).sub.ACC is applied to the fabric by padding at a speed of 2 m/min. After squeezing, the fabric is dried for 2 min at 120? C. in an oven, then left to cool for 30 min to 1 hour in the open air, at room temperature (20-24? C.) and atmospheric pressure. Sol(8).sub.omniP is then applied to the fabric by padding at a speed of 2 m/min. After squeezing, the fabric is dried for 10 min at 120? C. in an oven, then kept for 16-18 hours in a desiccator at 50% relative humidity, at room temperature (20-24? C.) and atmospheric pressure, before being stored for the washing, hydrophobicity and oleophobicity tests.

P(17).SUB.F

[0218] Sol(6).sub.ACC is applied to the fabric by padding at a speed of 2 m/min. After squeezing, the fabric is dried for 2 min at 120? C. in an oven, then left to cool for 30 min to 1 hour in the open air, at room temperature)(20-24? C. and atmospheric pressure. Sol(8).sub.omniP is then applied to the fabric by padding at a speed of 2 m/min. After squeezing, the fabric is dried for 5 min at 120? C. in an oven, then left to cool at room temperature (20-24? C.) and laboratory atmospheric pressure for 10-30 min, before undergoing the final padding/squeezing in a 0.065 mol/L sodium hydroxide solution at a speed of 2 m/min. The fabric is dried for 2 min at 120? C. in an oven, then kept for 16-18 hours in a desiccator at 50% relative humidity, at room temperature (20-24? C.) and atmospheric pressure, before being stored for the washing, hydrophobicity and oleophobicity tests.

P(18).SUB.F

[0219] Sol(6).sub.ACC is applied to the fabric by padding at a speed of 2 m/min. After squeezing, the fabric is dried for 2 min at 120? C. in an oven, then left to cool for 30 min to 1 hour in the open air, at room temperature (20-24? C.) and atmospheric pressure. Sol(8).sub.omniP is then applied to the fabric by padding at a speed of 2 m/min. After squeezing, the fabric is dried for 5 min at 120? C. in an oven, then kept for 16-18 hours in a desiccator at 50% relative humidity, at room temperature (20-24? C.) and atmospheric pressure, before being stored for the washing, hydrophobicity and oleophobicity tests.

P(19).SUB.F

[0220] Sol(6).sub.ACC is applied to the fabric by padding at a speed of 2 m/min. After squeezing, the fabric is dried for 2 min at 120? C. in an oven, then left to cool for 30 min to 1 hour in the open air, at room temperature (20-24? C.) and atmospheric pressure. Sol(8).sub.omniP is then applied to the fabric by padding at a speed of 2 m/min. After squeezing, the fabric is dried for 2 min at 120? C. in an oven, then left to cool at room temperature (20-24? C.) and laboratory atmospheric pressure for 10-30 min, before undergoing the final padding/squeezing in a 0.065 mol/L sodium hydroxide solution at a speed of 2 m/min. The fabric is dried for 2 min at 120? C. in an oven, then kept for 16-18 hours in a desiccator at 50% relative humidity, at room temperature (20-24? C.) and atmospheric pressure, before being stored for the washing, hydrophobicity and oleophobicity tests.

P(20).SUB.F

[0221] Sol(6).sub.ACC is applied to the fabric by padding at a speed of 2 m/min. After squeezing, the fabric is dried for 2 min at 150? C. in an oven, then left to cool for 30 min to 1 hour in the open air, at room temperature (20-24? C.) and atmospheric pressure. Sol(8).sub.omniP is then applied to the fabric by padding at a speed of 2 m/min. After squeezing, the fabric is dried for 2 min at 150? C. in an oven, then left to cool at room temperature (20-24? C.) and laboratory atmospheric pressure for 10-30 min, before undergoing the final padding/squeezing in a 0.065 mol/L sodium hydroxide solution at a speed of 2 m/min. The fabric is dried for 2 min at 150? C. in an oven, then kept for 16-18 hours in a desiccator at 50% relative humidity, at room temperature (20-24? C.) and atmospheric pressure, before being stored for the washing, hydrophobicity and oleophobicity tests.

P(21).SUB.F

[0222] Sol(6).sub.ACC is applied to the fabric by padding at a speed of 2 m/min. After squeezing, the fabric is dried for 2 min at 150? C. in an oven, then left to cool for 30 min to 1 hour in the open air, at room temperature (20-24? C.) and atmospheric pressure. Sol(8).sub.omniP is then applied to the fabric by padding at a speed of 2 m/min. After squeezing, the fabric is dried for 2 min at 150? C. in an oven, then kept for 16-18 hours in a desiccator at 50% relative humidity, at room temperature (20-24? C.) and atmospheric pressure, before being stored for the washing, hydrophobicity and oleophobicity tests.

P(22).SUB.F

[0223] Sol(6).sub.ACC is applied to the fabric by padding at a speed of 2 m/min. After squeezing, the fabric is dried for 2 min at 180? C. in an oven, then left to cool for 30 min to 1 hour in the open air, at room temperature (20-24? C.) and atmospheric pressure. Sol(8).sub.omniP is then applied to the fabric by padding at a speed of 2 m/min. After squeezing, the fabric is dried for 2 min at 180? C. in an oven, then left to cool at room temperature (20-24? C.) and laboratory atmospheric pressure for 10-30 min, before undergoing the final padding/squeezing in a 0.065 mol/L sodium hydroxide solution at a speed of 2 m/min. The fabric is dried for 2 min at 180? C. in an oven, then kept for 16-18 hours in a desiccator at 50% relative humidity, at room temperature (20-24? C.) and atmospheric pressure, before being stored for the washing, hydrophobicity and oleophobicity tests.

P(23).SUB.F

[0224] Sol(6).sub.ACC is applied to the fabric by padding at a speed of 2 m/min. After squeezing, the fabric is dried for 2 min at 180? C. in an oven, then left to cool for 30 min to 1 hour in the open air, at room temperature (20-24? C.) and atmospheric pressure. Sol(8).sub.omniP is then applied to the fabric by padding at a speed of 2 m/min. After squeezing, the fabric is dried for 2 min at 180? C. in an oven, then kept for 16-18 hours in a desiccator at 50% relative humidity, at room temperature (20-24? C.) and atmospheric pressure, before being stored for the washing, hydrophobicity and oleophobicity tests.

P(24).SUB.F

[0225] Sol(5).sub.ACC is applied to the fabric by padding at a speed of 2 m/min. After squeezing, the fabric is dried for 2 min at 120? C. in an oven, then left to cool for 30 min to 1 hour in the open air, at room temperature (20-24? C.) and atmospheric pressure. Sol(8).sub.omniP is then applied to the fabric by padding at a speed of 2 m/min. After squeezing, the fabric is dried for 10 min at 120? C. in an oven, then left to cool at room temperature (20-24? C.) and laboratory atmospheric pressure for 10-30 min, before undergoing the final padding/squeezing in a 0.065 mol/L sodium hydroxide solution at a speed of 2 m/min. The fabric is dried for 2 min at 120? C. in an oven, then kept for 16-18 hours in a desiccator at 50% relative humidity, at room temperature (20-24? C.) and atmospheric pressure, before being stored for the washing, hydrophobicity and oleophobicity tests.

P(25).SUB.F

[0226] Sol(6).sub.ACC is applied to the fabric by padding at a speed of 2 m/min. After squeezing, the fabric is dried for 2 min at 180? C. in an oven, then left to cool for 30 min to 1 hour in the open air, at room temperature (20-24? C.) and atmospheric pressure. Sol(1).sub.HYDRO is then applied to the fabric by padding at a speed of 2 m/min. After squeezing, the fabric is dried for 2 min at 180? C. in an oven, then kept for 16-18 hours in a desiccator at 50% relative humidity, at room temperature (20-24? C.) and atmospheric pressure, before being stored for the hydrophobicity tests.

P(26).SUB.F

[0227] Sol(6).sub.ACC is applied to the fabric by padding at a speed of 2 m/min. After squeezing, the fabric is dried for 2 min at 150? C. in an oven, then left to cool and to mature for 1 to 2 weeks in the open air, at room temperature (20-24? C.) and atmospheric pressure. Sol(12).sub.omniP is then applied to the fabric by padding at a speed of 2 m/min. After squeezing, the fabric is left to dry and to mature in the open air, at room temperature (20-24? C.) and laboratory atmospheric pressure for two weeks, before being stored for the washing, hydrophobicity and oleophobicity tests.

P(27).SUB.F

[0228] Sol(6).sub.ACC is applied to the fabric by padding at a speed of 2 m/min. After squeezing, the fabric is left to dry and to mature for 1 week to 3 months in the open air, at room temperature (20-24? C.) and laboratory atmospheric pressure. Sol(12).sub.omniP is then applied to the fabric by padding at a speed of 2 m/min. After squeezing, the fabric is left to dry and to mature in the open air, at room temperature (20-24? C.) and laboratory atmospheric pressure for two weeks, before being stored for the washing, hydrophobicity and oleophobicity tests.

P(28)

[0229] Sol(6).sub.ACC is applied to the fabric by padding at a speed of 2 m/min. After squeezing, the fabric is left to dry and to mature for 1 week to 3 months in the open air, at room temperature (20-24? C.) and laboratory atmospheric pressure. Sol(13).sub.omniP is then applied to the fabric by padding at a speed of 2 m/min. After squeezing, the fabric is left to dry and to mature in the open air, at room temperature (20-24? C.) and laboratory atmospheric pressure for two weeks, before being stored for the washing, hydrophobicity and oleophobicity tests.

P(29).SUB.F

[0230] Sol(6).sub.ACC is applied to the fabric by padding at a speed of 2 m/min. After squeezing, the fabric is left to dry and to mature for 1 week to 3 months in the open air, at room temperature (20-24? C.) and laboratory atmospheric pressure. Sol(13).sub.omniP is then applied to the fabric by padding at a speed of 2 m/min. After squeezing, the fabric is left to dry and to mature at 40? C. in an oven for 4 days and then to mature for 3 days in the open air, at room temperature (20-24? C.) and laboratory atmospheric pressure, before being stored for the washing, hydrophobicity and oleophobicity tests.

P(30).SUB.F

[0231] Sol(6).sub.ACC is applied to the fabric by padding at a speed of 2 m/min. After squeezing, the fabric is left to dry for 1 day in the open air, at room temperature (20-24? C.) and laboratory atmospheric pressure. The fabric is then left to mature at 40? C. in an oven for 1 day and then for 5 days in the open air, at room temperature (20-24? C.) and laboratory atmospheric pressure. Sol(13).sub.omniP is then applied to the fabric by padding at a speed of 2 m/min. After squeezing, the fabric is left to dry and to mature at 40? C. in an oven for 4 days and then for 3 days in the open air, at room temperature (20-24? C.) and laboratory atmospheric pressure, before being stored for the washing, hydrophobicity and oleophobicity tests.

Example 5: Preparation of Fabrics Coated by Spraying (FIG. 2) According to the Invention

P(1).SUB.SP

[0232] Sol(3).sub.ACC is applied by spraying (pressure 4 bar) at a distance of 10 cm from the fabric, said fabric being moved at a speed of 6 m/min. The assembly is placed in a chamber under pumping to evacuate the ethanol vapors. After deposition, the fabric is dried for 2 min at 120? C. in an oven, then left to cool for 30 min to 1 h in the open air, at room temperature (20-24? C.) and atmospheric pressure. Sol(8).sub.omniP is then applied by spraying (pressure 4 bar) at a distance of 10 cm from the fabric, in two passes, the latter being moved at a speed of 9 m/min. After deposition, the fabric is compressed using a 3 kg roller and dried for 10 min at 120? C. in an oven, then left to cool at room temperature (20-24? C.) and laboratory atmospheric pressure for 10 to 30 min, before undergoing the final padding/squeezing in a 0.065 mol/L sodium hydroxide solution at a speed of 2 m/min. The fabric is dried for 2 min at 120? C. in an oven, then kept for 16-18 hours in a desiccator at 50% relative humidity, at room temperature (20-24? C.) and atmospheric pressure, before being stored for the washing, hydrophobicity and oleophobicity tests.

P(2).SUB.SP

[0233] Sol(3).sub.ACC is applied by spraying (pressure 4 bar) at a distance of 10 cm from the fabric, said fabric being moved at a speed of 9 m/min. The assembly is placed in a chamber under pumping to evacuate the ethanol vapors. After deposition, the fabric is dried for 2 min at 120? C. in an oven, then left to cool for 30 min to 1 h in the open air, at room temperature (20-24? C.) and atmospheric pressure. Sol(8).sub.omniP is then applied by spraying (pressure 4 bar) at a distance of 10 cm from the fabric, in two passes, the latter being moved at a speed of 9 m/min. After deposition, the fabric is compressed using a 3 kg roller and dried for 10 min at 120? C. in an oven, then left to cool at room temperature (20-24? C.) and laboratory atmospheric pressure for 10 to 30 min, before undergoing the final padding/squeezing in a 0.065 mol/L sodium hydroxide solution at a speed of 2 m/min. The fabric is dried for 2 min at 120? C. in an oven, then kept for 16 to 18 h in a desiccator at 50% relative humidity, at room temperature (20-24? C.) and atmospheric pressure, before being stored for the washing, hydrophobicity and oleophobicity tests.

P(3).SUB.SP

[0234] Sol(3).sub.ACC is applied by spraying (pressure 4 bar) at a distance of 10 cm from the fabric, said fabric being moved at a speed of 12 m/min. The assembly is placed in a chamber under pumping to evacuate the ethanol vapors. After deposition, the fabric is dried for 2 min at 120? C. in an oven, then left to cool for 30 min to 1 h in the open air, at room temperature (20-24? C.) and atmospheric pressure. Sol(8).sub.omniP is then applied by spraying (pressure 4 bar) at a distance of 10 cm from the fabric, in two passes, the latter being moved at a speed of 9 m/min. After deposition, the fabric is compressed using a 3 kg roller and dried for 10 min at 120? C. in an oven, then left to cool at room temperature (20-24? C.) and laboratory atmospheric pressure for 10 to 30 min, before undergoing the final padding/squeezing in a 0.065 mol/L sodium hydroxide solution at a speed of 2 m/min. The fabric is dried for 2 min at 120? C. in an oven, then kept for 16-18 hours in a desiccator at 50% relative humidity, at room temperature (20-24? C.) and atmospheric pressure, before being stored for the washing, hydrophobicity and oleophobicity tests.

P(4).SUB.SP

[0235] Sol(3).sub.ACC is applied by spraying (pressure 4 bar) at a distance of 10 cm from the fabric, said fabric being moved at a speed of 12 m/min. The assembly is placed in a chamber under pumping to evacuate the ethanol vapors. After deposition, the fabric is dried for 2 min at 120? C. in an oven, then left to cool for 30 min to 1 h in the open air, at room temperature (20-24? C.) and atmospheric pressure. Sol(8).sub.omniP is then applied by spraying (pressure 4 bar) at a distance of 20 cm from the fabric, in two passes, the latter being moved at a speed of 9 m/min. After deposition, the fabric is compressed using a 3 kg roller and dried for 10 min at 120? C. in an oven, then left to cool at room temperature (20-24? C.) and laboratory atmospheric pressure for 10 to 30 min, before undergoing the final padding/squeezing in a 0.065 mol/L sodium hydroxide solution at a speed of 2 m/min. The fabric is dried for 2 min at 120? C. in an oven, then kept for 16-18 hours in a desiccator at 50% relative humidity, at room temperature (20-24? C.) and atmospheric pressure, before being stored for the washing, hydrophobicity and oleophobicity tests.

P(5).SUB.SP

[0236] Sol(3).sub.ACC is applied by spraying (pressure 4 bar) at a distance of 10 cm from the fabric, said fabric being moved at a speed of 12 m/min. The assembly is placed in a chamber under pumping to evacuate the ethanol vapors. After deposition, the fabric is dried for 2 min at 120? C. in an oven, then left to cool for 30 min to 1 h in the open air, at room temperature (20-24? C.) and atmospheric pressure. Sol(8).sub.omniP is then applied by spraying (pressure 4 bar) at a distance of 10 cm from the fabric, in two passes, the latter being moved at a speed of 9 m/min. After deposition, the fabric is compressed using a 3 kg roller and dried for 10 min at 120? C. in an oven, then left to cool at room temperature (20-24? C.) and laboratory atmospheric pressure for 10 to 30 min, before undergoing the final padding/squeezing in a 0.065 mol/L sodium hydroxide solution at a speed of 2 m/min. The fabric is dried for 2 min at 120? C. in an oven, then kept for 16-18 hours in a desiccator at 50% relative humidity, at room temperature (20-24? C.) and atmospheric pressure, before being stored for the washing, hydrophobicity and oleophobicity tests.

P(6).SUB.SP

[0237] Sol(6).sub.ACC is applied by spraying (pressure 4 bar) at a distance of 10 cm from the fabric, said fabric being moved at a speed of 9 m/min. The assembly is placed in a chamber under pumping to evacuate the ethanol vapors. After deposition, the fabric is dried for 2 min at 120? C. in an oven, then left to cool for 29 h in the open air, at room temperature (20-24? C.) and atmospheric pressure. Sol(11).sub.omniP is then applied by spraying (pressure 4 bar) at a distance of 10 cm from the fabric, in two passes, the latter being moved at a speed of 9 m/min. After deposition, the fabric is compressed using a 3 kg roller and dried for 10 min at 120? C. in an oven, then left to cool at room temperature (20-24? C.) and laboratory atmospheric pressure for 10 to 30 min, before undergoing the final padding/squeezing in a 0.065 mol/L sodium hydroxide solution at a speed of 2 m/min. The fabric is dried for 2 min at 120? C. in an oven, then kept for 16-18 hours in a desiccator at 50% relative humidity, at room temperature (20-24? C.) and atmospheric pressure, before being stored for the washing, hydrophobicity and oleophobicity tests.

Example 6: Tests of the Hydrophobic and Oleophobic Properties, Permeability and Resistance of Fabrics Prepared According to the Invention to Washing and to Strong Acids and Bases

[0238] The bonding of the sol-gel materials to the fibers is visualized by means of Scanning Electron Microscopy (SEM, ZEISS Ultra-55, GEMINI column) images, and is verified after the washes with hydrophobicity and oleophobicity tests.

[0239] The washing tests (1, 5, 10, 15, 20, 25, 30, 40, 50, 60, 70, and 80 washes) are performed in accordance with the standard ISO 6330. The various fabrics undergo a 2-hour wash cycle in a horizontal-axis, front-loading machine. Washing is performed at 60? C., in the presence of 77% ECE detergent (reference detergent A No. 3), 20% sodium perborate tetrahydrate, 3% tetraacetylethylenediamine (TAED). Spin-drying is performed at 1200 rpm. The fabrics are tumble-dried at 95? C. for 45 min after each wash.

[0240] Tests of the resistance of the omniphobic coating to strong acids and bases are performed by immersing the fabric in solutions of strong acid (HCl) or of strong base (NaOH). The contact angles of water and n-decane on the surface of sample P(15).sub.F were measured before and after the sample had been soaked for 24 hours in acidic solutions (pH=0) and basic solutions (pH=12 and 14). The results obtained, presented in FIG. 10, show very little variation in these contact angles, and also show preserved hydrophobicity and oleophobicity even after placing the textile in contact with solutions of strong acids and bases, demonstrating the high resistance of the textile thus coated to strong acids and bases. Such a coating on protective gowns will allow workers to be protected from splashes of strong acids or bases.

[0241] Hydrophobicity and oleophobicity tests were performed on coated fabrics (kermel-viscose fabric), when new, and after 1, 5, 10, 15, 20, 25, 30, 40, 50, 60, 70, and 80 washes. For the visual hydrophobicity test, 50 ?L drops (about 5 mm in diameter) of water are deposited using a micropipette on at least five different locations distributed over the surface of the fabric. The drops are observed for 30?2 s (minimum) at an angle of 45? C. The fabric is shaken to remove the water droplets. The test is successful when the reverse side of the fabric remains dry. For a more accurate measure of hydrophobicity, the contact angle of water on the coating is measured.

[0242] The contact angle is measured using an OCA 15EC goniometer (SCA 20). Ten 10 ?L drops of water are applied to the fabric using a needle (Hamilton 500 mL, HAMI91022) for each measurement. A coating is said to be hydrophobic when the contact angle of a drop of water is greater than 90 degrees.

[0243] For visual measurement of the oleophobicity index, 50 ?L drops of alkanes are applied using a micropipette to at least four different locations distributed over the surface of the fabric. The drops are observed for 30 s and their shape is rated according to the references of the standard ISO 14419. The grades attributed range from A to D for drop shape. A drop of n-index alkane is placed on the surface of a coated fabric. If the drop is well rounded (grade A), the test is successful and the coating is attributed the n-index. If the drop is rated B, the alkane is changed to a lower index n?1 for which the drop is rated A. Of the four drops deposited dispersed on a given coating, only one drop needs to have an index of n?1 for the coating to be rated n/(n?1). See the examples in Table 1. For a more precise measure of the oleophobicity, the contact angle of alkanes on the coating is measured.

[0244] The contact angle is measured using an OCA 15EC goniometer (SCA 20). Four to eight 10 ?L drops of an alkane are applied to the fabric using a needle (Hamilton 500 mL, HAMI91022) for each measurement. A coating is said to be oleophobic when the contact angle of a drop of alkane is greater than 90 degrees.

[0245] The results obtained are collated in Tables 1 and 2 below.

TABLE-US-00001 TABLE 1 Process Oleophobic index according to the number of washes Wash 0 1 5 10 15 20 25 30 40 50 60 70 80 Fabric = Kermel?/Lenzing FR? 50/50 (kermel-viscose fabric) P(1).sub.F 6 6/5 6/5 6/5 6/5 6/5 5 3 P(2).sub.F 6 6 6 6/5 6/5 5 5 5 P(3).sub.F 6 6 6/5 6/5 6/5 6/5 6/5 5/4 P(4).sub.F 6 5 5 5 5 5 5/4 5 P(5).sub.F 6 5 5 5 5 5 5 Het P(6).sub.F 6 6/5 6/5 5 5 5 5 5 P(7).sub.F 6/5 5 5 5 5 5 5 5/4 P(8).sub.F 6/5 6/5 6/5 6/5 6/5 6/5 6/5 6/5 P(9).sub.F 6 5 5 5 5 5 5/4 4/3 P(10).sub.F 5 5 5 5 5 5 5 5 P(11).sub.F 6/5 6/5 6/5 6/5 6/5 6/5 6/5 5 P(12).sub.F 5 5 5 5 6/5 6/5 P(13).sub.F 6 6 6 6 6 6 P(14).sub.F 6 6 6 6 6 6 P(15).sub.F 6 6 6 6 6 6 P(16).sub.F 6 6 6 6 6 6 P(17).sub.F 6 6 6 6 6 6 P(18).sub.F 6 6 6 6 6/5 6/5 P(19).sub.F 6 6 6 6 5 5 P(20).sub.F 6 6 6 6 6 6 P(21).sub.F 6 6 6 6 6 6 P(22).sub.F 6 6 6 6 6 6 P(23).sub.F 6 6 6 6 6 6 6 5 5 5/4 P(24).sub.F 6 6 6 6 6 6 6 6/5 6/5 6/5 Het P(1).sub.SP 6 6 6 6 6 6/5 P(2).sub.SP 6 6 6 6/5 6 6/5 P(3).sub.SP 6 6 6 5 5 5 P(4).sub.SP 6 6 6 6/5 6 6 6/5 6/5 6/5 4 P(5).sub.SP 6 6 6 6 6 6 6 6/5 6/5 <3 P(6).sub.SP 6 6 6/5 6/5 6/5 6/5 Cotton fabric P(13).sub.F 6 6 6 6 6 6 Het = Heterogeneous

TABLE-US-00002 TABLE 2 Process ?.sub.0 W water ?.sub.30 W water ?.sub.0 W decane ?.sub.30 W decane P.sub.v P.sub.e Fabric = Kermel?/Lenzing FR? 50/50 (kermel-viscose fabric) P(1).sub.F 150.0 110 54.7 44.5 P(2).sub.F 142.9 144.5 115.8 114.2 49.6 P(3).sub.F 143.6 126.2 118.2 113.3 P(4).sub.F 139.0 135.7 115.6 105.6 43.1 P(5).sub.F 140.5 na na na 39.9 P(6).sub.F 145.9 140.5 104.4 106.0 49.5 P(7).sub.F 148.1 140.7 126.6 113.9 44.4 P(8).sub.F 143.0 141.9 124.3 114.6 38.9 P(9).sub.F 143.5 141.5 115.4 115.8 44.8 P(10).sub.F 146.0 142.2 113.2 128.9 40.5 P(11).sub.F 146.9 140.0 123.3 114.7 44.5 P(12).sub.F 146.7 133.5 118.6 122.5 46.8 P(13).sub.F 146.0 135.1 93.9 116.5 52.0 P(14).sub.F 142.6 143.3 112.5 128.2 46.8 P(15).sub.F 145.4 141.5 129.7 122.8 49.8 P(16).sub.F 143.0 138.1 114.8 108.3 47.4 P(17).sub.F 145.5 139.1 110.4 114.8 46.0 P(18).sub.F 143.3 136.5 115.6 108.8 49.2 P(19).sub.F 143.9 136.6 119.0 102.4 51.5 P(20).sub.F 141.0 134.0 124.0 119.4 40.5 P(21).sub.F 146.3 135.7 120.4 110.3 38.1 P(22).sub.F 146.8 139.1 121.8 122.1 36.2 P(23).sub.F 147.4 129.9 119.0 115.1 43.3 P(24).sub.F 142.8 141.7 126.9 120.0 42.1 P(25).sub.F 141.3 P(1).sub.SP 147.7 133.8 116.7 105.2 51.0 P(2).sub.SP 146.3 137.3 108.8 125.2 52.3 P(3).sub.SP 145.6 137.9 114.8 123.7 53.0 P(4).sub.SP 144.8 132.4 122.2 104.2 49.8 P(5).sub.SP 135.0 109.9 51.2 P(6).sub.SP 147.1 138.4 130.0 116.6 44.9 Fabric = cotton P(13).sub.F 144.29 125.09 119.50 117.89 ?.sub.0 W = contact angle when the fabric is new, in degrees; ?.sub.30 W = contact angle after 30 washes; P.sub.v = permeability of untreated fabric, P.sub.e = permeability of coated fabric.

[0246] An example of visual analysis of hydrophobicity and oleophobicity with various alkanes is shown in FIG. 4. FIG. 5 shows an example of contact angle measurements with a coated fabric when new, and after having been washed 30 times.

[0247] Examples of Scanning Electron Microscope (SEM) analysis of untreated fabrics and of fabrics coated with sol-gel coating are shown in FIG. 6, FIG. 7 and FIG. 8. These images make it possible to observe the homogeneous sheathing of fibers with a coating according to the invention.