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Method for the Production of a Particle-Containing Aerosol

20170130314 ยท 2017-05-11

    Inventors

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    International classification

    Abstract

    The present invention relates to a method for the production of a particle-containing aerosol, which includes comminutating a particle-containing cylinder. These aerosols are for example particularly suitable for use in the form of an aerosol stream in a coating process. The present invention further relates to particle-containing cylinders which can be dispersed and converted into aerosol form by simple methods.

    Claims

    1. A method for the production of a particle-containing aerosol, comprising, comminutating a particle-containing cylinder, wherein the particle-containing cylinder has a volume of at least 5 cm.sup.3 and is dimensionally stable, the content of particles of the particle-containing cylinder lies in the range from 10 wt. % to 99.9 wt. %, based on the total weight of the particle-containing cylinder, the bending strength , of the particle-containing cylinder, is at most 3.75 N/mm.sup.2, where is calculated according to formula (I) = 3 F l 2 B D 2 ( I ) where F=maximum force, B=width of the particle-containing cylinder in rectangular shape, D=height of the particle-containing cylinder in rectangular shape, l=distance between the two points of support, the particles are selected from the group consisting of metal particles, glass particles, mica particles, ceramic particles, and mixtures thereof, the particles contained in the particle-containing cylinder have a d.sub.50 of at most 300 m, and the particle-containing cylinder contains at least 0.01 wt. % of binder, based on the total weight of the particle-containing cylinder, where the binder is selected from the group consisting of inorganic binders, organic binders, and mixtures thereof.

    2. The method of claim 1, wherein the inorganic binder is selected from the group consisting of calcium sulphate, talc, calcium hydroxide, silicon oxide, aluminium oxide, calcium carbonate, calcium silicate hydrates, calcium aluminate hydrates, and mixtures thereof.

    3. The method of claim 1, wherein the organic binder is selected from the group consisting of cellulose, cellulose derivatives, polysaccharides, gelatine, polyvinyls, polyacrylates, polyethylene oxides, polyethylene glycols, polyamides, epoxy resins, polyurethanes, polyaldehydes, polyolefins, polyacrylate copolymers, polyaldehyde copolymers, polycarbonyl copolymers, polyesters, polyolefin copolymers, salts of the aforesaid substances, and mixtures thereof.

    4. The method of claim 1, wherein the particle-containing cylinder has a bending strength of at least 0.0075 N/mm.sup.2.

    5. The method of claim 1, wherein the particle-containing cylinder contains at least 1.5 wt. % of inorganic binder or at least 0.01 wt. % of organic binder.

    6. The method of claim 1, wherein the content of non-flaky particles in the particle-containing cylinder lies in a range from 50 wt. % to 99.9 wt. %, in each case based on the total weight of the particle-containing cylinder.

    7. The method of claim 1, wherein the content of flaky particles in the particle-containing cylinder lies in a range from 30 wt. % to 75 wt. %, in each case based on the total weight of the particle-containing cylinder.

    8. The method of claim 1, wherein the total quantity of particles and binders in the particle-containing cylinder is at least 90 wt. %, based on the total weight of the particle-containing cylinder.

    9. The method of claim 1, wherein the quantity of the binder in the particle-containing cylinder lies in a range from 0.05 wt. % to 70 wt. %, based on total weight of the particle-containing cylinder.

    10. The method of claim 1, wherein at least one binder of the particle-containing cylinder is selected from the group consisting of calcium sulphate and cellulose derivatives.

    11. The method of claim 1, wherein the particles of the particle-containing cylinder are at least 75 wt. % metal particles, based on the total weight of the particles.

    12. A method of coating a substrate, comprising the following steps, a) providing a particle-containing aerosol prepared by the method of claim 1, b) depositing the particles of the particle-containing aerosol on a substrate by a coating method which is selected from the group consisting of cold gas spraying, flame spraying, high velocity flame spraying, thermal plasma spraying, and non-thermal plasma spraying.

    13. A particle-containing cylinder comprising particles, wherein the particle-containing cylinder has a volume of at least 5 cm.sup.3 and is dimensionally stable, the content of particles lies in the range from 10 wt. % to 99.9 wt. %, based on the total weight of the particle-containing cylinder, the bending strength , of the particle-containing cylinder, is at most 3.75 N/mm.sup.2, where is calculated according to formula (I), = 3 F l 2 B D 2 ( I ) where F=maximum force, B=width of the particle-containing cylinder in rectangular shape, D=height of the particle-containing cylinder in rectangular shape, l=distance between the two points of support, the particles are selected from the group consisting of metal particles, glass particles, mica particles, ceramic particles and mixtures thereof, the particles contained in the particle-containing cylinder have a d.sub.50 of at most 300 m and the particle-containing cylinder contains at least 0.01 wt. % of binder, based on the total weight of the particle-containing cylinder, where the binder is selected from the group consisting of inorganic binders, organic binders and mixtures thereof.

    14. The particle-containing cylinder of claim 13, wherein the particle-containing cylinder has a bending strength of at least 0.0075 N/mm.sup.2, the inorganic binder is selected from the group consisting of calcium sulphate, talc, calcium hydroxide, silicon oxide, aluminium oxide, calcium carbonate, calcium silicate hydrates, calcium aluminate hydrates, and mixtures thereof, and the organic binder is selected from the group consisting of cellulose, cellulose derivatives, polysaccharides, gelatine, polyvinyls, polyacrylates, polyethylene oxides, polyethylene glycols, polyamides, epoxy resins, polyurethanes, polyaldehydes, polyolefins, polyacrylate copolymers, polyaldehyde copolymers, polycarbonyl copolymers, polyesters, polyolefin copolymers, the salts of the aforesaid substances, and mixtures thereof.

    15. A particle-containing aerosol prepared by a method comprising, comminutating a particle-containing cylinder, wherein the particle-containing cylinder has a volume of at least 5 cm.sup.3 and is dimensionally stable, the content of particles lies in the range from 10 wt. % to 99.9 wt. %, based on the total weight of the particle-containing cylinder, the bending strength , of the particle-containing cylinder, is at most 3.75 N/mm.sup.2, where is calculated according to formula (I), = 3 F l 2 B D 2 ( I ) where F=maximum force, B=width of the particle-containing cylinder in rectangular shape, D=height of the particle-containing cylinder in rectangular shape, l=distance between the two points of support, the particles are selected from the group consisting of metal particles, glass particles, mica particles, ceramic particles, and mixtures thereof, the particles contained in the particle-containing cylinder have a d.sub.50 of at most 300 m, and the particle-containing cylinder contains at least 0.01 wt. % of binder, based on the total weight of the particle-containing cylinder, where the binder is selected from the group consisting of inorganic binders, organic binders and mixtures thereof.

    Description

    FIGURES

    [0149] FIG. 1: schematic layout of the measurement of the bending strength (1=particle-containing cylinder, 2=support rods, 3=loading rod)

    [0150] FIG. 2: Curve of the three point measurement of a cylinder according to example 1-13 (force in N (y axis) against traverse distance in mm (x axis))

    [0151] FIG. 3: SEM micrograph perpendicular to the coating of a coated glass slide, where this had been broken apart in the region of the coating. Best fit lines were laid through the base surface and the surface of the coating. The thickness of the coating is 25 m.

    EXAMPLE 1: PRODUCTION OF PARTICLE-CONTAINING CYLINDERS USING PLASTER

    [0152] Plaster of the type A/Quick Rock Class 4 (Quick Dental Co.) or type B/Quick Dur S (Quick Dental Co.) and various particles according to table 1 were firstly mixed together and then mixed with deionized water (demineralized water) and ethanol. The now readily flowable material was introduced into a cylindrical mould lined with paper (circular base area, diameter 32 mm). After the cylinder was sufficiently hardened to be dimensionally stable, it was removed from the mould. Next, the cylinder obtained was dried in a drying cabinet at 50 C.

    TABLE-US-00001 TABLE 1 Particle-containing cylinders with binder plaster: CE: comparative example, Ex.: Example, (G): non-flaky particles, (F): flaky particles Quantity Bending of Deionized strength Particle d.sub.50 pigment Plaster water EtOH [N/mm.sup.2] Observation Ex. 1-1 Copper (G) 6 m 95 g 6 g A 20.0 g 2.0 g Ex. 1-2 Copper (G) 30 m 95 g 6 g A 15.0 g 1.5 g Ex. 1-3 Aluminium (G) 2 m 95 g 6 g A 30.0 g 0.0 g Ex. 1-4 Copper (F) 3 m 50 g 54 g A 77.2 g 8.4 g Ex. 1-5 Copper (F) 42 m 70 g 32 g A 65.0 g 7.0 g Ex. 1-6 Brass (F) 16 m 70 g 32 g A 95.0 g 10.0 g Ex. 1-7 Copper- 12 m 70 g 32 g A 105.0 g 11.0 g nickel-zinc alloy (F) Ex. 1-8 Copper 4 m 50 g 54 g A 77.2 g 8.4 g coated with silver (F) Ex. 1-9 Copper (G) 10 m 90 g 12 g A .sup.26 g 3.75 g Ex. 1-10 Copper (F) 3 m 30 g 32 g A .sup.45 g 5.0 g Ex. 1-11 Copper (F) 16 m 30 g 77 g A 95.0 g 10.0 g 0.72 Ex. 1-12 Copper (F) 16 m 70 g 32 g A 95.0 g 10.0 g 0.0195 Ex. 1-13 Copper (F) 16 m 50 g 54 g B 95.0 g 10.0 g 0.21 Ex. 1-14 Copper (F) 16 m 70 g 32 g B 95.0 g 10.0 g 0.3 Ex. 1-15 Copper (G) 6 m 150 g 164 g A 73.0 g 25.0 g 3.15 Ex. 1-16 Copper (G) 6 m 150 g 164 g B 73.0 g 25.0 g 2.4 Ex. 1-17 Copper (G) 6 m 210 g 99 g B 73.0 g 25.0 g 1.1 Ex. 1-18 Copper (G) 6 m 270 g 32 g A 73.0 g 25.0 g 0.22 Ex. 1-19 Copper (G) 6 m 270 g 32 g B 73.0 g 25.0 g 0.14 Ex. 1-20 Copper (F) 16 m 50 g 30 g A 68.0 g 17.0 g Tin (G) 45 m 20 g Ex. 1-21 Copper (G) 10 m 60 g 30 g A 68.0 g 17.0 g Tin (G) 45 m 20 g Ex. 1-22 Glass (F) 20 m 84 g 50 g A 85.0 g 0.0 g Ex. 1-23 Aluminium 11 m 5 g 95 g A 75.0 g 0.0 g oxide (F) CE 1-1 Copper (G) 10 m 95 g 6 g A 20.0 g 2.5 g not dimensionally stable CE 1-2 Copper (G) 6 m 98 g 3 g A .sup.14 g 1.4 g not dimensionally stable CE 1-3 Copper (F) 16 m 80 g 22 g A 110.0 g 11.3 g not dimensionally stable CE 1-4 Copper (F) 42 m 80 g 22 g A 73.0 g 8.0 g not dimensionally stable CE 1-5 Brass (F) 16 m 80 g 22 g A 110.0 g 11.3 g not dimensionally stable

    TABLE-US-00002 TABLE 2 Average densities from Example 1-17 Piece 1 Piece 2 Piece 3 Disc 1 4.59 g/cm.sup.3 4.56 g/cm.sup.3 4.53 g/cm.sup.3 Disc 2 4.57 g/cm.sup.3 4.57 g/cm.sup.3 4.53 g/cm.sup.3 Disc 3 4.50 g/cm.sup.3 4.57 g/cm.sup.3 4.52 g/cm.sup.3

    EXAMPLE 2: PRODUCTION OF PARTICLE-CONTAINING CYLINDERS USING ETHYLCELLULOSE

    [0153] Ethocel Standard 200 Premium (Example 2-1, DOW), Aqualon Ethylcellulose N100 (Example 2-2, Ashland) or Ethocel Std 300 Industrial (Example 2-3, DOW) and particles were first mixed together and then with acetone. The material was introduced into a cylindrical mould lined with paper (circular base area, diameter 32 mm). After the cylinder had hardened sufficiently to be dimensionally stable, it was removed from the mould. Next, the cylinder obtained was dried in a drying cabinet at 50 C.

    TABLE-US-00003 TABLE 3 Particle-containing cylinder with binder ethylcellulose: Ex.: Example, (G): non-flaky particles Particle d.sub.50 Pigment Ethylcellulose Acetone Ex. 2-1 Tin (G) 15 m 199.9 g 0.3 g 14.0 g Ex. 2-2 Tin (G) 15 m 199.9 g 0.3 g 14.0 g Ex. 2-3 Tin (G) 15 m 199.9 g 0.3 g 14.0 g

    EXAMPLE 3: PRODUCTION OF PARTICLE-CONTAINING CYLINDERS USING MICROCRYSTALLINE CELLULOSE

    [0154] Avicel PH-101 and particles were first mixed together and then filled into a tablet press of the Vaneox type (Fluxana Co.). The compression was performed in pressing tools with a diameter of 40 mm by means of a pressure of 3 tons for 10 seconds.

    TABLE-US-00004 TABLE 4 Particle-containing cylinders with binder microcrystalline cellulose: Ex.: Example, (G): non-flaky particles Particle d.sub.50 Pigment Avicel PH-101 Ex. 3-1 Tin (G) 15 m 24.00 g 1.0 g Ex. 3-2 Tin (G) 15 m 24.25 g 0.75 g Ex. 3-3 Tin (G) 15 m 24.5 g 0.50 g Ex. 3-4 Tin (G) 15 m 24.75 g 0.25 g Ex. 3-5 Tin (G) 15 m 23.75 g 1.25 g Ex. 3-6 Tin (G) 15 m 24.88 g 0.12 g Ex. 3-7 Tin (G) 15 m 24.90 g 0.10 g Ex. 3-8 Tin (G) 15 m 24.93 g 0.07 g Ex. 3-9 Tin (G) 15 m 24.25 g 0.75 g Ex. 3-10 Tin (G) 15 m 1.25 g 3.75 g Ex. 3-11 Tin (G) 15 m 5.00 g 5.00 g Ex. 3-12 Tin (G) 15 m 7.50 g 2.50 g Ex. 3-13 Tin (G) 15 m 13.50 g 1.50 g

    EXAMPLE 4: PRODUCTION OF PARTICLE-CONTAINING CYLINDERS USING VARIOUS BINDERS

    [0155] The following binders were first mixed with the non-flaky metal particles (G: non-flaky particles, F: flaky particles) and then with solvent (E: ethanol, W: water, FA: 90% formic acid, EA: ethyl acetate). The material was introduced into a cylindrical mould lined with paper (circular base area, diameter 32 mm). After the cylinder had hardened sufficiently to be dimensionally stable, it was removed from the mould. Next, the cylinders obtained were dried in a drying cabinet at 50 C. In experiment 4-1, drying was then performed at 70 C. In experiment 4-2, drying was performed at 170 C.

    TABLE-US-00005 TABLE 5 Particle-containing cylinders with various binders Particle d.sub.50 Pigment Binder Solvent Ex. 4-1 Copper (G) 15 m 195 g 5 g Acronal 12 DE 15 g W Ex. 4-2 Copper (G) 15 m 195 g 5 g Acronal S747 S 15 g W Ex. 4-3 Copper (G) 15 m 195 g 5 g Acrodur DS 3530 15 g W Ex. 4-4 Copper (G) 15 m 195 g 5 g cellulose 15 g W Thickener C 6000 Ex. 4-5 Copper (G) 15 m 195 g 5 g Gelita Imagel 15 g W Ex. 4-6 Copper (G) 15 m 195 g 5 g Polyglycol 10000 S 15 g W Ex. 4-7 Copper (G) 15 m 195 g 5 g Polyglycol 1500 S 15 g W Ex. 4-8 Copper (G) 15 m 195 g 5 g Ultramid A 15 g FA Ex. 4-9 Copper (G) 15 m 198 g 2 g Sakret PU Ex. 4-10 Copper (G) 15 m 198 g 2 g Epoxy resin binder 2000 EP Ex. 4-11 Copper (G) 15 m 95 g 5 g Laropal A 101 300 g E Ex. 4-12 Copper (G) 15 m 97 g 3 g Laropal A 101 300 g E Ex. 4-13 Copper (G) 15 m 98 g 2 g Laropal A 101 300 g E Ex. 4-14 Copper (G) 15 m 97.5 g 2.5 g Laropal A 101 50 g E Ex. 4-15 Copper (G) 15 m 98.5 g 1.5 g Laropal A 101 50 g E Ex. 4-16 Copper (G) 15 m 97.5 g 2.5 g Resin CA 0002 50 g E Ex. 4-17 Copper (G) 15 m 98.5 g 1.5 g Resin CA 0002 50 g E Ex. 4-18 Copper (G) 15 m 99 g 1 g Resin CA 0002 50 g E Ex. 4-19 Copper (G) 15 m 97.5 g 2 g Degalan P24 50 g EA Ex. 4-20 Copper (G) 15 m 99 g 2 g Degalan P24 50 g EA Ex. 4-21 Copper (G) 15 m 97.5 g 2.5 g CAB 531-1 40 g E Ex. 4-22 Copper (G) 15 m 95 g 5 g CAB 531-1 40 g E Ex. 4-23 Copper (G) 15 m 99 g 1 g Butavar B-76 50 g E Ex. 4-24 Copper (G) 15 m 98.5 g 1.5 g Butavar B-76 50 g E Ex. 4-25 Copper (G) 15 m 98 g 1 g Butavar B-76 50 g E Ex. 4-26 Copper (G) 15 m 98 g 2 g Butavar B-76 50 g E Ex. 4-27 Copper (G) 15 m 195 g 5 g Acronal 32 D 15 g W Ex. 4-28 Copper (G) 15 m 195 g 5 g Styrofan D 780 S 15 g W Ex. 4-29 Copper (G) 15 m 195 g 5 g Urecoll 135 15 g W Ex. 4-30 Copper (G) 15 m 195 g 5 g Saduren 163 15 g W Ex. 4-31 Copper (G) 15 m 195 g 5 g Acronal S 888 S 15 g W Ex. 4-32 Copper (G) 15 m 195 g 5 g Acrodur DS 3515 15 g W Ex. 4-33 Copper (G) 15 m 195 g 5 g Acronal LN 838 S 15 g W Ex. 4-34 Copper (G) 15 m 195 g 5 g Acronal LN 579 S 15 g W

    [0156] Acronal 12 DE, Acronal S747 S (Polyacrylate), Acronal 32 D, Styrofan D 780 S, Urecoll 135, Saduren 163, Acrodur DS 3530, Acronal LN 838 S, Acrodur DS 3515, Acronal LN 579 S, Acronal S 888 S and Ultramid A (polyamide) are marketed by BASF. Cellulose thickener C 6000 (sodium carboxyethylcellulose) is marketed by Kremer Pigments. Gelita Imagel is marketed by the company Gelita. Polyglycol 10000 S and Polyglycol 1500 S are marketed by the company Clariant. Sakret PU is marketed by the company SAKRET Trockenbaustoffe Europa GmbH & Co. KG. Epoxy resin binder 2000 EP is marketed by the company SolipurHfer & Stankowska GbR. CAB 531-1 (cellulose acetate butyrate) is marketed by the company Eastman. Butavar B-76 (polyvinylbutyral) is marketed by Eastman Chemical B.V. Degalan P24 (polyacrylate) is marketed by Evonik.

    [0157] In initial evaluations, the cylinders obtained were found suitable for the method according to the invention.

    EXAMPLE 5: PRODUCTION OF PARTICLE-CONTAINING CYLINDERS USING ACRYLATE MONOMERS

    [0158] 0.5 g of dimethyl-2.2-azobis(2-methylpropionate) (Trade name V 601; available from WAKO Chemicals GmbH, Fuggerstrae 12, 41468 Neuss) and 10 g of trimethylolpropane trimethacrylate are mixed in 50 ml isopropanol. The solution obtained is mixed with 190 g of non-flaky copper particles (d.sub.50=15 m) and introduced into a cylindrical mould lined with paper (circular base area, diameter 32 mm). Next, the cylinder is hardened for 3 hrs at 90 C. In initial evaluations, the cylinders obtained were found suitable for the method according to the invention.

    APPLICATION EXAMPLE 1: DISPERSION

    [0159] Cylinders according to the invention were converted into an aerosol by means of an aerosol generator (Palas RBG 10001). The aerosol stream generated was collected and the solid particles contained therein were measured in a particle size measuring instrument HELOS from the company Sympatec GmbH, Clausthal-Zellerfeld, Germany. Further, the particle material incorporated in the cylinders was dispersed by means of a disperser unit of the Rodos T4.1 type at a primary pressure of for example 4 bar and measured. The assessment of the scattered light signals was performed by the Fraunhofer method.

    TABLE-US-00006 TABLE 6 Dispersion experiments Average particle size of Average particle size of Experiment aerosol collected particles obtained Example 1-10 7 m 3 m Example 1-12 24 m 16 m Example 2-1 29 m 15 m