CN103342364B - A kind of method of silica flour in mixture and impurity being carried out be separated - Google Patents
A kind of method of silica flour in mixture and impurity being carried out be separated Download PDFInfo
- Publication number
- CN103342364B CN103342364B CN201310324443.1A CN201310324443A CN103342364B CN 103342364 B CN103342364 B CN 103342364B CN 201310324443 A CN201310324443 A CN 201310324443A CN 103342364 B CN103342364 B CN 103342364B
- Authority
- CN
- China
- Prior art keywords
- organic solvent
- silica flour
- mixture
- water
- parts
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 306
- 235000013312 flour Nutrition 0.000 title claims abstract description 153
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 153
- 239000012535 impurity Substances 0.000 title claims abstract description 75
- 239000000203 mixture Substances 0.000 title claims abstract description 71
- 238000000034 method Methods 0.000 title claims abstract description 23
- 239000003960 organic solvent Substances 0.000 claims abstract description 165
- 239000012071 phase Substances 0.000 claims abstract description 84
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 67
- 239000011324 bead Substances 0.000 claims abstract description 49
- 239000013527 degreasing agent Substances 0.000 claims abstract description 30
- 239000008188 pellet Substances 0.000 claims abstract description 25
- 239000008346 aqueous phase Substances 0.000 claims abstract description 14
- 238000001914 filtration Methods 0.000 claims abstract description 9
- 239000007788 liquid Substances 0.000 claims abstract description 9
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 44
- 239000011863 silicon-based powder Substances 0.000 claims description 43
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 42
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 42
- 239000002245 particle Substances 0.000 claims description 33
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 16
- -1 stir Substances 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 9
- REYJJPSVUYRZGE-UHFFFAOYSA-N Octadecylamine Chemical compound CCCCCCCCCCCCCCCCCCN REYJJPSVUYRZGE-UHFFFAOYSA-N 0.000 claims description 8
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 8
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 8
- 238000002360 preparation method Methods 0.000 claims description 8
- 230000000717 retained effect Effects 0.000 claims description 8
- 238000000926 separation method Methods 0.000 claims description 8
- 239000001488 sodium phosphate Substances 0.000 claims description 8
- 229910000162 sodium phosphate Inorganic materials 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 6
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 6
- 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
- DMEGYFMYUHOHGS-UHFFFAOYSA-N cycloheptane Chemical compound C1CCCCCC1 DMEGYFMYUHOHGS-UHFFFAOYSA-N 0.000 claims description 2
- 238000009775 high-speed stirring Methods 0.000 claims description 2
- 239000013067 intermediate product Substances 0.000 abstract 2
- 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
- ZGEGCLOFRBLKSE-UHFFFAOYSA-N 1-Heptene Chemical compound CCCCCC=C ZGEGCLOFRBLKSE-UHFFFAOYSA-N 0.000 description 2
- LIKMAJRDDDTEIG-UHFFFAOYSA-N 1-hexene Chemical compound CCCCC=C LIKMAJRDDDTEIG-UHFFFAOYSA-N 0.000 description 2
- JRZJOMJEPLMPRA-UHFFFAOYSA-N 1-nonene Chemical compound CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 2
- YNQLUTRBYVCPMQ-UHFFFAOYSA-N Ethylbenzene Chemical compound CCC1=CC=CC=C1 YNQLUTRBYVCPMQ-UHFFFAOYSA-N 0.000 description 2
- 150000001335 aliphatic alkanes Chemical class 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
- SNRUBQQJIBEYMU-UHFFFAOYSA-N dodecane Chemical compound CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 2
- 230000001804 emulsifying effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000012074 organic phase Substances 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 125000000753 cycloalkyl group Chemical group 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
- 230000000694 effects Effects 0.000 description 1
- 210000002615 epidermis Anatomy 0.000 description 1
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 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
- YWAKXRMUMFPDSH-UHFFFAOYSA-N pentene Chemical group CCCC=C YWAKXRMUMFPDSH-UHFFFAOYSA-N 0.000 description 1
- 239000000843 powder Substances 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
- 229930195735 unsaturated hydrocarbon Natural products 0.000 description 1
Landscapes
- Silicon Compounds (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a kind of method of silica flour in mixture and impurity being carried out be separated, comprise: pending mixture is placed in the liquid be made up of organic solvent and water, silica flour in mixture enters in organic solvent phase, obtain by the organic solvent phase bead of parcel silica flour, the system of impurity and water composition, strainer is adopted to filter the organic solvent phase bead of the parcel silica flour in system and impurity again, after obtaining the organic solvent phase pellet of parcel silica flour, add degreaser and water, organic solvent and degreaser react and obtain water miscible intermediate product and enter in aqueous phase, and silica flour is water insoluble, with filtration unit, silica flour and the water miscible intermediate product entered in aqueous phase are being separated, obtain the silica flour after being separated, the method can greatly reduce the separating treatment time, save the usage quantity of organic solvent, silica flour in minimizing separating mixture and the cost of impurity, also reduce simultaneously and use a large amount of organic solvent to the negative impact of environment.
Description
Technical field
The present invention relates to a kind of method of silica flour in mixture and impurity being carried out be separated of photovoltaic and semiconductor applications.
Background technology
Adopt organic solvent to process the silica flour in mixture and impurity in prior art, be separated and obtain silicon
Powder and impurity, although can realize being separated of silica flour and impurity, the organic solvent amount consumed is large, and the time of organic solvent process is longer, cause cost higher, and treatment cycle is also longer.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of method of silica flour in mixture and impurity being carried out be separated, after obtaining the organic solvent phase bead of parcel silica flour after silica flour being processed by adopting organic solvent, by strainer, the organic solvent phase bead of this parcel silica flour and impurity are filtered, realize silica flour and magazins' layout, can greatly reduce the separating treatment time, improve processing efficiency, save the usage quantity of organic solvent simultaneously, silica flour in minimizing separating mixture and the cost of impurity, and reduce a large amount of organic solvent of use to the negative impact of environment.
Technical scheme of the present invention is:
Silica flour in mixture and impurity are carried out the method be separated, comprising: pending mixture is placed in the liquid be made up of organic solvent and water, the consumption of water doubly configures by the 20-100 of institute's silicon powder-containing weight in mixture; The consumption of organic solvent doubly configures by the 0.2-4 of institute's silicon powder-containing weight in mixture, the organic solvent adopted by volume: alkane 28-48 part, aromatic hydrocarbons 20-50 part, unsaturated hydrocarbons 1-6 part, cyclic hydrocarbon 17-44 part; Silica flour in mixture enters in organic solvent phase, and organic solvent is completely coated thus form the organic solvent phase bead of parcel silica flour relative to silicon powder particle, obtains the system be made up of the parcel organic solvent phase bead of silica flour, silicon carbide impurity and water; Strainer is adopted to filter the organic solvent phase bead of the parcel silica flour in system and silicon carbide impurity, silicon carbide impurity particle diameter is 0.1-30 μm, the organic solvent phase bead particle diameter of described parcel silica flour is 10mm, the aperture of this strainer is 300 μm, the organic solvent phase pellet of parcel silica flour is retained by the strainer that aperture is 300 μm, silicon carbide impurity is the strainer of 300 μm through aperture with water, realizes the parcel organic solvent phase pellet of silica flour and the initial gross separation of silicon carbide impurity.
After obtaining the organic solvent phase pellet of parcel silica flour, add degreaser and water, the consumption of degreaser doubly configures by the 0.5-2 of institute's silicon powder-containing weight in mixture, the consumption of water doubly configures by the 10-80 of institute's silicon powder-containing weight in mixture, stir, degreaser is formed by the preparation of raw material of following weight proportion: 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, have employed degreaser, parcel between organic solvent and silica flour is balanced upset, effective constituent generation emulsifying effect in organic solvent and degreaser and enter in aqueous phase, and silica flour is water insoluble, with filtration unit, silica flour and the organic solvent entered in aqueous phase are being separated, obtain the silica flour after being separated.
In the present invention, organic solvent is scattered in the aqueous solution containing silica flour under the condition of high-speed stirring, namely realize organic solvent by stirring disperse in aqueous and exist with small droplets form, simultaneously in whipping process, silica flour in the aqueous solution constantly and organic solvent small droplets collide and adsorbed by organic solvent drop, along with the carrying out of this process, increasing silica flour is adsorbed on around drop and forms the large organic solvent phase bead including silica flour.
Principle of work of the present invention: when adopting organic solvent to process the silica flour in mixture and impurity, due to the lipophilicity of silica flour, silica flour will enter into organic solvent mutually, completely coated relative to silicon powder particle of organic solvent can be realized, and insoluble due to organic solvent phase and aqueous phase, and silica flour blocks mutually converging of organic solvent phase and organic solvent phase, thus realize silica flour be distributed in organic solvent mutually in and formed parcel silica flour organic solvent phase bead float on or be scattered in aqueous phase, obtain the organic solvent phase bead wrapping up silica flour, the system of impurity and water composition, utilize the particle diameter of organic solvent phase bead particle diameter much larger than impurity particle of parcel silica flour, aperture is used to be greater than the particle diameter of impurity particle, the strainer being less than the organic solvent phase bead particle diameter of parcel silica flour filters the organic solvent phase bead of the parcel silica flour in system and impurity, silica flour and magazins' layout can be realized, so the separating treatment time can greatly be reduced, also reduce the usage quantity of organic solvent.
Because prior art adopts organic solvent to carry out separating treatment to silica flour and impurity, be the hydrophilic different difference depending on silica flour lipophilicity, impurity, realize being separated completely of silica flour and impurity.Usually, need to add relatively large organic solvent in treating processes, silica flour enters in organic solvent, and impurity is scattered in the aqueous solution, and due to 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, realize the recovery to silica flour, such method need expend the longer treatment time, also needs to expend relatively large organic solvent simultaneously, is unfavorable for applying aborning.
Table 1 the present invention compares with the implementation result of prior art
Advantage of the present invention: after obtaining the organic solvent phase bead of parcel silica flour after silica flour being processed by adopting organic solvent, by strainer, the organic solvent phase bead of this parcel silica flour and impurity are filtered, realize silica flour and magazins' layout, can greatly reduce the separating treatment time, improve processing efficiency, save the usage quantity of organic solvent simultaneously, silica flour in minimizing separating mixture and the cost of impurity, namely time shorter, formed organic phase bead is larger, cost is lower, concerning better purifying silicon powder.And reduce a large amount of organic solvent of use to the negative impact of environment.
Embodiment
Embodiment 1,
Silica flour in mixture and impurity are carried out the method be separated, comprising: pending mixture is placed in the liquid be made up of organic solvent and water, the consumption of water presses 20 times of configurations of institute's silicon powder-containing weight in mixture; The consumption of organic solvent presses 0.2 times of configuration of institute's silicon powder-containing weight in mixture, the organic solvent adopted by volume: hexane 28 parts, propyl benzene 20 parts, 1-butylene 1 part, suberane 17 parts; Silica flour in mixture enters in organic solvent phase, and organic solvent is completely coated thus form the organic solvent phase bead of parcel silica flour relative to silicon powder particle, obtains the system be made up of the parcel organic solvent phase bead of silica flour, silicon carbide impurity and water; Strainer is adopted to filter the organic solvent phase bead of the parcel silica flour in system and silicon carbide impurity, silicon carbide impurity particle diameter is 0.1-30 μm, the organic solvent phase bead particle diameter of described parcel silica flour is 11.3mm, the aperture of this strainer is 300 μm, the organic solvent phase pellet of parcel silica flour is retained by the strainer that aperture is 300 μm, silicon carbide impurity is the strainer of 300 μm through aperture with water, realizes the parcel organic solvent phase pellet of silica flour and the initial gross separation of silicon carbide impurity.
After obtaining the organic solvent phase pellet of parcel silica flour, add degreaser and water, the consumption of degreaser presses 0.5 times of configuration of institute's silicon powder-containing weight in mixture, the consumption of water presses 10 times of configurations of institute's silicon powder-containing weight in mixture, stir, degreaser is formed by the preparation of raw material of following weight proportion: 90 parts, water, fatty alcohol-polyoxyethylene ether 5 parts, tertiary sodium phosphate 1.8 parts, sodium phosphate 2.0 parts, 95% ethanol 1.0 parts, stearylamine 1.5 parts, 0.6 part, sodium hydroxide, with filtration unit, silica flour and the organic solvent entered in aqueous phase are separated again, obtain the silica flour after being separated.
Embodiment 2,
Silica flour in mixture and impurity are carried out the method be separated, comprising: pending mixture is placed in the liquid be made up of organic solvent and water, the consumption of water presses 60 times of configurations of institute's silicon powder-containing weight in mixture; The consumption of organic solvent presses 2.1 times of configurations of institute's silicon powder-containing weight in mixture, the organic solvent adopted by volume: heptane 38 parts, dimethylbenzene 35 parts, 1-nonene 3 parts, tetramethylene 30 parts; Silica flour in mixture enters in organic solvent phase, and organic solvent is completely coated thus form the organic solvent phase bead of parcel silica flour relative to silicon powder particle, obtains the system be made up of the parcel organic solvent phase bead of silica flour, silicon carbide impurity and water; Strainer is adopted to filter the organic solvent phase bead of the parcel silica flour in system and silicon carbide impurity, silicon carbide impurity particle diameter is 0.1-30 μm, the organic solvent phase bead particle diameter of described parcel silica flour is 10.8mm, the aperture of this strainer is 300 μm, the organic solvent phase pellet of parcel silica flour is retained by the strainer that aperture is 300 μm, silicon carbide impurity is the strainer of 300 μm through aperture with water, realizes the parcel organic solvent phase pellet of silica flour and the initial gross separation of silicon carbide impurity.
After obtaining the organic solvent phase pellet of parcel silica flour, add degreaser and water, the consumption of degreaser presses 1.2 times of configurations of institute's silicon powder-containing weight in mixture, the consumption of water presses 45 times of configurations of institute's silicon powder-containing weight in mixture, stir, degreaser is formed by the preparation of raw material of following weight proportion: 95 parts, water, fatty alcohol-polyoxyethylene ether 8 parts, tertiary sodium phosphate 2.4 parts, sodium phosphate 2.5 parts, 95% ethanol 1.5 parts, stearylamine 2.0 parts, 0.8 part, sodium hydroxide, with filtration unit, silica flour and the organic solvent entered in aqueous phase are separated again, obtain the silica flour after being separated.
Embodiment 3,
Silica flour in mixture and impurity are carried out the method be separated, comprising: pending mixture is placed in the liquid be made up of organic solvent and water, the consumption of water presses 100 times of configurations of institute's silicon powder-containing weight in mixture; The consumption of organic solvent presses 4 times of configurations of institute's silicon powder-containing weight in mixture, the organic solvent adopted by volume: octane 48 parts, toluene 50 parts, 1-amylene 6 parts, hexanaphthene 44 parts; Silica flour in mixture enters in organic solvent phase, and organic solvent is completely coated thus form the organic solvent phase bead of parcel silica flour relative to silicon powder particle, obtains the system be made up of the parcel organic solvent phase bead of silica flour, silicon carbide impurity and water; Strainer is adopted to filter the organic solvent phase bead of the parcel silica flour in system and silicon carbide impurity, silicon carbide impurity particle diameter is 0.1-30 μm, the organic solvent phase bead particle diameter of described parcel silica flour is 11.1mm, the aperture of this strainer is 300 μm, the organic solvent phase pellet of parcel silica flour is retained by the strainer that aperture is 300 μm, silicon carbide impurity is the strainer of 300 μm through aperture with water, realizes the parcel organic solvent phase pellet of silica flour and the initial gross separation of silicon carbide impurity.
After obtaining the organic solvent phase pellet of parcel silica flour, add degreaser and water, the consumption of degreaser presses 2 times of configurations of institute's silicon powder-containing weight in mixture, the consumption of water presses 80 times of configurations of institute's silicon powder-containing weight in mixture, stir, degreaser is formed by the preparation of raw material of following weight proportion: 100 parts, water, fatty alcohol-polyoxyethylene ether 10 parts, tertiary sodium phosphate 3.0 parts, sodium phosphate 3.0 parts, 95% ethanol 2.0 parts, stearylamine 2.5 parts, 1.0 parts, sodium hydroxide, with filtration unit, silica flour and the organic solvent entered in aqueous phase are separated again, obtain the silica flour after being separated.
Embodiment 4,
Silica flour in mixture and impurity are carried out the method be separated, comprising: pending mixture is placed in the liquid be made up of organic solvent and water, the consumption of water presses 40 times of configurations of institute's silicon powder-containing weight in mixture; The consumption of organic solvent presses 1.0 times of configurations of institute's silicon powder-containing weight in mixture, the organic solvent adopted by volume: 48 parts, certain herbaceous plants with big flowers alkane, 25 parts, ethylbenzene, 1-hexene 6 parts, cyclooctane 31 parts; Silica flour in mixture enters in organic solvent phase, and organic solvent is completely coated thus form the organic solvent phase bead of parcel silica flour relative to silicon powder particle, obtains the system be made up of the parcel organic solvent phase bead of silica flour, silicon carbide impurity and water; Strainer is adopted to filter the organic solvent phase bead of the parcel silica flour in system and silicon carbide impurity, silicon carbide impurity particle diameter is 0.1-30 μm, the organic solvent phase bead particle diameter of described parcel silica flour is 10.9mm, the aperture of this strainer is 300 μm, the organic solvent phase pellet of parcel silica flour is retained by the strainer that aperture is 300 μm, silicon carbide impurity is the strainer of 300 μm through aperture with water, realizes the parcel organic solvent phase pellet of silica flour and the initial gross separation of silicon carbide impurity.
After obtaining the organic solvent phase pellet of parcel silica flour, add degreaser and water, the consumption of degreaser presses 0.8 times of configuration of institute's silicon powder-containing weight in mixture, the consumption of water presses 20 times of configurations of institute's silicon powder-containing weight in mixture, stir, degreaser is formed by the preparation of raw material of following weight proportion: 90 parts, water, fatty alcohol-polyoxyethylene ether 8 parts, tertiary sodium phosphate 2.0 parts, sodium phosphate 2.2 parts, 95% ethanol 1.3 parts, stearylamine 1.8 parts, 0.8 part, sodium hydroxide, with filtration unit, silica flour and the organic solvent entered in aqueous phase are separated again, obtain the silica flour after being separated.
Embodiment 5,
Silica flour in mixture and impurity are carried out the method be separated, comprising: pending mixture is placed in the liquid be made up of organic solvent and water, the consumption of water presses 90 times of configurations of institute's silicon powder-containing weight in mixture; The consumption of organic solvent presses 3.5 times of configurations of institute's silicon powder-containing weight in mixture, the organic solvent adopted by volume: dodecane 42 parts, butylbenzene 38 parts, 1-heptene 6 parts, pentamethylene 44 parts; Silica flour in mixture enters in organic solvent phase, and organic solvent is completely coated thus form the organic solvent phase bead of parcel silica flour relative to silicon powder particle, obtains the system be made up of the parcel organic solvent phase bead of silica flour, silicon carbide impurity and water; Strainer is adopted to filter the organic solvent phase bead of the parcel silica flour in system and silicon carbide impurity, silicon carbide impurity particle diameter is 0.1-30 μm, the organic solvent phase bead particle diameter of described parcel silica flour is 10.7mm, the aperture of this strainer is 300 μm, the organic solvent phase pellet of parcel silica flour is retained by the strainer that aperture is 300 μm, silicon carbide impurity is the strainer of 300 μm through aperture with water, realizes the parcel organic solvent phase pellet of silica flour and the initial gross separation of silicon carbide impurity.
After obtaining the organic solvent phase pellet of parcel silica flour, add degreaser and water, the consumption of degreaser presses 1.8 times of configurations of institute's silicon powder-containing weight in mixture, the consumption of water presses 70 times of configurations of institute's silicon powder-containing weight in mixture, stir, degreaser is formed by the preparation of raw material of following weight proportion: 98 parts, water, fatty alcohol-polyoxyethylene ether 10 parts, tertiary sodium phosphate 2.8 parts, sodium phosphate 2.9 parts, 95% ethanol 1.8 parts, stearylamine 2.2 parts, 0.9 part, sodium hydroxide, with filtration unit, silica flour and the organic solvent entered in aqueous phase are separated again, obtain the silica flour after being separated.
Embodiment 6,
Silica flour in mixture and impurity are carried out the method be separated, comprising: pending mixture is placed in the liquid be made up of organic solvent and water, the consumption of water presses 15 times of configurations of institute's silicon powder-containing weight in mixture; The consumption of organic solvent presses 5 times of configurations of institute's silicon powder-containing weight in mixture, the organic solvent adopted by volume: heptane 12 parts, dimethylbenzene 53 parts, tetramethylene 10 parts; Silica flour in mixture enters in organic solvent phase, and organic solvent is completely coated thus form the organic solvent phase bead of parcel silica flour relative to silicon powder particle, obtains the system be made up of the parcel organic solvent phase bead of silica flour, silicon carbide impurity and water; Strainer is adopted to filter the organic solvent phase bead of the parcel silica flour in system and silicon carbide impurity, silicon carbide impurity particle diameter is 0.1-30 μm, the organic solvent phase bead particle diameter of described parcel silica flour is 7.5mm, the aperture of this strainer is 300 μm, the organic solvent phase pellet of parcel silica flour is retained by the strainer that aperture is 300 μm, silicon carbide impurity is the strainer of 300 μm through aperture with water, realizes the parcel organic solvent phase pellet of silica flour and the initial gross separation of silicon carbide impurity.
After obtaining the organic solvent phase pellet of parcel silica flour, add degreaser and water, the consumption of degreaser presses 0.4 times of configuration of institute's silicon powder-containing weight in mixture, the consumption of water presses 85 times of configurations of institute's silicon powder-containing weight in mixture, stir, degreaser is formed by the preparation of raw material of following weight proportion: 80 parts, water, fatty alcohol-polyoxyethylene ether (AEO7) 10 parts, tertiary sodium phosphate 3.5 parts, sodium phosphate 3.5 parts, 95% ethanol 0.8 part, stearylamine 1.2 parts, 1.2 parts, sodium hydroxide, have employed degreaser, parcel between organic solvent and silica flour is balanced upset, effective constituent generation emulsifying effect in organic solvent and degreaser and enter in aqueous phase, and silica flour is water insoluble, with filtration unit, silica flour and the organic solvent entered in aqueous phase are being separated, obtain the silica flour after being separated.
The effect of each embodiment is as shown in the table:
As can be seen from upper table data, embodiment 1-5 invention step within the scope of the technology of the present invention repeats can obtain the silica flour that purity is more than 99% respectively 2-3 time, especially can obtain with embodiment 1 silica flour that purity is 99.6%, but embodiment 6 have to purity be the silica flour of 80.3%; The organic solvent amount that embodiment 1-5 is used is simultaneously also less compared to embodiment 6, the organic solvent phase bead particle diameter of parcel silica flour is larger, the required treatment time is shorter, especially minimum with the organic solvent amount of embodiment 1, the organic solvent phase bead particle diameter of parcel silica flour is maximum, and the required treatment time is also the shortest; Therefore the present invention not only achieves being separated of silica flour and impurity, also greatly reduce the separating treatment time, improve processing efficiency, save the usage quantity of organic solvent simultaneously, silica flour in minimizing separating mixture and the cost of impurity, namely time shorter, formed organic phase bead is larger, cost is lower, concerning better purifying silicon powder, and reduce and uses a large amount of organic solvent to the negative impact of environment.
Be separated simultaneously the purity obtained be 99% silica flour can obtain the higher silica flour of purity further by the happy and harmonious mode of high temperature of conventional silica flour ingot casting, because most silicon carbide is removed, the happy and harmonious mode of high temperature that remaining non-silicon carbide impurity is 20 hours by the cycle also can obtain good removal, obtain the higher silica flour of purity to be like this expected to enter sun power ingot casting field as raw material, substantially increase the value of recovery.
Claims (1)
1. silica flour in mixture and impurity are carried out the method be separated, it is characterized in that: pending mixture is placed in the liquid be made up of organic solvent and water, the consumption of water presses 20 times of configurations of institute's silicon powder-containing weight in mixture; The consumption of organic solvent presses 0.2 times of configuration of institute's silicon powder-containing weight in mixture, the organic solvent adopted by volume: hexane 28 parts, propyl benzene 20 parts, 1-butylene 1 part, suberane 17 parts; Silica flour in mixture enters in organic solvent phase, and organic solvent is completely coated thus form the organic solvent phase bead of parcel silica flour relative to silicon powder particle, obtains the system be made up of the parcel organic solvent phase bead of silica flour, silicon carbide impurity and water; Strainer is adopted to filter the organic solvent phase bead of the parcel silica flour in system and silicon carbide impurity, silicon carbide impurity particle diameter is 0.1-30 μm, the organic solvent phase bead particle diameter of described parcel silica flour is 11.3mm, the aperture of this strainer is 300 μm, the organic solvent phase pellet of parcel silica flour is retained by the strainer that aperture is 300 μm, silicon carbide impurity is the strainer of 300 μm through aperture with water, realizes the parcel organic solvent phase pellet of silica flour and the initial gross separation of silicon carbide impurity;
Organic solvent is scattered in the aqueous solution containing silica flour under the condition of high-speed stirring, namely realize organic solvent by stirring disperse in aqueous and exist with small droplets form, simultaneously in whipping process, silica flour in the aqueous solution constantly and organic solvent small droplets collide and adsorbed by organic solvent drop, along with the carrying out of this process, increasing silica flour is adsorbed on around drop and forms the large organic solvent phase bead including silica flour;
After obtaining the organic solvent phase pellet of parcel silica flour, add degreaser and water, the consumption of degreaser presses 0.5 times of configuration of institute's silicon powder-containing weight in mixture, the consumption of water presses 10 times of configurations of institute's silicon powder-containing weight in mixture, stir, degreaser is formed by the preparation of raw material of following weight proportion: 90 parts, water, fatty alcohol-polyoxyethylene ether 5 parts, tertiary sodium phosphate 1.8 parts, sodium phosphate 2.0 parts, 95% ethanol 1.0 parts, stearylamine 1.5 parts, 0.6 part, sodium hydroxide, with filtration unit, silica flour and the organic solvent entered in aqueous phase are separated again, obtain the silica flour after being separated.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310324443.1A CN103342364B (en) | 2013-07-30 | 2013-07-30 | A kind of method of silica flour in mixture and impurity being carried out be separated |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310324443.1A CN103342364B (en) | 2013-07-30 | 2013-07-30 | A kind of method of silica flour in mixture and impurity being carried out be separated |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103342364A CN103342364A (en) | 2013-10-09 |
| CN103342364B true CN103342364B (en) | 2016-02-03 |
Family
ID=49277207
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310324443.1A Expired - Fee Related CN103342364B (en) | 2013-07-30 | 2013-07-30 | A kind of method of silica flour in mixture and impurity being carried out be separated |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103342364B (en) |
Citations (4)
| 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 |
| 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 |
-
2013
- 2013-07-30 CN CN201310324443.1A patent/CN103342364B/en not_active Expired - Fee Related
Patent Citations (4)
| 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103342364A (en) | 2013-10-09 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108328761A (en) | MTO washes the method and device of hydraulic art continuous operation cycle stretch-out | |
| CN103657199A (en) | Multilayer filter | |
| TW201040109A (en) | Recovery of silicon and silicon carbide powder from kerf loss slurry using particle phase-transfer method | |
| CN104028250A (en) | Filtering medium for removing aluminum in drinking water, filter element and method for preparing filtering medium | |
| CN107779258A (en) | The preparation method of low arsenic content krill oil | |
| CN104437822A (en) | C-SiC micro powder separating method | |
| CN103980096B (en) | Extractive distillation with salt is separated the method for methyl tertiary butyl ether and methylene dichloride | |
| CN205099601U (en) | System for hydrogenation device and production hydrogen peroxide | |
| CN103342364B (en) | A kind of method of silica flour in mixture and impurity being carried out be separated | |
| CN101823716A (en) | Method for separating silica powder and impurities in mixture | |
| CN107935578A (en) | Bacteriostasis antibiosis ceramic element | |
| CN105664845B (en) | It is a kind of to be used to adsorb compound adsorbent of rubidium ion and its preparation method and application | |
| CN110467445A (en) | A kind of graphene Ceramic Composite filter core and preparation method thereof | |
| CN103272564B (en) | Method for rapidly preparing efficient adsorbent with low cost by adopting organosilicone high-boiling residue | |
| CN102079883B (en) | Novel process for extracting capsanthin and chilli extract by composite solvent | |
| CN204686671U (en) | The abradant lapping liquid retracting device of a kind of silicon single crystal flake | |
| CN202246100U (en) | Trichlorosilane separating and purifying system in polysilicon production process | |
| CN202655030U (en) | Preparation kettle with filter screen cylinder | |
| CN107158798A (en) | One kind removes DEHP filter mediums, filter core and preparation method in drinking water | |
| Pathak et al. | Green synthesis of Pd@ rGO nanocomposite using Piper (Piper nigrum) leaf extract and its catalytic activity towards alcohol oxidation in water at room temperature | |
| CN105689153A (en) | High-selectivity flotation solvent for separating silicon carbide and silicon | |
| CN206214896U (en) | Extractant recycle device in a kind of polymethoxy dimethyl ether synthesis | |
| CN203030042U (en) | Oil-water separator filter element | |
| CN202762213U (en) | Novel oil-water separation device with inorganic ceramic membrane | |
| CN221332794U (en) | Preparation system of high-purity tetra (dimethylamino) titanium |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20160203 |