CN103342364A - Method for separating silicon powder and impurities from mixture - Google Patents
Method for separating silicon powder and impurities from mixture Download PDFInfo
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- CN103342364A CN103342364A CN2013103244431A CN201310324443A CN103342364A CN 103342364 A CN103342364 A CN 103342364A CN 2013103244431 A CN2013103244431 A CN 2013103244431A CN 201310324443 A CN201310324443 A CN 201310324443A CN 103342364 A CN103342364 A CN 103342364A
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- silica flour
- organic solvent
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- water
- impurity
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- 239000012535 impurity Substances 0.000 title claims abstract description 86
- 239000000203 mixture Substances 0.000 title claims abstract description 78
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 title claims abstract description 21
- 239000011863 silicon-based powder Substances 0.000 title claims abstract description 20
- 239000003960 organic solvent Substances 0.000 claims abstract description 172
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 76
- 238000001914 filtration Methods 0.000 claims abstract description 10
- 239000007788 liquid Substances 0.000 claims abstract description 10
- 238000000926 separation method Methods 0.000 claims abstract description 10
- 239000013067 intermediate product Substances 0.000 claims abstract 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 380
- 235000013312 flour Nutrition 0.000 claims description 190
- 239000000377 silicon dioxide Substances 0.000 claims description 190
- 239000012071 phase Substances 0.000 claims description 76
- 239000011324 bead Substances 0.000 claims description 50
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 47
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 47
- 239000002245 particle Substances 0.000 claims description 36
- 239000013527 degreasing agent Substances 0.000 claims description 31
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 27
- 239000008188 pellet Substances 0.000 claims description 27
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 18
- 239000001488 sodium phosphate Substances 0.000 claims description 16
- 235000011008 sodium phosphates Nutrition 0.000 claims description 16
- 239000008346 aqueous phase Substances 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 10
- REYJJPSVUYRZGE-UHFFFAOYSA-N Octadecylamine Chemical compound CCCCCCCCCCCCCCCCCCN REYJJPSVUYRZGE-UHFFFAOYSA-N 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 9
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 9
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 9
- -1 stir Substances 0.000 claims description 9
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical class CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 4
- ODLMAHJVESYWTB-UHFFFAOYSA-N propylbenzene Chemical compound CCCC1=CC=CC=C1 ODLMAHJVESYWTB-UHFFFAOYSA-N 0.000 claims description 4
- 125000000383 tetramethylene group Chemical group [H]C([H])([*:1])C([H])([H])C([H])([H])C([H])([H])[*:2] 0.000 claims description 4
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 3
- 150000004945 aromatic hydrocarbons Chemical class 0.000 claims description 2
- 125000000753 cycloalkyl group Chemical group 0.000 claims description 2
- DMEGYFMYUHOHGS-UHFFFAOYSA-N cycloheptane Chemical compound C1CCCCCC1 DMEGYFMYUHOHGS-UHFFFAOYSA-N 0.000 claims description 2
- 229910000162 sodium phosphate Inorganic materials 0.000 claims description 2
- 229930195735 unsaturated hydrocarbon Natural products 0.000 claims description 2
- 239000004005 microsphere Substances 0.000 abstract 3
- 239000003795 chemical substances by application Substances 0.000 abstract 2
- 239000003921 oil Substances 0.000 abstract 2
- 239000007864 aqueous solution Substances 0.000 description 5
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 4
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- ZGEGCLOFRBLKSE-UHFFFAOYSA-N 1-Heptene Chemical compound CCCCCC=C ZGEGCLOFRBLKSE-UHFFFAOYSA-N 0.000 description 2
- YNQLUTRBYVCPMQ-UHFFFAOYSA-N Ethylbenzene Chemical compound CCC1=CC=CC=C1 YNQLUTRBYVCPMQ-UHFFFAOYSA-N 0.000 description 2
- OCKPCBLVNKHBMX-UHFFFAOYSA-N butylbenzene Chemical compound CCCCC1=CC=CC=C1 OCKPCBLVNKHBMX-UHFFFAOYSA-N 0.000 description 2
- 238000005266 casting Methods 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 230000001804 emulsifying effect Effects 0.000 description 2
- 239000012074 organic phase Substances 0.000 description 2
- JRZJOMJEPLMPRA-UHFFFAOYSA-N 1-nonene Chemical class CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- WJTCGQSWYFHTAC-UHFFFAOYSA-N cyclooctane Chemical compound C1CCCCCCC1 WJTCGQSWYFHTAC-UHFFFAOYSA-N 0.000 description 1
- 239000004914 cyclooctane Substances 0.000 description 1
- SNRUBQQJIBEYMU-UHFFFAOYSA-N dodecane Chemical class CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 210000002615 epidermis Anatomy 0.000 description 1
- 125000004836 hexamethylene group Chemical class [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 description 1
- 238000009775 high-speed stirring Methods 0.000 description 1
- RGSFGYAAUTVSQA-UHFFFAOYSA-N pentamethylene Natural products C1CCCC1 RGSFGYAAUTVSQA-UHFFFAOYSA-N 0.000 description 1
- 125000004817 pentamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
Landscapes
- Silicon Compounds (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a method for separating silicon powder and impurities from a mixture, which comprises the following steps: putting a mixture to be treated in a liquid composed of an organic solvent and water, thereby obtaining a system composed of silicon-powder-coated organic solvent phase microspheres, impurities and water after the silicon powder in the mixture enters the organic solvent phase; filtering the silicon-powder-coated organic solvent phase microspheres and impurities in the system by using a filter to obtain the silicon-powder-coated organic solvent phase microspheres; adding an oil removal agent and water; and since a water-soluble intermediate product obtained by the reaction between the organic solvent and oil removal agent enters the water phase and the silicon powder is insoluble in water, separating the silicon powder from the water-soluble intermediate product in the water phase by using a filter to obtain the separated silicon powder. The method can greatly lower the separation treatment time, saves the consumption of the organic solvent, lowers the cost for separating the silicon powder and impurities from the mixture, and reduces the negative influence of abundant organic solvent on the environment.
Description
Technical field
The present invention relates to a kind of method that silica flour in the mixture is separated with impurity of photovoltaic and semiconductor applications.
Background technology
The available technology adopting organic solvent is handled the silica flour in the mixture and impurity, separates to obtain silicon
Powder and impurity, though can realize silica flour and separate impurities, the organic solvent amount that consumes is big, the time that organic solvent is handled is longer, cause cost higher, and the processing cycle is also longer.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of method that silica flour in the mixture is separated with impurity, after obtaining wrapping up the organic solvent phase bead of silica flour after adopting organic solvent that silica flour is handled, filter by organic solvent phase bead and the impurity of strainer to this parcel silica flour, realize that silica flour separates with impurity, can reduce greatly the separating treatment time, improve processing efficiency, saved the usage quantity of organic solvent simultaneously, silica flour in the minimizing separating mixture and the cost of impurity, and reduced and used a large amount of organic solvents to the negative impact of environment.
Technical scheme of the present invention is:
A kind of method that silica flour in the mixture is separated with impurity comprises: pending mixture is placed the liquid of being made up of organic solvent and water, and the consumption of water doubly disposes by the 20-100 of contained silica flour weight in the mixture; The consumption of organic solvent doubly disposes by the 0.2-4 of contained silica flour weight in the mixture, and the organic solvent that adopts is by volume: alkane 28-48 part, aromatic hydrocarbons 20-50 part, unsaturated hydrocarbons 1-6 part, cyclic hydrocarbon 17-44 part; Silica flour in the mixture enter organic solvent mutually in, thereby the relative silicon powder particle of organic solvent coats the organic solvent phase bead that forms the parcel silica flour fully, obtains the system of being made up of organic solvent phase bead, silicon carbide impurity and the water of parcel silica flour; Adopt strainer that organic solvent phase bead and the silicon carbide impurity of the parcel silica flour in the system are filtered, silicon carbide impurity particle diameter is 0.1-30 μ m, the organic solvent phase bead particle diameter of described parcel silica flour is 10mm, the aperture of this strainer is 300 μ m, the organic solvent phase pellet of parcel silica flour is that the strainer of 300 μ m is held back by the aperture, silicon carbide impurity passes the strainer that the aperture is 300 μ m with water, realizes the organic solvent phase pellet of parcel silica flour and the initial gross separation of silicon carbide impurity.
After obtaining wrapping up the organic solvent phase pellet of silica flour, add degreaser and water, the consumption of degreaser doubly disposes by the 0.5-2 of contained silica flour weight in the mixture, the consumption of water doubly disposes by the 10-80 of contained silica flour weight in the mixture, stir, degreaser is formulated by following materials of weight proportions: water 80-90 part, fatty alcohol-polyoxyethylene ether 5-10 part, tertiary sodium phosphate 1.8-3.0 part, sodium phosphate 2.0-3.0 part, 95% ethanol 1.0-2.0 part, stearylamine 1.5-2.5 part, sodium hydroxide 0.6-1.0 part, adopted degreaser, make that the parcel balance between organic solvent and the silica flour is upset, effective constituent generation emulsifying effect in organic solvent and the degreaser and enter aqueous phase, and silica flour is water insoluble, with filtration unit silica flour and the organic solvent that enters aqueous phase are being separated the silica flour after obtaining separating.
Organic solvent is scattered in the aqueous solution that contains silica flour under the condition of high-speed stirring among the present invention, namely realize that by stirring organic solvent disperses and exists with the small droplets form in the aqueous solution, simultaneously in whipping process, silica flour in the aqueous solution constantly collides with the organic solvent small droplets and is adsorbed by the organic solvent drop, along with the carrying out of this process, increasing silica flour forms the big organic solvent phase bead that includes silica flour around being adsorbed on drop.
Principle of work of the present invention: when adopting organic solvent that the silica flour in the mixture and impurity are handled, because the lipophilicity of silica flour, silica flour will enter into organic solvent mutually, can realize the coating fully of the relative silicon powder particle of organic solvent, and because organic solvent and water is insoluble, and silica flour has stopped converging mutually of organic solvent and organic solvent phase, thereby realize silica flour be distributed in organic solvent mutually in and the organic solvent phase bead that forms the parcel silica flour float on or be scattered in aqueous phase, obtain wrapping up the organic solvent phase bead of silica flour, the system that impurity and water are formed, utilize the organic solvent phase bead particle diameter of parcel silica flour much larger than the particle diameter of impurity particle, use the aperture greater than the particle diameter of impurity particle, strainer less than the organic solvent phase bead particle diameter of parcel silica flour filters organic solvent phase bead and the impurity of the parcel silica flour in the system, can realize that silica flour separates with impurity, so can reduce greatly the separating treatment time, also reduce the usage quantity of organic solvent.
Because prior art adopts organic solvent that silica flour and impurity are carried out separating treatment, is the hydrophilic different differences that depend on silica flour lipophilicity, impurity, realize separating fully of silica flour and impurity.Usually, need to add relatively large organic solvent in treating processes, silica flour enters in the organic solvent, and impurity is scattered in the aqueous solution, and because the not mutual solubility of organic solvent and water, and density is lower than water, silica flour be scattered in organic solvent mutually in and float on aqueous solution upper epidermis, by the collection to organic solvent layer, realization is to the recovery of silica flour, such method need expend the long treatment time, also need expend relatively large organic solvent simultaneously, is unfavorable for applying aborning.
The implementation result of table 1 the present invention and prior art relatively
Advantage of the present invention: after obtaining wrapping up the organic solvent phase bead of silica flour after adopting organic solvent that silica flour is handled, filter by organic solvent phase bead and the impurity of strainer to this parcel silica flour, realize that silica flour separates with impurity, can reduce greatly the separating treatment time, improve processing efficiency, saved the usage quantity of organic solvent simultaneously, silica flour in the minimizing separating mixture and the cost of impurity, be that time organic phase bead more short, that become is more big, cost is more low, just more good concerning silica flour is purified.And reduced and used a large amount of organic solvents to the negative impact of environment.
Embodiment
Embodiment 1,
A kind of method that silica flour in the mixture is separated with impurity comprises: pending mixture is placed the liquid of being made up of organic solvent and water, and the consumption of water is pressed 20 times of configurations of contained silica flour weight in the mixture; The consumption of organic solvent is pressed 0.2 times of configuration of contained silica flour weight in the mixture, and the organic solvent that adopts is by volume: 28 parts of hexanes, 20 parts of propyl benzene, 1 part of 1-butylene, 17 parts of suberane; Silica flour in the mixture enter organic solvent mutually in, thereby the relative silicon powder particle of organic solvent coats the organic solvent phase bead that forms the parcel silica flour fully, obtains the system of being made up of organic solvent phase bead, silicon carbide impurity and the water of parcel silica flour; Adopt strainer that organic solvent phase bead and the silicon carbide impurity of the parcel silica flour in the system are filtered, silicon carbide impurity particle diameter is 0.1-30 μ m, the organic solvent phase bead particle diameter of described parcel silica flour is 11.3mm, the aperture of this strainer is 300 μ m, the organic solvent phase pellet of parcel silica flour is that the strainer of 300 μ m is held back by the aperture, silicon carbide impurity passes the strainer that the aperture is 300 μ m with water, realizes the organic solvent phase pellet of parcel silica flour and the initial gross separation of silicon carbide impurity.
After obtaining wrapping up the organic solvent phase pellet of silica flour, add degreaser and water, the consumption of degreaser is pressed 0.5 times of configuration of contained silica flour weight in the mixture, the consumption of water is pressed 10 times of configurations of contained silica flour weight in the mixture, stir, degreaser is formulated by following materials of weight proportions: 90 parts in water, 5 parts of fatty alcohol-polyoxyethylene ether, 1.8 parts of tertiary sodium phosphates, 2.0 parts of sodium phosphates, 1.0 parts of 95% ethanol, 1.5 parts of stearylamines, 0.6 part in sodium hydroxide, with filtration unit silica flour and the organic solvent that enters aqueous phase are separated the silica flour after obtaining separating again.
Embodiment 2,
A kind of method that silica flour in the mixture is separated with impurity comprises: pending mixture is placed the liquid of being made up of organic solvent and water, and the consumption of water is pressed 60 times of configurations of contained silica flour weight in the mixture; The consumption of organic solvent is pressed 2.1 times of configurations of contained silica flour weight in the mixture, and the organic solvent that adopts is by volume: 38 parts of heptane, 35 parts of dimethylbenzene, 3 parts of 1-nonenes, 30 parts of tetramethylene; Silica flour in the mixture enter organic solvent mutually in, thereby the relative silicon powder particle of organic solvent coats the organic solvent phase bead that forms the parcel silica flour fully, obtains the system of being made up of organic solvent phase bead, silicon carbide impurity and the water of parcel silica flour; Adopt strainer that organic solvent phase bead and the silicon carbide impurity of the parcel silica flour in the system are filtered, silicon carbide impurity particle diameter is 0.1-30 μ m, the organic solvent phase bead particle diameter of described parcel silica flour is 10.8mm, the aperture of this strainer is 300 μ m, the organic solvent phase pellet of parcel silica flour is that the strainer of 300 μ m is held back by the aperture, silicon carbide impurity passes the strainer that the aperture is 300 μ m with water, realizes the organic solvent phase pellet of parcel silica flour and the initial gross separation of silicon carbide impurity.
After obtaining wrapping up the organic solvent phase pellet of silica flour, add degreaser and water, the consumption of degreaser is pressed 1.2 times of configurations of contained silica flour weight in the mixture, the consumption of water is pressed 45 times of configurations of contained silica flour weight in the mixture, stir, degreaser is formulated by following materials of weight proportions: 95 parts in water, 8 parts of fatty alcohol-polyoxyethylene ether, 2.4 parts of tertiary sodium phosphates, 2.5 parts of sodium phosphates, 1.5 parts of 95% ethanol, 2.0 parts of stearylamines, 0.8 part in sodium hydroxide, with filtration unit silica flour and the organic solvent that enters aqueous phase are separated the silica flour after obtaining separating again.
Embodiment 3,
A kind of method that silica flour in the mixture is separated with impurity comprises: pending mixture is placed the liquid of being made up of organic solvent and water, and the consumption of water is pressed 100 times of configurations of contained silica flour weight in the mixture; The consumption of organic solvent is pressed 4 times of configurations of contained silica flour weight in the mixture, and the organic solvent that adopts is by volume: 48 parts of octanes, 50 parts of toluene, 6 parts of 1-amylenes, 44 parts of hexanaphthenes; Silica flour in the mixture enter organic solvent mutually in, thereby the relative silicon powder particle of organic solvent coats the organic solvent phase bead that forms the parcel silica flour fully, obtains the system of being made up of organic solvent phase bead, silicon carbide impurity and the water of parcel silica flour; Adopt strainer that organic solvent phase bead and the silicon carbide impurity of the parcel silica flour in the system are filtered, silicon carbide impurity particle diameter is 0.1-30 μ m, the organic solvent phase bead particle diameter of described parcel silica flour is 11.1mm, the aperture of this strainer is 300 μ m, the organic solvent phase pellet of parcel silica flour is that the strainer of 300 μ m is held back by the aperture, silicon carbide impurity passes the strainer that the aperture is 300 μ m with water, realizes the organic solvent phase pellet of parcel silica flour and the initial gross separation of silicon carbide impurity.
After obtaining wrapping up the organic solvent phase pellet of silica flour, add degreaser and water, the consumption of degreaser is pressed 2 times of configurations of contained silica flour weight in the mixture, the consumption of water is pressed 80 times of configurations of contained silica flour weight in the mixture, stir, degreaser is formulated by following materials of weight proportions: 100 parts in water, 10 parts of fatty alcohol-polyoxyethylene ether, 3.0 parts of tertiary sodium phosphates, 3.0 parts of sodium phosphates, 2.0 parts of 95% ethanol, 2.5 parts of stearylamines, 1.0 parts in sodium hydroxide, with filtration unit silica flour and the organic solvent that enters aqueous phase are separated the silica flour after obtaining separating again.
Embodiment 4,
A kind of method that silica flour in the mixture is separated with impurity comprises: pending mixture is placed the liquid of being made up of organic solvent and water, and the consumption of water is pressed 40 times of configurations of contained silica flour weight in the mixture; The consumption of organic solvent is pressed 1.0 times of configurations of contained silica flour weight in the mixture, and the organic solvent that adopts is by volume: 48 parts in certain herbaceous plants with big flowers alkane, 25 parts in ethylbenzene, 6 parts of 1-hexenes, 31 parts of cyclooctane; Silica flour in the mixture enter organic solvent mutually in, thereby the relative silicon powder particle of organic solvent coats the organic solvent phase bead that forms the parcel silica flour fully, obtains the system of being made up of organic solvent phase bead, silicon carbide impurity and the water of parcel silica flour; Adopt strainer that organic solvent phase bead and the silicon carbide impurity of the parcel silica flour in the system are filtered, silicon carbide impurity particle diameter is 0.1-30 μ m, the organic solvent phase bead particle diameter of described parcel silica flour is 10.9mm, the aperture of this strainer is 300 μ m, the organic solvent phase pellet of parcel silica flour is that the strainer of 300 μ m is held back by the aperture, silicon carbide impurity passes the strainer that the aperture is 300 μ m with water, realizes the organic solvent phase pellet of parcel silica flour and the initial gross separation of silicon carbide impurity.
After obtaining wrapping up the organic solvent phase pellet of silica flour, add degreaser and water, the consumption of degreaser is pressed 0.8 times of configuration of contained silica flour weight in the mixture, the consumption of water is pressed 20 times of configurations of contained silica flour weight in the mixture, stir, degreaser is formulated by following materials of weight proportions: 90 parts in water, 8 parts of fatty alcohol-polyoxyethylene ether, 2.0 parts of tertiary sodium phosphates, 2.2 parts of sodium phosphates, 1.3 parts of 95% ethanol, 1.8 parts of stearylamines, 0.8 part in sodium hydroxide, with filtration unit silica flour and the organic solvent that enters aqueous phase are separated the silica flour after obtaining separating again.
Embodiment 5,
A kind of method that silica flour in the mixture is separated with impurity comprises: pending mixture is placed the liquid of being made up of organic solvent and water, and the consumption of water is pressed 90 times of configurations of contained silica flour weight in the mixture; The consumption of organic solvent is pressed 3.5 times of configurations of contained silica flour weight in the mixture, and the organic solvent that adopts is by volume: 42 parts of dodecanes, 38 parts of butylbenzene, 6 parts of 1-heptene, 44 parts of pentamethylene; Silica flour in the mixture enter organic solvent mutually in, thereby the relative silicon powder particle of organic solvent coats the organic solvent phase bead that forms the parcel silica flour fully, obtains the system of being made up of organic solvent phase bead, silicon carbide impurity and the water of parcel silica flour; Adopt strainer that organic solvent phase bead and the silicon carbide impurity of the parcel silica flour in the system are filtered, silicon carbide impurity particle diameter is 0.1-30 μ m, the organic solvent phase bead particle diameter of described parcel silica flour is 10.7mm, the aperture of this strainer is 300 μ m, the organic solvent phase pellet of parcel silica flour is that the strainer of 300 μ m is held back by the aperture, silicon carbide impurity passes the strainer that the aperture is 300 μ m with water, realizes the organic solvent phase pellet of parcel silica flour and the initial gross separation of silicon carbide impurity.
After obtaining wrapping up the organic solvent phase pellet of silica flour, add degreaser and water, the consumption of degreaser is pressed 1.8 times of configurations of contained silica flour weight in the mixture, the consumption of water is pressed 70 times of configurations of contained silica flour weight in the mixture, stir, degreaser is formulated by following materials of weight proportions: 98 parts in water, 10 parts of fatty alcohol-polyoxyethylene ether, 2.8 parts of tertiary sodium phosphates, 2.9 parts of sodium phosphates, 1.8 parts of 95% ethanol, 2.2 parts of stearylamines, 0.9 part in sodium hydroxide, with filtration unit silica flour and the organic solvent that enters aqueous phase are separated the silica flour after obtaining separating again.
Embodiment 6,
A kind of method that silica flour in the mixture is separated with impurity comprises: pending mixture is placed the liquid of being made up of organic solvent and water, and the consumption of water is pressed 15 times of configurations of contained silica flour weight in the mixture; The consumption of organic solvent is pressed 5 times of configurations of contained silica flour weight in the mixture, and the organic solvent that adopts is by volume: 12 parts of heptane, 53 parts of dimethylbenzene, 10 parts of tetramethylene; Silica flour in the mixture enter organic solvent mutually in, thereby the relative silicon powder particle of organic solvent coats the organic solvent phase bead that forms the parcel silica flour fully, obtains the system of being made up of organic solvent phase bead, silicon carbide impurity and the water of parcel silica flour; Adopt strainer that organic solvent phase bead and the silicon carbide impurity of the parcel silica flour in the system are filtered, silicon carbide impurity particle diameter is 0.1-30 μ m, the organic solvent phase bead particle diameter of described parcel silica flour is 7.5mm, the aperture of this strainer is 300 μ m, the organic solvent phase pellet of parcel silica flour is that the strainer of 300 μ m is held back by the aperture, silicon carbide impurity passes the strainer that the aperture is 300 μ m with water, realizes the organic solvent phase pellet of parcel silica flour and the initial gross separation of silicon carbide impurity.
After obtaining wrapping up the organic solvent phase pellet of silica flour, add degreaser and water, the consumption of degreaser is pressed 0.4 times of configuration of contained silica flour weight in the mixture, the consumption of water is pressed 85 times of configurations of contained silica flour weight in the mixture, stir, degreaser is formulated by following materials of weight proportions: 80 parts in water, 10 parts of fatty alcohol-polyoxyethylene ether (AEO7), 3.5 parts of tertiary sodium phosphates, 3.5 parts of sodium phosphates, 0.8 part of 95% ethanol, 1.2 parts of stearylamines, 1.2 parts in sodium hydroxide, adopted degreaser, make that the parcel balance between organic solvent and the silica flour is upset, effective constituent generation emulsifying effect in organic solvent and the degreaser and enter aqueous phase, and silica flour is water insoluble, with filtration unit silica flour and the organic solvent that enters aqueous phase are being separated the silica flour after obtaining separating.
The effect of each embodiment is as shown in the table:
From last table data as can be seen, it is silica flour more than 99% that embodiment 1-5 invention step in the technology of the present invention scope repeats can to obtain respectively for 2-3 time purity, especially can obtain purity with embodiment 1 is 99.6% silica flour, is 80.3% silica flour but embodiment 6 has to purity; Simultaneously the used organic solvent amount of embodiment 1-5 is also less than embodiment 6, the organic solvent phase bead particle diameter of parcel silica flour is bigger, the required treatment time is shorter, especially minimum with the organic solvent amount of embodiment 1, the organic solvent phase bead particle diameter maximum of parcel silica flour, the required treatment time is also the shortest; Therefore the present invention has not only realized silica flour and separate impurities, also greatly reduce the separating treatment time, improve processing efficiency, saved the usage quantity of organic solvent simultaneously, silica flour in the minimizing separating mixture and the cost of impurity, be that time organic phase bead more short, that become is more big, cost is more low, just more good concerning silica flour is purified, and reduced and used a large amount of organic solvents to the negative impact of environment.
The happy and harmonious mode of high temperature of separating the purity obtain simultaneously and be the silica flour ingot casting that 99% silica flour can be by routine further obtains the higher silica flour of purity, because most silicon carbide are removed, remaining non-silicon carbide impurity is that the happy and harmonious mode of high temperature about 20 hours also can obtain good removal by the cycle, obtain the higher silica flour of purity like this and be expected to enter sun power ingot casting field as raw material, improved the value that reclaims greatly.
Claims (4)
1. method that silica flour in the mixture is separated with impurity, it is characterized in that: pending mixture is placed the liquid of being made up of organic solvent and water, and the consumption of water doubly disposes by the 20-100 of contained silica flour weight in the mixture; The consumption of organic solvent doubly disposes by the 0.2-4 of contained silica flour weight in the mixture, and the organic solvent that adopts is by volume: alkane 28-48 part, aromatic hydrocarbons 20-50 part, unsaturated hydrocarbons 1-6 part, cyclic hydrocarbon 17-44 part; Silica flour in the mixture enter organic solvent mutually in, thereby the relative silicon powder particle of organic solvent coats the organic solvent phase bead that forms the parcel silica flour fully, obtains the system of being made up of organic solvent phase bead, silicon carbide impurity and the water of parcel silica flour; Adopt strainer that organic solvent phase bead and the silicon carbide impurity of the parcel silica flour in the system are filtered, silicon carbide impurity particle diameter is 0.1-30 μ m, the organic solvent phase bead particle diameter of described parcel silica flour is 10mm, the aperture of this strainer is 300 μ m, the organic solvent phase pellet of parcel silica flour is that the strainer of 300 μ m is held back by the aperture, silicon carbide impurity passes the strainer that the aperture is 300 μ m with water, realizes the organic solvent phase pellet of parcel silica flour and the initial gross separation of silicon carbide impurity.
2. a kind of method that silica flour in the mixture is separated with impurity as claimed in claim 1, it is characterized in that: after obtaining wrapping up the organic solvent phase pellet of silica flour, add degreaser and water, the consumption of degreaser doubly disposes by the 0.5-2 of contained silica flour weight in the mixture, the consumption of water doubly disposes by the 10-80 of contained silica flour weight in the mixture, stir, degreaser is formulated by following materials of weight proportions: water 90-100 part, fatty alcohol-polyoxyethylene ether 5-10 part, tertiary sodium phosphate 1.8-3.0 part, sodium phosphate 2.0-3.0 part, 95% ethanol 1.0-2.0 part, stearylamine 1.5-2.5 part, sodium hydroxide 0.6-1.0 part, with filtration unit silica flour and the water miscible intermediate product that enters aqueous phase are separated the silica flour after obtaining separating again.
3. a kind of method that silica flour in the mixture is separated with impurity as claimed in claim 1, it is characterized in that: pending mixture is placed the liquid of being made up of organic solvent and water, and the consumption of water is pressed 20 times of configurations of contained silica flour weight in the mixture; The consumption of organic solvent is pressed 0.2 times of configuration of contained silica flour weight in the mixture, and the organic solvent that adopts is by volume: 28 parts of hexanes, 20 parts of propyl benzene, 1 part of 1-butylene, 17 parts of suberane; Silica flour in the mixture enter organic solvent mutually in, thereby the relative silicon powder particle of organic solvent coats the organic solvent phase bead that forms the parcel silica flour fully, obtains the system of being made up of organic solvent phase bead, silicon carbide impurity and the water of parcel silica flour; Adopt strainer that organic solvent phase bead and the silicon carbide impurity of the parcel silica flour in the system are filtered, silicon carbide impurity particle diameter is 0.1-30 μ m, the organic solvent phase bead particle diameter of described parcel silica flour is 11.3mm, the aperture of this strainer is 300 μ m, the organic solvent phase pellet of parcel silica flour is that the strainer of 300 μ m is held back by the aperture, silicon carbide impurity passes the strainer that the aperture is 300 μ m with water, realizes the organic solvent phase pellet of parcel silica flour and the initial gross separation of silicon carbide impurity.
4. a kind of method that silica flour in the mixture is separated with impurity as claimed in claim 2, it is characterized in that: after obtaining wrapping up the organic solvent phase pellet of silica flour, add degreaser and water, the consumption of degreaser is pressed 0.5 times of configuration of contained silica flour weight in the mixture, the consumption of water is pressed 10 times of configurations of contained silica flour weight in the mixture, stir, degreaser is formulated by following materials of weight proportions: 90 parts in water, 5 parts of fatty alcohol-polyoxyethylene ether, 1.8 parts of tertiary sodium phosphates, 2.0 parts of sodium phosphates, 1.0 parts of 95% ethanol, 1.5 parts of stearylamines, 0.6 part in sodium hydroxide, with filtration unit silica flour and the organic solvent that enters aqueous phase are separated the silica flour after obtaining separating again.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP4335541B2 (en) * | 2003-01-20 | 2009-09-30 | 隼次 芝田 | Method and apparatus for separating SiO2 particles and SiC particles, and separation and recovery SiC |
| CN101597119A (en) * | 2008-06-03 | 2009-12-09 | 新疆德蓝科技有限公司 | Integrating technology of water supplying and saving and sewage reusing technology system in petroleum and petrochemical industry |
| CN101823716A (en) * | 2010-03-09 | 2010-09-08 | 江西赛维Ldk太阳能高科技有限公司 | Method for separating silica powder and impurities in mixture |
| CN102060299A (en) * | 2009-11-12 | 2011-05-18 | 江西赛维Ldk太阳能高科技有限公司 | Method for separating silica powder from impurities in mixture |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4335541B2 (en) * | 2003-01-20 | 2009-09-30 | 隼次 芝田 | Method and apparatus for separating SiO2 particles and SiC particles, and separation and recovery SiC |
| CN101597119A (en) * | 2008-06-03 | 2009-12-09 | 新疆德蓝科技有限公司 | Integrating technology of water supplying and saving and sewage reusing technology system in petroleum and petrochemical industry |
| CN102060299A (en) * | 2009-11-12 | 2011-05-18 | 江西赛维Ldk太阳能高科技有限公司 | Method for separating silica powder from impurities in mixture |
| CN101823716A (en) * | 2010-03-09 | 2010-09-08 | 江西赛维Ldk太阳能高科技有限公司 | Method for separating silica powder and impurities in mixture |
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