Fabric care composition comprising silicone materials

Abstract

The present invention relates to fabric care compositions comprising a silicone based material cured via a condensation cure chemistry, and at least one fabric care ingredient, in an acceptable medium. Also disclosed is a process to prepare the fabric care compositions and uses of said fabric care compositions.

Claims

1. A fabric care composition comprising: a silicone based material cured via a condensation cure chemistry; and at least one fabric care ingredient; wherein the silicone based material cured via a condensation cure chemistry is the reaction product of: (i) at least one condensation curable silyl terminated polymer having at least one hydroxyl functional group per molecule, and having a viscosity of 1,000 to 300,000 mPa s at 25° C. measured by using a Brookfield cone plate viscometer (RV DIII) using a cone plate; (ii) a cross-linker selected from silanes having at least 2 hydrolysable groups and/or silyl functional molecules having at least 2 silyl groups, each silyl group containing at least one hydrolysable group; and (iii) a condensation catalyst selected from the group of titanates or zirconates; wherein the molar ratio of hydroxyl groups to total hydrolysable groups is between 0.4:1 to 2:1 using a silane cross-linker (ii) or 0.2:1 to 10:1 using a silyl functional molecule cross-linker (ii); and wherein the molar ratio of condensation catalyst (iii) M-OR functions to the total hydroxyl groups is between 0.01:1 and 0.6:1, where M is titanium or zirconium, and R is an aliphatic hydrocarbon group.

2. The fabric care composition of claim 1, wherein the silicone based material cured via a condensation cure chemistry is in neat form, in diluted form, or in emulsion form.

3. The fabric care composition of claim 1, wherein the at least one fabric care ingredient is selected from surface active materials, surfactants, detergents emulsifiers, thickeners, water phase stabilizing agents, pH controlling agents, preservatives, biocides, proteins or amino-acids and their derivatives, pigments, colorants, silicone conditioning agents, cationic conditioning agents, non-ionic conditioning agents, hydrophobic conditioning agents, UV absorbers, sunscreen agents, dyes, fragrances, perfumes, antioxidants, soil release agents, oxidizing agents, reducing agents, propellant gases, dispersibility aids, inorganic salts, antibacterial agents, antifungal agents, bleaching agents, sequestering agents, enzymes, diluents, antifoam compounds, builders, abrasives, fabric softeners, optical brighteners, soil-suspending agents, dispersants, dye transfer inhibitors, dye sequestrants, color fixatives, anti-re-deposition agents, fatty alcohols, color care additives, ironing agents, suspending agents, and mixtures thereof.

4. The fabric care composition of claim 1, wherein the at least one fabric care ingredient is selected from a cationic conditioning agent, a non-ionic conditioning agent, a hydrophobic conditioning agent, and mixtures thereof.

5. A process for preparing an emulsion, the process comprising: I) forming a mixture comprising; A) 100 parts by weight of the silicone based material cured via a condensation cure chemistry of claims 1, and B) 0.1 to 50 parts by weight of a surfactant; and , and II) admixing a sufficient amount of water to the mixture from step I) to form an emulsion.

6. A process to prepare the fabric care composition of claim 1, the process comprising mixing the silicone based material cured via a condensation cure chemistry and the at least one fabric care ingredient.

7. A process of washing and/or conditioning fabric substrates and fibres, the process comprising applying the fabric care composition of claim 1 to the fabric substrates and fibres.

8. The process of claim 7, further comprising letting the fabric care composition stand on the fabric substrates and fibres.

9. The process of claim 8, further comprising rinsing the fabric substrates and fibres.

Description

EXAMPLES

(1) The following examples are included to demonstrate preferred embodiments of the invention. Unless otherwise indicated, all recipes are in mass parts, therefore the sum is not necessarily 100.

Examples of Silicone Based Gel Cured Via a Condensation Cure Chemistry (G)=Example Materials

(2) Unless stated otherwise, all experiments were made at ambient conditions, that is temperature of 23° C.±1° and approx. 30% relative humidity. All numbers relating to the condensation cure composition are mass parts.

(3) Typically 80-90 g of condensation cure silicone based material cured via a condensation cure chemistry are prepared using the following protocol: the linear OH-terminated polydimethyl siloxane(s) was mixed with the cross-linker (x-linker) and with the optional diluent, using a speed mixer DAC 150.1 FV (available from Hauschield, Germany) at 3000 RPM for 30s. The catalyst, typically tetrabutyl titanate (TNBT), was then added and the mixture was stirred again for 90 seconds at maximum speed using the same device. Thus obtained material was left in an open container at ambient conditions for 1 to 3 weeks to allow for full cure. Unless stated otherwise all compositions were crystal clear polymers or gels.

(4) Cure was characterized using a TA.XT Plus Texture Analyser, available from Texture Technologies and equipped with rounded-end plastic probe. The latter was approached to the surface of the cure material at given speed until reaching certain penetration depth. At maximum penetration (in this case 5 mm), one records the maximal positive force, hereafter abbreviated as F(+).The higher F(+) the harder the material. The probe is then retracted until it is fully detached from the material. During retraction, the maximum adhesion force is measured. The adhesion force is abbreviated hereafter as F(−). With the onset of cure, the F(+) starts to increase and reaches a plateau when fully cured. The cure is deemed completed when the time variation in F(+) is less than 15%. The lower the F(+) the more flowable the material. The integration of the F(−) curve produces the adhesion energy. The value is standardly calculated by the software of the instrument. The higher the absolute value the stronger the adhesion. Particularly interesting are materials which present the combination of F(+) below 10 g, F(−) higher than −10 g and adhesion energy—the domain −200 to −80. These materials are characterized with high stringiness and ability to form filaments; said filaments detach cleanly from the probe.

(5) For the purpose of this invention, “flowable” is defined as follows: the condensation cure silicone based material is prepared in a shallow aluminium dish (ca 5 cm in diameter, 1 cm depth). Upon full cure, the dish is held inclined at an angle of 90° C. with respect to its normal orientation approximately 15 cm above the lab balance, and the material is allowed to flow. The time (t(flow)) to pour (as measured by the balance) 1 g of cured material has been measured. When t(flow) is less that 3 minutes, the material is deemed flowable. Obviously more flowable materials are characterized by lower t(flow). Less flowable material are deemed useful in the scope of the present invention, as long as their handling allows for dispersion and miscibility with other ingredients of the fabric care composition.

(6) Following abbreviations are used in the tables below: Polymer type 1: α,ω-Dihydroxy polydimethyl siloxane with viscosity at 23° C. of 2,000 mPa.Math.s (viscosity measured using a Brookfield cone plate viscometer RV DIII using a cone plate CP-52 at 20 rpm), Mn of 22,000, SiOH content=2*100*1000/22000=9.09 mmol/100 g Polymer type 5: α,ω-Dihydroxy polydimethyl siloxane with viscosity at 23° C. of 13,500 mPa.Math.s (viscosity measured using a Brookfield cone plate viscometer RV DIII using a cone plate CP-52 at 5 rpm), Mn of 43,000, SiOH content=2*100*1000/43000=4.65 mmol/100 g Polymer type P: α,ω-Dihydroxy polydimethyl siloxane with viscosity at 23° C. of 50,000 mPa.Math.s (viscosity measured using a Brookfield cone plate viscometer RV DIII using a cone plate CP-52 at 0.55 rpm), Mn of 63,000, SiOH content=2*100*1000/63000=3.17 mmol/100 g TEOS: tetraethoxy silane X-linker E: W—B—W type polymer where W is (EtO).sub.3—Si-D-, B is [SiO.sub.2(CH.sub.3).sub.2].sub.800-900, D is C.sub.2H.sub.4, having a viscosity at 23° C. of 50,000 mPa.Math.s (viscosity measured using a Brookfield cone plate viscometer RV DIII using a cone plate CP-52 at 3 rpm), Mn of 66,000 TNBT=tetra n-butyl titanate, commercially available as Tyzor ® TNBT from Dorf Ketal

(7) Diluent (where used) were abbreviated as follows: 200 fluid 5 cSt: trimethyl end-capped polydimethyl siloxane with viscosity of 5 cSt at 23° C. commercially available from Dow Corning under the trade name Dow Corning ® 200 fluid 5 cSt (about 5 mPa.Math.s) 200 fluid 100 cSt: trimethyl end-capped polydimethyl siloxane with viscosity of 100 cSt at 23° C. commercially available from Dow Corning under the trade name Dow Corning ® 200 fluid 100 cSt (about 100 mPa.Math.s) 200 fluid 2 cst: trimethyl end-capped polydimethyl siloxane with viscosity of 2 cSt at 23° C. commercially available from Dow Corning under the trade name Dow Corning ® 200 fluid 2 sct . This material is volatile and when used as diluent the inventors have topped-up the material with the amount of evaporated diluent on a daily basis. Lytol: light mineral oil commercially available as Lytol™ from Sonneborn.

(8) Example Materials 1 to 4 are disclosed in Table 1.

(9) TABLE-US-00001 TABLE 1 Example Example Example Example Reactant material 1 material 2 material 3 material 4 polymer type 1 100.00 100.00 — — polymer type 5 — — 100.00 100.00 TEOS 1.00 1.00 0.51 0.51 TNBT 0.20 0.20 0.11 0.11 200 fluid* 5 cSt — 100.00 — 100.00 F(+)- after 3 521.7 13.0 533.4 2.6 weeks [g] F(−) after 3 −52.0 −5.4 −151.4 −2.6 weeks [g] t(flow) >5 min >5 min >5 min >5 min

(10) Example Materials 5 to 8 are disclosed in Table 2.

(11) TABLE-US-00002 TABLE 2 Example Example Example Example Reactant material 5 material 6 material 7 material 8 X-linker E 150.00 300.00 150.00 150.00 polymer type 1 — — 74.50 74.50 polymer type 5 146.00 146.00 — — TNBT 0.15 0.15 0.15 0.15 200 fluid* 5 cSt — 250.00 — 250.00 F(+)- after 3 964.7 113.4 1581.5 115.4 weeks [g] F(−) after 3 −21.5 −8.3 −33.7 −8.1 weeks [g] t(flow) >5 min >5 min >5 min >5 min

(12) Example Materials 9 to 14 are disclosed in Table 3.

(13) TABLE-US-00003 TABLE 3 Example Example Example Example Example Example Reactant material 9 material 10 material 11 material 12 material 13 material 14 X-linker E 10.00 5.00 20.00 10.00 30.00 15.00 polymer type 5 100.00 100.00 100.00 100.00 100.00 100.00 TNBT 0.10 0.10 0.20 0.20 0.25 0.25 200 fluid* 5 cSt — — 100.00 100.00 200.00 200.00 F(+)- after 3 weeks [g] 4.6 2.0 2.3 1.1 2.3 1.2 F(−) after 3 weeks [g] −3.6 −2.4 −2.5 −2.6 −5.1 −2.6 Adhesion energy after 86.9 0.1 167 0 3 weeks (AU) t(flow) 2 min 35 sec 25 sec >3 min

(14) Example Materials 15 to 17 are disclosed in Table 4.

(15) TABLE-US-00004 TABLE 4 Example Example Example Reactant material 15 material 16 material 17 X-linker E 10.00 20.00 30.00 polymer type P 200.00 200.00 200.00 TNBT 0.20 0.25 0.30 200 fluid* 5 cSt — 200.00 400.00 F(+)- after 3 7.7 1.2 1.2 weeks [g] F(−) after 3 −6.5 −2.6 −2.6 weeks [g] Adhesion energy 98 0.1 0.1 after 3 weeks (AU) t(flow) — — 4 sec

(16) Example Materials 18 to 23 are disclosed in Table 5.

(17) TABLE-US-00005 TABLE 5 Example Example Example Example Example Example Reactant material 18 material 19 material 20 material 21 material 22 material 23 X-linker E 50.00 20.00 100.00 40.00 150.00 60.00 polymer type 5 100.00 100.00 100.00 100.00 100.00 100.00 TNBT 0.11 0.11 0.20 0.20 0.25 0.25 200 fluid* 5 cSt — — 100.00 100.00 200.00 200.00 F(+)- after 3 weeks [g] 311.1 24.5 165.3 24.9 61.8 24.6 F(−) after 3 weeks [g] −38.6 −34.2 −10.5 −14.2 −6.9 −5.5 Adhesion energy after 67.8 27.3 14.0 71.3 12.2 14.6 3 weeks (AU)

(18) Example Materials 24 to 26 are disclosed in Table 6.

(19) TABLE-US-00006 TABLE 6 Example Example Example Reactant material 24 material 25 material 26 X-linker E 20.00 40.00 60.00 polymer type P 200.00 200.00 200.00 TNBT 0.20 0.25 0.35 200 fluid* 5 cSt — 200.00 400.00 F(+)- after 3 17.5 4.1 3.9 weeks [g] F(−) after 3 −15.3 −7.0 −5.8 weeks [g] Adhesion energy 718 218 60 after 3 weeks (AU)

(20) Example Materials 27 to 29 are disclosed in Table 7.

(21) TABLE-US-00007 TABLE 7 Example Example Example Reactant material 27 material 28 material 29 X-linker E 100.00 300.00 226.30 polymer type 5 100.00 100.00 100.00 TNBT 0.20 0.20 0.35 200 fluid* 5 cSt 200.00 200.00 300.00 F(+)- after 3 6.4 1.1 1.4 weeks [g] F(−) after 3 −6.4 −2.7 −3.6 weeks [g] Adhesion energy 34.6 22.8 0.1 after 3 weeks (AU)

(22) Example Materials 30 to 35 are disclosed in Table 8.

(23) TABLE-US-00008 TABLE 8 Example Example Example Example Example Example Reactant material 30 material 31 material 32 material 33 material 34 material 35 X-linker E 20.00 40.00 30.00 60.00 100.00 300.00 polymer type 5 100.00 100.00 100.00 100.00 100.00 100.00 TNBT 0.20 0.20 0.25 0.25 0.20 0.25 LYTOL 100.00 100.00 200.00 200.00 200.00 200.00 F(+)- after 3 weeks [g] 1.8 18.2 3.5 23.0 1.6 1.1 F(−) after 3 weeks [g] −2.4 −11.7 −4.5 −4.2 −4.2 −2.7 t(flow), min >2 min 40 sec — — >5 min — — Adhesion energy after 0.1 67.7 318 17 73.7 0.1 3 weeks (AU) Appearance — — Turbid Turbid — —

(24) Example Materials 36 to 38 are disclosed in Table 9.

(25) TABLE-US-00009 TABLE 9 Example Example Example Reactant material 36 material 37 material 38 X-linker E 100.00 300.00 226.30 polymer type 5 100.00 100.00 100.00 TNBT 0.20 0.20 0.35 200 fluid* 100 cSt 200.00 200.00 300.00 F(+)- after 3 80.927 61.8 220.2 weeks [g] F(−) after 3 −6.077 −24.1 −5.1 weeks [g]

(26) Example Materials 39 to 44 are disclosed in Table 10.

(27) TABLE-US-00010 TABLE 10 Example Example Example Example Example Example Reactant material 39 material 40 material 41 material 42 material 43 material 44 X-linker E 30.0 15.0 30.0 40.0 60.0 polymer type 5 100.00 100.00 100.00 polymer type P 200.00 200.00 200.00 TEOS 0.51 TNBT 0.11 0.25 0.25 0.30 0.25 0.35 200 fluid, 2 cst 100.00 200.00 200.00 400.00 200.00 400.00 F(+)- after 3 weeks [g] 3.4 1.1 1.2 8.8 F(−) after 3 weeks [g] −6.6 −2.5 −2.6 −12.4 Adhesion (AU) after 168 0.1 0.1 154 3 weeks

(28) The evolution of the material properties of selected example materials are shown in Table 11.

(29) TABLE-US-00011 TABLE 11 Example Example Example material 11 material 13 material 15 F(+) day 0 1.0 1.1 1.0 F(−) day 0 −1.2 −1. −1.4 Adhesion energy, Day 0 0.1 0.1 0.1 F(+) day 7 2.2 2.0 7.2 F(−) day 7 −2.4 −3.7 −5.8 Adhesion energy, Day 7 0.1 78.6 83.6 F(+) day 14 2.3 2.3 7.5 F(−) day 14 −3.2 −5.0 −6.2 Adhesion energy, Day 14 204.0 138.5 102.2 F(+) day 21 2.3 2.3 7.7 F(−) day 21 −2.5 −5.1 −6.5 Adhesion energy, Day 21 0.1 167.0 98.0 F(+) day 28 2.5 2.5 7.7 F(−) day 28 −2.4 −5.3 −6.4 Adhesion energy, Day 28 0.1 219.6 100.8 F(+) day + 1 year 3.7 2.5 12.8 F(−) day + 1 year −3.0 −3.7 −9.7 Adhesion energy, + 1 year 15 240 132

(30) Example Material 45 and Comparative Material 1

(31) An emulsion was prepared as follows: 30 g of Polymer Type 1 was combined with 1.5 g of C11-15 Pareth-40 (70% active in water), 0.75 g of C11-15 Pareth-5 (100% active) and 3 g water, and mixed twice using a dental mixer at 3540 rpm for 30 second (each time), forming a satisfying emulsion, which was further diluted with 12.5 g water to form a final emulsion containing 60% active of Polymer Type 1.

(32) The final emulsion was then split in two parts to provide for the Emulsion of Example material 45 and for Comparative material 1 as follows: Comparative material 1 consists in the emulsion left to dry, in absence of any catalyst; while for the Emulsion of Example material 45, an amount of 2% of triethanolamine titanium complex with 80% active ingredient in alcohol was added to the selected part of the final emulsion and also left to dry for 2 days at room temperature.

(33) After drying, no film is observed for the Comparative material 1 which indicates no polymer was formed and that no reaction took place. On the other hand, for Example material 45, a thick film was formed indicating the reaction took place in the emulsion droplet.

Fabric Care Composition Examples Softness Testing

(34) The silicone based materials were evaluated for their impact on softness of terry towels, prepared as per the below method:

(35) A 1kg fabric load composed of 4 little terry towels (further used for panel test)+5 pillow cases (as ballast-recycled) is washed and treated with a softening composition, and line dried overnight before being used for panel test.

(36) Test conditions: Washing Machine: Miele W377 Water Hardness: 0 dH Water quantity: not fixed Detergent powder: Dash powder (10 g)—Added in the drum of the washing machine Fabric softener: lab made dispersion of esterquat at 16% in water, to which is added the amount of emulsion of silicone based material or comparative system at the level of active indicated in Table 1, under mixing using a magnetic stirrer during 5 min, 24 h before the test 6 g of prepared fabric softening composition are then placed in the softener compartment of the washing machine, which will dispense the composition automatically at the last rinse Panel test: 16 assessors are asked to indicate which terry towel is the softest, when presented with 2 terry towels treated with different softening compositions

(37) TABLE-US-00012 TABLE 12 Test Comparison Emulsion of example Comparative Equivalent softness material 22 - 1% emulsion containing performance, with trend active silicone a commercial for softness improvement silicone softening for the emulsion of agent - 1% active Example material 22 silicone

(38) A second test (equivalent conditions as first test here above) was conducted for the evaluation of emulsions of the Example material 42: the emulsion was prepared as follows: 30 g of Example material 42 was combined with 1.5 g of 011-15 Pareth-40 (70% active in water), and 0.75 g of 011-15 Pareth-5 (100% active) and mixed twice using a dental mixer at 3540 rpm for 30 second (each time), forming a satisfying emulsion, which was further diluted with 12.5 g water to form a final emulsion containing 50% active of Example material 42.

(39) The fabric softener containing the emulsion of Example material 42 is found to provide a better softness than the control fabric softener.

Detergent Composition

(40) The Example materials were included in a detergent composition as per Table 2:

(41) TABLE-US-00013 TABLE 13 Detergent Detergent composition 1 composition 2 Ingredient (% wt) (% wt) Water 83.64 83.64 Propylene glycol 2.00 2.00 Sodium xylene sulfonate 0.82 0.82 Linear potassium 6.13 6.13 alklylbenzene sulfonate Alcohol ethoxylate 3.02 3.02 Sodium lauryl ether sulfate 2.14 2.14 Sodium citrate 2.00 2.00 Example material 13 0.25 — Example material 26 — 0.25