CN101983919A - Method for producing white carbon black by polycrystalline silicon cut waste alkali-wash waste water - Google Patents
Method for producing white carbon black by polycrystalline silicon cut waste alkali-wash waste water Download PDFInfo
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- CN101983919A CN101983919A CN 201010556239 CN201010556239A CN101983919A CN 101983919 A CN101983919 A CN 101983919A CN 201010556239 CN201010556239 CN 201010556239 CN 201010556239 A CN201010556239 A CN 201010556239A CN 101983919 A CN101983919 A CN 101983919A
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- waste water
- water
- alkali cleaning
- carbon black
- white carbon
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 115
- 239000002351 wastewater Substances 0.000 title claims abstract description 78
- 229910021420 polycrystalline silicon Inorganic materials 0.000 title claims abstract description 67
- 239000002699 waste material Substances 0.000 title claims abstract description 48
- 239000006229 carbon black Substances 0.000 title claims abstract description 38
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 19
- 239000007787 solid Substances 0.000 claims abstract description 126
- 238000004140 cleaning Methods 0.000 claims abstract description 69
- 239000004576 sand Substances 0.000 claims abstract description 44
- 238000000034 method Methods 0.000 claims abstract description 40
- 239000007788 liquid Substances 0.000 claims abstract description 21
- 238000000498 ball milling Methods 0.000 claims abstract description 16
- 239000002245 particle Substances 0.000 claims abstract description 16
- 238000007710 freezing Methods 0.000 claims abstract description 8
- 230000008014 freezing Effects 0.000 claims abstract description 8
- 238000000926 separation method Methods 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 128
- 239000003513 alkali Substances 0.000 claims description 77
- 229920005591 polysilicon Polymers 0.000 claims description 61
- 238000005520 cutting process Methods 0.000 claims description 46
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 27
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 27
- 239000002002 slurry Substances 0.000 claims description 22
- 239000004033 plastic Substances 0.000 claims description 18
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 15
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 15
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims description 14
- 239000003729 cation exchange resin Substances 0.000 claims description 14
- 238000001914 filtration Methods 0.000 claims description 14
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 12
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 10
- 239000000126 substance Substances 0.000 claims description 10
- 230000001105 regulatory effect Effects 0.000 claims description 9
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 8
- 239000004744 fabric Substances 0.000 claims description 8
- 239000000919 ceramic Substances 0.000 claims description 7
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 6
- 235000019253 formic acid Nutrition 0.000 claims description 6
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 5
- 230000002378 acidificating effect Effects 0.000 claims description 5
- 239000000908 ammonium hydroxide Substances 0.000 claims description 5
- 229910017604 nitric acid Inorganic materials 0.000 claims description 5
- 125000001453 quaternary ammonium group Chemical group 0.000 claims description 5
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 4
- 239000005357 flat glass Substances 0.000 claims description 4
- 238000012856 packing Methods 0.000 claims description 4
- 238000005554 pickling Methods 0.000 claims description 4
- 229910001220 stainless steel Inorganic materials 0.000 claims description 4
- 239000010935 stainless steel Substances 0.000 claims description 4
- 239000004568 cement Substances 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 239000013618 particulate matter Substances 0.000 claims description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 claims description 2
- 230000015572 biosynthetic process Effects 0.000 claims description 2
- 230000008021 deposition Effects 0.000 claims description 2
- 238000005507 spraying Methods 0.000 claims description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 17
- 229910052710 silicon Inorganic materials 0.000 abstract description 11
- 239000010703 silicon Substances 0.000 abstract description 11
- 238000011084 recovery Methods 0.000 abstract description 6
- 239000004615 ingredient Substances 0.000 abstract description 5
- 238000010257 thawing Methods 0.000 abstract description 5
- 239000008346 aqueous phase Substances 0.000 abstract description 3
- LRCFXGAMWKDGLA-UHFFFAOYSA-N dioxosilane;hydrate Chemical compound O.O=[Si]=O LRCFXGAMWKDGLA-UHFFFAOYSA-N 0.000 abstract 1
- 238000007598 dipping method Methods 0.000 abstract 1
- 239000002244 precipitate Substances 0.000 abstract 1
- 229960004029 silicic acid Drugs 0.000 abstract 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 27
- 239000000243 solution Substances 0.000 description 24
- 235000019241 carbon black Nutrition 0.000 description 23
- 239000000203 mixture Substances 0.000 description 20
- 239000002253 acid Substances 0.000 description 17
- 239000000377 silicon dioxide Substances 0.000 description 16
- 238000001816 cooling Methods 0.000 description 14
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 14
- 229910010271 silicon carbide Inorganic materials 0.000 description 14
- 235000012239 silicon dioxide Nutrition 0.000 description 14
- 229960001866 silicon dioxide Drugs 0.000 description 14
- 238000003756 stirring Methods 0.000 description 14
- 235000011167 hydrochloric acid Nutrition 0.000 description 13
- 235000019353 potassium silicate Nutrition 0.000 description 13
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 13
- 238000006243 chemical reaction Methods 0.000 description 12
- 239000011734 sodium Substances 0.000 description 12
- 229910052742 iron Inorganic materials 0.000 description 11
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 11
- 239000006210 lotion Substances 0.000 description 9
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 7
- 239000011863 silicon-based powder Substances 0.000 description 6
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 6
- 229910001948 sodium oxide Inorganic materials 0.000 description 6
- 229910004298 SiO 2 Inorganic materials 0.000 description 5
- 239000003595 mist Substances 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 238000004062 sedimentation Methods 0.000 description 5
- 239000007864 aqueous solution Substances 0.000 description 4
- 238000005119 centrifugation Methods 0.000 description 4
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 238000007654 immersion Methods 0.000 description 3
- 229910001415 sodium ion Inorganic materials 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 238000006418 Brown reaction Methods 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 1
- 239000003082 abrasive agent Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 238000005056 compaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000010612 desalination reaction Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 244000144992 flock Species 0.000 description 1
- 150000004674 formic acids Chemical class 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
Landscapes
- Processing Of Solid Wastes (AREA)
Abstract
The invention discloses a method for producing white carbon black by polycrystalline silicon cut waste alkali-wash waste water, which not only can economically and reliably utilize silicon contents contained in alkaline waste water generated by chemically cleaning polycrystalline silicon cut waste but also can realize the zero emission of alkaline waste water and complete recovery of effective ingredients. The method comprises the following steps: (1) adjusting the pH of the alkaline waste water to 7.0-11.1; (2) removing a small quantity of suspended solid or precipitate by using a solid-liquid separation method; (3) freezing processed alkaline waste water into glacial solid, then thawing, and separating hydrated silica contained in waste water from aqueous phase in the mode of sand particles with the size of 0.05-4 mm; (4) dipping the sand particles, and washing for 3-6 times; and (5) drying the dipped and washed sand particles for 12-36 hours at the temperature of 100-110 DEG C to obtain dry sand solid particles, carrying out ball milling and obtaining the white carbon black.
Description
Technical field
The present invention relates to polysilicon cutting waste material reutilization technology field, particularly a kind of method of utilizing the white carbon black of polysilicon cutting waste material alkali cleaning waste water production.
Background technology
In recent decades, solar cell industry development rapidly, it is not poor to realize that with multiple material the solar cell layer of opto-electronic conversion goes out, wherein with polysilicon solar cell with the fastest developing speed in more than ten years recently.At present, China has become the big producing country of polysilicon solar cell, and the annual polysilicon that consumes of the production of the needed polysilicon chip of polysilicon solar cell reaches more than 100,000 tons.
Polysilicon chip is to utilize polycrystalline silicon rod the method for line cutting to process.Wire cutting method be to use 1200 orders with thin superfine silicon carbide powder as abrasive material, earlier silicon carbide abrasive and cutting liquid are allocated the slurry that becomes good fluidity, then this slurry is drenched on the iron wire line of high-speed straight-line motion, polycrystalline silicon rod is cut and obtains polysilicon chip.With the carrying out of line cutting, iron filings in the slurry and silicon bits increase gradually, owing to wear and tear, some silicon carbide abrasive particulate sharpness also descend simultaneously, and the factor of this two aspect all makes cutting power descend the cutting quality variation.So behind the polysilicon chip that cuts out some amount, slurry must be changed, the slurry that use preparation again instead could continue cutting.Used not reusable slurry to be called the polysilicon cutting waste liquor in industry.Wherein contain following several composition: silicon-carbide particle, iron filings, polysilicon bits, polysilicon micro mist, cutting liquid, ferric oxide, silicon-dioxide, impurity and a spot of water.Wherein, iron filings and polysilicon bits, polysilicon micro mist grind from iron wire line and polycrystalline silicon rod respectively, silicon-dioxide is silicon bits, the oxidized generation of silicon powder, ferric oxide is the oxidized generations of iron filings, impurity is the unexpected foreign matter that enters in producing, and a spot of water is absorbed from air by hydrophilic cutting liquid.
The annual polysilicon cutting waste slurry few hundred thousand tonnes of that produces of present national polysilicon solar cell silicon chip industry effluxes if directly abandon, not only can serious environment pollution, also can cause the huge wasting of resources.All to obtain purified cutting liquid and silicon carbide abrasive and return the production repeated use of polysilicon cutting factory at present through handling.Specifically the flow process of recovery polysilicon cutting waste slurry roughly like this: first solid-liquid separation, dehydration, decolouring, take off foreign ion, obtain clean available and reclaim cutting liquid, the solid slag that solid-liquid separation produces is the diffusing shape pug of a kind of hygrometric state of approximate black, i.e. polysilicon cutting waste material.Kept all solids composition in the polysilicon cutting waste slurry in the polysilicon cutting waste material.Overall estimation, the carborundum content in the polysilicon cutting waste material is 40～60wt%, polysilicon micro mist and silica 1 0～20wt%, irony composition are less than 10wt%, about moisture 15wt%.
The waste recovery of polysilicon cutting at present industry all is to use the method for matting, promptly add the method that acid-respons (being pickling) He Jiashui adds alkali reaction (being alkali cleaning) and remove de-iron, ferric oxide composition and polysilicon bits, polysilicon micro mist, silicon-dioxide respectively with adding water respectively, all will make water come rinsing after pickling, the alkali cleaning.Wherein, contain water glass, hydrated SiO 2 and unnecessary alkali (as sodium hydroxide) in the rinse water after alkali cleaning water and the alkali cleaning, water glass, hydrated SiO 2 are that silicon powder and alkali reaction generation are considered, tasted with discrimination more to the silicon in many product silicon cutting waste materials to be worth doing.Can only accomplish cutting liquid and silicon carbide recycling in the industry at present, and a large amount of water glass, the hydrated SiO 2 that contain in the alkali cleaning waste water that matting cutting waste material produces are not used, waste water filters the back discharging through simple neutralization, exist serious environmental to pollute, water glass wherein, hydrated SiO 2 can cause soil compaction and can not cultivate.
From the alkali cleaning waste water that polysilicon cutting waste recovery process produces, recycle siliceous composition, not only can reduce environmental pollution, also have very big economic worth.At present polysilicon reclaims industry and is badly in need of a kind of method that can recycle siliceous composition from polysilicon cuts the alkali cleaning waste water of waste material.
Summary of the invention
The object of the present invention is to provide a kind of economy, utilize polysilicon to cut the method for the white carbon black of waste material alkali cleaning waste water production reliably, it can not only realize the effective utilization to the siliceous composition the alkaline waste water that cleans from polysilicon cutting waste chemistry, and, can further purify alkali cleaning waste water, make it to become the alkalescent water of saliferous and small amount of alkali, finally realize the zero release of alkali cleaning waste water and the recovery fully of effective constituent.
Technical solution proposed by the invention is such:
A kind of method of utilizing the white carbon black of polysilicon cutting waste material alkali cleaning waste water production, this alkali cleaning waste water contain a kind of in sodium hydroxide, potassium hydroxide and the quaternary ammonium hydroxide, and the step of its method is:
(1) polysilicon being cut waste material uses chemical cleaning method to reclaim and the alkali cleaning waste water that obtains is adjusted to pH=7.0～11.1;
The small amount of solid suspended substance or the throw out that can produce when (2) the alkali cleaning waste water after the above-mentioned pH of the regulating value is removed adjusting pH value by solid-liquid separating method;
(3) the low temperature resistant container of packing into of the alkali cleaning waste water after handling with the above-mentioned pH of regulating value and through solid-liquid separating method is placed on that low temperature environment is freezing ices the shape solid to freezing fully to become, should ice the shape solid then shifts out and thaws, thaw finish after, the bottom of container is the deposition of solids layer that one deck is of a size of 0.05～4 millimeter sand shape particle packing formation, and the upper strata is a water;
(4) with above-mentioned sand shape granular deposit and the aqueous phase separation that obtains, solid-liquid separation is soaked again after then the sand shape granular deposit being soaked in water 2～36 hours, washes for 3～6 times repeatedly, obtains the sand shape solid particulate; The sand shape solid particulate adopts tipping to separate with water, and the water on upper strata is toppled over away, obtains the sand shape solid particulate of lower floor;
(5) above-mentioned washing is good sand shape solid particulate was 100～110 ℃ of bakings 12～36 hours, and the exsiccant sand shape solid particulate that obtains obtains white carbon black, i.e. the soft silica superfine powder through dry ball milling.
Ice shape solid shifts out also can be placed on the porous water filtration object behind the low temperature environment and thaws, ice shape solid thaws on one side, the water that produces is filtered away on one side, thaws directly to obtain the sand shape solid particulate after finishing, and this porous water filtration object is a kind of among filter cloth, porous ceramic plate, the screen cloth.Ice shape solid shifts out also can be placed on the flat board behind the low temperature environment and thaws, ice shape solid thaws on one side, the water that produces flows away on one side, thawing directly obtains the sand shape solid particulate after finishing, and this flat board is a kind of among sheet glass, ceramic of compact plate, stainless steel plate, plank, cement plate, plastic plate, the rubber plate.
Contained alkaline matter depends on the kind of the alkali that uses in the described alkaline waste water when alkali cleaning polysilicon waste material, is generally a kind of in sodium hydroxide, potassium hydroxide, the quaternary ammonium hydroxide.Described quaternary ammonium hydroxide is meant that molecular formula is R
4The compounds of NOH, wherein R is that chemical formula is C
nH
2n+1Alkyl, n=1～4.
The method of described adjusting alkali cleaning waste water ph is to add the polysilicon waste material to clean the not fluoride of generation and/or the acid waste water of hydrofluoric acid in described alkali cleaning waste water.
The method of described adjusting alkaline waste water pH value can also be one or more the combination that adds in described alkali cleaning waste water among acidic cation-exchange resin, hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, acetate, the formic acid, adds this resin to be leached after acidic cation-exchange resin regulates the pH value.
The method of regulating alkaline waste water pH has determined the solute species and the content of upper strata aqueous phase behind the above-mentioned freeze-thaw.When using acidic cation-exchange resin to turn down the pH value, contain the sodium hydroxide and the water glass of trace in the water that produces after ice shape solid thaws, the content of sodium hydroxide and water glass is relevant with the height of pH value, and the low more then content of pH value is low more.When using acid waste water or directly add acid when turning down the pH value, mainly contain sodium salt and a certain amount of water glass of respective acids in the water layer after thawing, the low more then water glass of pH value content is low more, and correspondingly, salts contg is high more.
The sedimental composition of solid particulate that container lower floor produces after thawing mainly is silicon-dioxide and a small amount of sodium ion, and internal capillary contains moisture.Sodium ions content in the solid particulate settling is relevant with above-mentioned freezing preceding pH value of regulating, and freezing preceding pH value of regulating is low more, and the sodium ions content in the silicon-dioxide sand shape settling that obtains is low more.When regulating pH value=11.1, the silicon-dioxide sand shape settling that obtains is about 5wt% through 100～110 ℃ of sodium oxide contents after drying by the fire 12～36 hours, detects water glass in the water that obtains that thaws simultaneously; Adjusting pH value=10 o'clock, the silicon-dioxide sand shape settling that obtains is about 2wt% through the sodium oxide content of 100～110 ℃ of bakings after 12～36 hours, can not detect water glass in the water that obtains that thaws simultaneously; Adjusting pH value=8.5 o'clock, the silicon-dioxide sand shape settling that obtains is about 1wt% through the sodium oxide content of 100～110 ℃ of bakings after 12～36 hours, can not detect water glass in the water that obtains that thaws simultaneously; Adjusting pH value=7.0 o'clock, the silicon-dioxide sand shape settling that obtains is about 0.2wt% through the sodium oxide content of 100～110 ℃ of bakings after 12～36 hours, can not detect water glass in the water that obtains that thaws.If the silicon-dioxide sand shape settling that obtains is dry again after with the abundant rinsing of pure water, the sodium oxide content of the silica dioxide granule that obtains can be reduced to about 0.1wt%, if with the aqueous hydrochloric acid rinsing of pH=1, can will be reduced to about 0.01wt% with method dried silicon dioxide particulate sodium oxide content.
The water that described water-washing step uses is pure water, or for containing one or more the aqueous solution of combination among hydrochloric acid, sulfuric acid, phosphoric acid, nitric acid, acetate, the formic acid.
Described washing wet solid particulate matter clean and that solid-liquid separation obtains also can directly carry out wet ball grinding, and the slurry that obtains carries out spraying drying, makes white carbon black.
Compared with prior art, the present invention has following unusual effect:
By to carrying out freezing and the processing of thawing through the alkali cleaning waste water after adjusting of pH value and the solid-liquid separation, from alkali cleaning waste water, directly remove siliceous composition, come out with the isolated in form of silicon-dioxide, finally make white carbon black.Like this, not only realized the effective utilization utilization of the polysilicon micro mist in the polysilicon cutting waste slurry and silicon bits, silicon-dioxide (just to) to the siliceous composition in the alkali cleaning waste water, and further purified alkali cleaning waste water, make the alkali cleaning waste water of composition relative complex be transformed into the single relatively saliferous alkalescent water of composition.This weakly alkaline waste water is through neutralizing treatment, can utilize the triple effect thin-film evaporator realize desalination obtain can reuse distilled water and Industrial Salt, thereby realize the zero release of alkali cleaning waste water and the recovery fully of useful component.If do not remove siliceous compositions such as water glass, hydrated SiO 2 in the alkali cleaning waste water, then, so just can not effectively, thoroughly realize separately recycling of evaporation concentration and various useful components owing to the multiviscosisty phenomenon that viscosity increases in the middle of heating, evaporation, concentration process, can occur.
The kind that contains alkali in the alkali cleaning waste water depends on the kind of the alkali that the alkali cleaning link is used, except sodium hydroxide, can also use potassium hydroxide and quaternary ammonium hydroxide such as Tetramethylammonium hydroxide, the alkali cleaning waste water that obtains also can reclaim siliceous composition according to method of the present invention fully and obtain white carbon black.
Present method is by reclaiming the siliceous composition in the polysilicon cutting waste slurry, is used for a large amount of white carbon blacks (silicon-dioxide superfine powder) that use in the manufacture, turns waste into wealth, and has the great environmental protection and the double meaning of economic aspect.
Key equipment used in the present invention is the ripe conventional equipment that uses in the present industrial production for producing the refrigerating apparatus of low temperature environment, and therefore technology of the present invention is highly susceptible to promoting the use of.
Embodiment
By following embodiment the present invention is further elaborated.
Embodiment 1
Get 1000 gram polysilicon cutting waste materials, chemical ingredients is roughly by weight percentage: 15wt% moisture, 60wt% silicon carbide, 18wt% silicon powder and silicon bits, iron and ferric oxide 6wt%, other compositions 1wt%; 1000 gram polysilicon cutting waste materials are added 1000 grams contain the aqueous hydrochloric acid that HCl concentration is 15wt%, stirring reaction 24 hours, the slurry that obtains is placed in the centrifuge tube to handle with whizzer makes the solid matter sedimentation, the reddish-brown iron-containing liquor on centrifuge tube upper strata is inclined to, lower floor's solid matter takes out and adds 1000 gram water stirrings 30 minutes, carrying out centrifugal settling again handles, wash so repeatedly five times, the solid settlement thing that obtains is washed pH=6.8 (reddish-brown reaction soln and follow-up sour water washing lotion are acid waste water).Above-mentioned process added acid-respons and wash and add 1000 gram water near the neutral solid matter and stir and become slurries, add 14 gram sodium hydroxide then, stirring reaction 24 hours, the slurry that obtains is placed in the centrifuge tube to handle with whizzer makes the solid matter sedimentation, the solution on centrifuge tube upper strata is inclined to and keep, lower floor's solid matter takes out and adds 1000 gram water stirrings 30 minutes, carrying out centrifugal settling again handles, wash so repeatedly five times (and keeping water lotion), the solid settlement thing that obtains is washed pH=7.5, oven dry just obtains reclaiming silicon carbide abrasive, the alkali reaction solution that centrifugation is gone out and follow-up each time water lotion are collected and are mixed, and are exactly the alkali cleaning waste water of polysilicon waste material.
Above-mentioned alkali cleaning waste water filtering is removed a small amount of suspended substance, with this Zeo-karb of filtering behind the storng-acid cation exchange resin adjusting pH=11.1, the solution that obtains is put into plastic containers and is built in the reach in freezer internal cooling to becoming ice shape solid fully, should ice the shape solid then together shifts out together with container and thaws, wait to thaw finish after, container bottom forms one deck size at about 50 grams of 0.05～4 millimeter sand shape solid particulate settling, and the container upper strata is a water.The water on upper strata is inclined to, obtain the sand shape solid particulate.The aqueous hydrochloric acids that this solid particulate is added 1000 gram pH=1 soak and change pure water after 2 hours and soak, soak altogether and change water 6 times, the solid particulate that obtains 100 ℃ of bakings after 36 hours dry ball milling obtain white carbon black, Na
2O content is 0.1wt%.
Embodiment 2
The alkali cleaning waste water that embodiment 1 is obtained is adjusted to this Zeo-karb of filtering behind the pH=10 with storng-acid cation exchange resin, the solution that obtains is put into plastic containers and is built in the reach in freezer internal cooling to becoming ice shape solid fully, should ice the shape solid then and take out to be placed on the porous ceramic plate and thaw, waiting to thaw obtains a pile size at about 60 grams of 0.05～4 millimeter sand shape solid particulate matter after finishing.This solid particulate is put into container, and the aqueous hydrochloric acids that add 1000 gram pH=1 soak and change pure water after 36 hours and soak, soak altogether and change water 3 times, the solid particulate that obtains 105 ℃ of bakings after 24 hours dry ball milling obtain white carbon black, Na
2O content is 0.01wt%.
Embodiment 3
The alkali cleaning waste water that embodiment 1 is obtained is adjusted to this Zeo-karb of filtering behind the pH=8.5 with storng-acid cation exchange resin, with hydrochloric acid the pH value is turned down 7.0 again, the solution that obtains is put into plastic containers and is built in the reach in freezer internal cooling to becoming ice shape solid fully, should ice the shape solid then takes out to be placed on the filter cloth and thaws, wait to thaw finish after, obtain on the filter cloth a pile particle size 0.05～4 millimeter sand shape solid particulate about 60 the gram.This solid particulate is put into container, the aqueous solution (the pH value is regulated with 1: 1 sulfuric acid, hydrochloric acid mixture) that adds 1000 gram pH=1 soaks after 8 hours and changes the pure water immersion, soak altogether and change water 5 times, the solid particulate that obtains 105 ℃ of bakings after 24 hours dry ball milling obtain white carbon black, Na
2O content is 0.01wt%.
Embodiment 4
The alkali cleaning waste water that embodiment 1 is obtained is adjusted to this Zeo-karb of filtering behind the pH=8.5 with storng-acid cation exchange resin, the solution that obtains is put into plastic containers and is built in the reach in freezer internal cooling to becoming ice shape solid fully, should ice the shape solid then takes out to be placed on the screen cloth and thaws, wait to thaw finish after, obtain on the screen cloth a pile particle size 0.05～4 millimeter sand shape solid about 60 the gram.This solid particulate is put into container, and the aqueous hydrochloric acids that add 1000 gram pH=1 soak and change pure water after 16 hours and soak, soak altogether and change water 4 times, the solid particulate that obtains 110 ℃ of bakings after 12 hours dry ball milling obtain white carbon black, Na
2O content is 0.01wt%.
Embodiment 5
The alkali cleaning waste water that embodiment 1 is obtained is adjusted to pH=10.5 with hydrochloric acid, the solution that obtains is put into plastic containers and is built in the reach in freezer internal cooling to becoming ice shape solid fully, should ice the shape solid then takes out to be placed on the sheet glass and thaws, wait to thaw and finish, after water drops down and does, obtain a pile particle size on the sheet glass at about 60 grams of 0.05～4 millimeter sand shape solid particulate settling.This solid particulate is put into container, the pure water immersion is changed in mixed acid aqueous solution (with hydrochloric acid, sulfuric acid, phosphoric acid by 1: 1: the 1 composite mixing acid for adjusting pH value) immersion that adds 1000 gram pH=1 after 24 hours, soak altogether and change water 5 times, the hygrometric state solid particulate that obtains behind the filtering water and the water of homogenous quantities obtained white carbon black, Na in 24 hours 105 ℃ of bakings after mixing the back wet ball grinding
2O content is 0.01wt%.
Embodiment 6
The alkali cleaning waste water that embodiment 1 is obtained is adjusted to pH=10 with sulfuric acid, the solution that obtains is put into plastic containers and is built in the reach in freezer internal cooling to becoming ice shape solid fully, should ice the shape solid then takes out to be placed on the ceramic of compact plate and thaws, wait to thaw and finish, after water drops down and does, obtain a pile particle size on the ceramic of compact plate at about 60 grams of 0.05～4 millimeter sand shape solid.This solid particulate is put into container, and the aqueous formic acids that add 1000 gram pH=1 soak and change pure water after 24 hours and soak, soak altogether and change water 5 times, the solid particulate that obtains 110 ℃ of bakings after 36 hours dry ball milling obtain white carbon black, Na
2O content is 0.01wt%.
Embodiment 7
The alkali cleaning waste water that embodiment 1 is obtained is adjusted to pH=10 with phosphoric acid, be adjusted to pH=8.5 with acetate again, the solution that obtains is put into plastic containers and is built in the reach in freezer internal cooling to becoming ice shape solid fully, should ice the shape solid then takes out to be placed on the stainless steel plate and thaws, wait to thaw and finish, after water drops down and does, obtain a pile particle size on the stainless steel plate at about 60 grams of 0.05～4 millimeter sand shape solid.This solid particulate is put into container, and the acetate that adds 1000 gram pH=1 solution soaking forever changes pure water and soaks after 30 hours, soak altogether and change water 3 times, the solid particulate that obtains 105 ℃ of bakings after 24 hours dry ball milling obtain white carbon black, Na
2O content is 0.01wt%.
Embodiment 8
The alkali cleaning waste water that embodiment 1 is obtained is adjusted to pH=9 with acetate, the solution that obtains is put into plastic containers and is built in the reach in freezer internal cooling to becoming ice shape solid fully, should ice the shape solid then takes out to be placed on the plank and thaws, wait to thaw and finish, after water drops down and do, obtain a pile particle size on the plank at about 60 grams of 0.05～4 millimeter sand shape solid.This solid particulate is put into container, and the aqueous hydrochloric acids that add 1000 gram pH=1 soak and change pure water after 6 hours and soak, soak altogether and change water 5 times, the solid particulate that obtains 105 ℃ of bakings after 24 hours dry ball milling obtain white carbon black, Na
2O content is 0.01wt%.
Embodiment 9
The alkali cleaning waste water that embodiment 1 is obtained is adjusted to this storng-acid cation exchange resin of filtering behind the pH=10 with storng-acid cation exchange resin, be adjusted to pH=9 with hydrochloric acid then, be adjusted to pH=7.5 with acetate more at last, the solution that obtains is put into plastic containers and is built in the reach in freezer internal cooling to becoming ice shape solid fully, should ice the shape solid then takes out to be placed on the cement plate and thaws, wait to thaw and finish, after water drops down and do, obtain a pile particle size on the plank at about 60 grams of 0.05～4 millimeter sand shape solid.This solid particulate is put into container, adds 1000 gram pure water and soak and change the water logging bubble after 36 hours, soak altogether and change water 3 times, the solid particulate that obtains 100 ℃ of bakings after 36 hours dry ball milling obtain white carbon black, Na
2O content is 0.1wt%.
Embodiment 10
The alkali cleaning waste water that embodiment 1 is obtained is adjusted to pH=10 with formic acid, the solution that obtains is put into plastic containers and is built in the reach in freezer internal cooling to becoming ice shape solid fully, should ice the shape solid then takes out to be placed on the plastic plate and thaws, wait to thaw and finish, after water drops down and do, obtain a pile particle size on the plastic plate at about 60 grams of 0.05～4 millimeter sand shape solid.This solid particulate is put into container, adds 1000 gram pure water and soak and change the water logging bubble after 24 hours, soak altogether and change water 5 times, the solid particulate that obtains 105 ℃ of bakings after 24 hours dry ball milling obtain white carbon black, Na
2O content is 0.1wt%.
Embodiment 11
The alkali cleaning waste water that embodiment 1 is obtained is adjusted to pH=8.5 with acid waste water, remove by filter the ironic hydroxide flocks of generation then, the solution that obtains is put into plastic containers and is built in the reach in freezer internal cooling to becoming ice shape solid fully, should ice the shape solid then takes out to be placed on the rubber plate and thaws, wait to thaw and finish, after water drops down and do, obtain a pile particle size on the rubber plate at about 60 grams of 0.05～4 millimeter sand shape solid.This solid particulate is put into container, adds 1000 gram pure water and soak to change forever after 24 hours and soak, soak altogether and change water 5 times, the solid particulate that obtains 110 ℃ of bakings after 12 hours dry ball milling obtain white carbon black, Na
2O content is 0.1wt%, Fe
2O
3Content is 0.6wt%.
Embodiment 12
Get 1000 gram polysilicon cutting waste materials, chemical ingredients is roughly by weight percentage: 15wt% moisture, 60wt% silicon carbide, 18wt% silicon powder and silicon bits, iron and ferric oxide 6wt%, other compositions 1wt%; Add 1000 gram water stirring becoming slurries, add 14 gram sodium hydroxide then, stirring reaction 24 hours, then the slurry that obtains is placed in the centrifuge tube and makes the solid matter sedimentation with the whizzer processing, the solution on centrifuge tube upper strata is inclined to and keep, lower floor's solid matter takes out and adds 1000 gram water stirrings 30 minutes, carrying out centrifugal settling again handles, wash so repeatedly five times (and keeping water lotion), the solid settlement thing that obtains is washed pH=7.5, oven dry just obtains reclaiming silicon carbide abrasive, and the alkali reaction solution that centrifugation is gone out and follow-up each time water lotion are collected mixing, are exactly the alkali cleaning waste water of polysilicon waste material.This alkali cleaning waste water is adjusted to this Zeo-karb of filtering behind the pH=10 with storng-acid cation exchange resin, the solution that obtains is put into plastic containers and is built in the reach in freezer internal cooling to becoming ice shape solid fully, should ice the shape solid then together shifts out together with container and thaws, wait to thaw finish after, container bottom forms one deck size at about 60 grams of 0.05～4 millimeter sand shape solid particulate settling, and the container upper strata is a liquid.The aqueous sulfuric acids that this solid particulate is added 1000 gram pH=1 soak and change pure water after 24 hours and soak, soak altogether and change water 5 times, the solid particulate that obtains 105 ℃ of bakings after 24 hours dry ball milling obtain white carbon black, Na
2O content is 0.01wt%, Fe
2O
3Content is 0.6wt%.
Embodiment 13
Get 1000 gram polysilicon cutting waste materials, chemical ingredients is roughly by weight percentage: 15wt% moisture, 60wt% silicon carbide, 18wt% silicon powder and silicon bits, iron and ferric oxide 6wt%, other compositions 1wt%; Add 1000 gram water stirring becoming slurries, add 18 gram potassium hydroxide then, stirring reaction 24 hours, then the slurry that obtains is placed in the centrifuge tube and makes the solid matter sedimentation with the whizzer processing, the solution on centrifuge tube upper strata is inclined to and keep, lower floor's solid matter takes out and adds 1000 gram water stirrings 30 minutes, carrying out centrifugal settling again handles, wash so repeatedly five times (and keeping water lotion), the solid settlement thing that obtains is washed pH=7.5, oven dry just obtains reclaiming silicon carbide abrasive, and the alkali reaction solution that centrifugation is gone out and follow-up each time water lotion are collected mixing, are exactly the alkali cleaning waste water of polysilicon waste material.This alkali cleaning waste water is adjusted to this Zeo-karb of filtering behind the pH=9.5 with storng-acid cation exchange resin, the solution that obtains is put into plastic containers and is built in the reach in freezer internal cooling to becoming ice shape solid fully, should ice the shape solid then together shifts out together with container and thaws, wait to thaw finish after, container bottom forms one deck size at about 60 grams of 0.05～4 millimeter sand shape solid particulate settling, and the container upper strata is a liquid.The aqueous nitric acid that this solid particulate is added 1000 gram pH=1 soak and change pure water after 36 hours and soak, soak altogether and change water 6 times, the solid particulate that obtains 105 ℃ of bakings after 36 hours dry ball milling obtain white carbon black, K
2O content is 0.01wt%, Fe
2O
3Content is 0.6wt%.
Embodiment 14
Get 1000 gram polysilicon cutting waste materials, chemical ingredients is roughly by weight percentage: 15wt% moisture, 60wt% silicon carbide, 18wt% silicon powder and silicon bits, iron and ferric oxide 6wt%, other compositions 1wt%; Add 1000 gram water stirring becoming slurries, add 10 gram Tetramethylammonium hydroxide then, stirring reaction is 24 hours between 70～90 ℃, then the slurry that obtains is placed in the centrifuge tube and makes the solid matter sedimentation with the whizzer processing, the solution on centrifuge tube upper strata is inclined to and keep, lower floor's solid matter takes out and adds 1000 gram water stirrings 30 minutes, carrying out centrifugal settling again handles, wash so repeatedly five times (and keeping water lotion), the solid settlement thing that obtains is washed pH=7.5, oven dry just obtains reclaiming silicon carbide abrasive, and the alkali reaction solution that centrifugation is gone out and follow-up each time water lotion are collected mixing, are exactly the alkali cleaning waste water of polysilicon waste material.This alkali cleaning waste water is adjusted to this Zeo-karb of filtering behind the pH=10 with storng-acid cation exchange resin, the solution that obtains is put into plastic containers and is built in the reach in freezer internal cooling to becoming ice shape solid fully, should ice the shape solid then together shifts out together with container and thaws, wait to thaw finish after, container bottom forms one deck size at about 60 grams of 0.05～4 millimeter sand shape solid particulate settling, and the container upper strata is a liquid.The phosphate aqueous solutions that this solid particulate is added 1000 gram pH=1 soak and change pure water after 36 hours and soak, soak altogether and change water 4 times, the solid particulate that obtains 105 ℃ of bakings after 24 hours dry ball milling obtain white carbon black, Fe
2O
3Content is 0.6wt%.
Claims (10)
1. method of utilizing the white carbon black of polysilicon cutting waste material alkali cleaning waste water production, this alkali cleaning waste water contain a kind of in sodium hydroxide, potassium hydroxide and the quaternary ammonium hydroxide, it is characterized in that, steps of the method are:
(1) polysilicon being cut waste material uses chemical cleaning method to reclaim and the alkali cleaning waste water that obtains is adjusted to pH=7.0～11.1;
The small amount of solid suspended substance or the throw out that can produce when (2) the alkali cleaning waste water after the above-mentioned pH of the regulating value is removed adjusting pH value by solid-liquid separating method;
(3) the low temperature resistant container of packing into of the alkali cleaning waste water after handling with the above-mentioned pH of regulating value and through solid-liquid separating method is placed on that low temperature environment is freezing ices the shape solid to freezing fully to become, should ice the shape solid then shifts out and thaws, thaw finish after, the bottom of container is the deposition of solids layer that one deck is of a size of 0.05～4 millimeter sand shape particle packing formation, and the upper strata is a water;
(4) the above-mentioned sand shape granular deposit that obtains is separated with water, solid-liquid separation is soaked again after then the sand shape granular deposit being soaked in water 2～36 hours, washes for 3～6 times repeatedly, obtains the sand shape solid particulate;
(5) above-mentioned washing is good sand shape solid particulate was 100～110 ℃ of bakings 12～36 hours, and the exsiccant sand shape solid particulate that obtains obtains white carbon black through dry ball milling.
2. the method for utilizing the white carbon black of polysilicon cutting waste material alkali cleaning waste water production according to claim 1 is characterized in that: the described water that thaws container upper strata, back is removed with tipping, the sand shape solid particulate that makes lower floor with separated mutually forever.
3. the method for utilizing the white carbon black of polysilicon cutting waste material alkali cleaning waste water production according to claim 1, it is characterized in that: described ice shape solid shifts out to be placed on the porous water filtration object behind the low temperature environment and thaws, ice shape solid thaws on one side, the water that produces is filtered away on one side, thaws directly to obtain the sand shape solid particulate after finishing.
4. the method for utilizing the white carbon black of polysilicon cutting waste material alkali cleaning waste water production according to claim 3 is characterized in that: described porous water filtration object is a kind of among filter cloth, porous ceramic plate, the screen cloth.
5. the method for utilizing the white carbon black of polysilicon cutting waste material alkali cleaning waste water production according to claim 1, it is characterized in that: described ice shape solid shifts out to be placed on the flat board behind the low temperature environment and thaws, ice shape solid thaws on one side, the water that produces drops down on one side, thaws directly to obtain the sand shape solid particulate after finishing.
6. the method for utilizing the white carbon black of polysilicon cutting waste material alkali cleaning waste water production according to claim 5 is characterized in that: described flat board is a kind of among sheet glass, ceramic of compact plate, stainless steel plate, wood-block, cement plate, plastic plate, the rubber plate.
7. the method for utilizing the white carbon black of polysilicon cutting waste material alkali cleaning waste water production according to claim 1 is characterized in that: the method for described adjusting alkali cleaning waste water ph is the not fluoride of adding polysilicon waste material pickling generation in described alkali cleaning waste water and/or the pickling waste waters of hydrofluoric acid.
8. the method for utilizing the white carbon black of polysilicon cutting waste material alkali cleaning waste water production according to claim 1, it is characterized in that: the method for described adjusting pH value will leach this Zeo-karb after the adding acidic cation-exchange resin regulates the pH value for add one or more the combination among acidic cation-exchange resin, hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, acetate, the formic acid in described alkali cleaning waste water.
9. the method for utilizing the white carbon black of polysilicon cutting waste material alkali cleaning waste water production according to claim 1 is characterized in that: contain one or more the combination among hydrochloric acid, sulfuric acid, phosphoric acid, nitric acid, acetate, the formic acid in the water that described water-washing step uses.
10. the method for utilizing the white carbon black of polysilicon cutting waste material alkali cleaning waste water production according to claim 1, it is characterized in that: describedly carry out wet ball grinding through washing wet solid particulate matter clean and that solid-liquid separation obtains, the slurry that obtains carries out spraying drying, makes white carbon black.
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| CN102604154A (en) * | 2012-02-27 | 2012-07-25 | 周其强 | Application of polysilicon waste material in preparing rubber-modified masterbatch |
| CN103086385A (en) * | 2013-02-27 | 2013-05-08 | 中煤平朔集团有限公司 | Method for preparing rubber-grade white carbon black by using fly ash |
| CN109809414A (en) * | 2019-03-25 | 2019-05-28 | 江苏中江材料技术研究院有限公司 | A kind of solar panel cutting waste material recycling processing method |
| CN110002450A (en) * | 2019-01-11 | 2019-07-12 | 成亚资源科技股份有限公司 | The processing method that useless silicon mud recycles |
| CN114604873A (en) * | 2022-03-25 | 2022-06-10 | 中昊黑元化工研究设计院有限公司 | Process for producing high-dispersion precipitated white carbon black by utilizing recycled waste plastics |
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| CN102604154A (en) * | 2012-02-27 | 2012-07-25 | 周其强 | Application of polysilicon waste material in preparing rubber-modified masterbatch |
| CN103086385A (en) * | 2013-02-27 | 2013-05-08 | 中煤平朔集团有限公司 | Method for preparing rubber-grade white carbon black by using fly ash |
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| CN114604873A (en) * | 2022-03-25 | 2022-06-10 | 中昊黑元化工研究设计院有限公司 | Process for producing high-dispersion precipitated white carbon black by utilizing recycled waste plastics |
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