CN1524787A - Silicon dioxide rapid precipitation process - Google Patents
Silicon dioxide rapid precipitation process Download PDFInfo
- Publication number
- CN1524787A CN1524787A CNA031350100A CN03135010A CN1524787A CN 1524787 A CN1524787 A CN 1524787A CN A031350100 A CNA031350100 A CN A031350100A CN 03135010 A CN03135010 A CN 03135010A CN 1524787 A CN1524787 A CN 1524787A
- Authority
- CN
- China
- Prior art keywords
- precipitation
- silicon
- deposition
- quartz powder
- bicarbonate
- 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.)
- Granted
Links
- 238000001556 precipitation Methods 0.000 title claims abstract description 24
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 title claims description 10
- 239000000377 silicon dioxide Substances 0.000 title claims description 8
- 235000012239 silicon dioxide Nutrition 0.000 title description 5
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000002002 slurry Substances 0.000 claims abstract description 10
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 8
- 238000011010 flushing procedure Methods 0.000 claims abstract description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 27
- 229910052742 iron Inorganic materials 0.000 claims description 13
- 150000003839 salts Chemical class 0.000 claims description 10
- 238000005516 engineering process Methods 0.000 claims description 5
- 239000013049 sediment Substances 0.000 claims description 4
- 238000004900 laundering Methods 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims description 2
- 238000010298 pulverizing process Methods 0.000 claims 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 21
- 238000003756 stirring Methods 0.000 abstract description 10
- 239000000654 additive Substances 0.000 abstract description 6
- 239000000843 powder Substances 0.000 abstract description 6
- 229910052710 silicon Inorganic materials 0.000 abstract description 5
- 239000010703 silicon Substances 0.000 abstract description 5
- 239000000126 substance Substances 0.000 abstract description 2
- 230000008021 deposition Effects 0.000 abstract 3
- 239000010453 quartz Substances 0.000 abstract 3
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 abstract 1
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 abstract 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 abstract 1
- 230000000996 additive effect Effects 0.000 abstract 1
- 239000001099 ammonium carbonate Substances 0.000 abstract 1
- 238000005119 centrifugation Methods 0.000 abstract 1
- 238000005137 deposition process Methods 0.000 abstract 1
- 235000011194 food seasoning agent Nutrition 0.000 abstract 1
- 239000002184 metal Substances 0.000 abstract 1
- 238000005201 scrubbing Methods 0.000 abstract 1
- 229910052814 silicon oxide Inorganic materials 0.000 abstract 1
- 239000011863 silicon-based powder Substances 0.000 description 18
- 238000004062 sedimentation Methods 0.000 description 11
- 239000002699 waste material Substances 0.000 description 11
- 239000000047 product Substances 0.000 description 9
- 239000007787 solid Substances 0.000 description 9
- 238000011109 contamination Methods 0.000 description 7
- 238000005406 washing Methods 0.000 description 7
- VTYYLEPIZMXCLO-UHFFFAOYSA-L calcium carbonate Substances [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 238000001035 drying Methods 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 229960001866 silicon dioxide Drugs 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 235000010216 calcium carbonate Nutrition 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- 229910000019 calcium carbonate Inorganic materials 0.000 description 2
- 239000000084 colloidal system Substances 0.000 description 2
- 238000013467 fragmentation Methods 0.000 description 2
- 238000006062 fragmentation reaction Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 235000012204 lemonade/lime carbonate Nutrition 0.000 description 2
- 238000000247 postprecipitation Methods 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-M Bicarbonate Chemical compound OC([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-M 0.000 description 1
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- WNQQFQRHFNVNSP-UHFFFAOYSA-N [Ca].[Fe] Chemical compound [Ca].[Fe] WNQQFQRHFNVNSP-UHFFFAOYSA-N 0.000 description 1
- 230000002238 attenuated effect Effects 0.000 description 1
- NKWPZUCBCARRDP-UHFFFAOYSA-L calcium bicarbonate Chemical compound [Ca+2].OC([O-])=O.OC([O-])=O NKWPZUCBCARRDP-UHFFFAOYSA-L 0.000 description 1
- 229910000020 calcium bicarbonate Inorganic materials 0.000 description 1
- 229910001424 calcium ion Inorganic materials 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000009686 powder production technique Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000007785 strong electrolyte Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
Landscapes
- Silicon Compounds (AREA)
Abstract
The invention relates to a silicon oxide deposition process wherein on the basis of water scrubbing natural deposition, ammonium bicarbonate (orammonium carbonate) is filled as deposition addition agent, and metal magnetic stripes able to adsorb foreign substance are used as stirring rods to homogenize the silicon micronized quartz powder slurry and deposition additive, taking out of the container after 10 minutes, flushing with clean water for alternative, the slurry is in standstill for 6-12 hours, the silicon micronized quartz powder precipitation is rinsed twice using clean water, after mechanical centrifugation, seasoning at the under the temperature of 600-900 deg. C, thus realizing porous, easy-fragmenting and high purity silicon micronized quartz powder.
Description
1, technical background
In wet ball grinding explained hereafter silicon powder process, adopt the washing settling process to obtain the precipitated silica of solid content about 70%.The intermediate processing of this classics, shortcoming are that settling velocity is slow, residual quantity height in the waste pulp, and product purity is not high.To fineness at 200 orders-600 purpose silicon powder, generally precipitate 24 hours after, solid content reaches 12-25% in the suspension of upper strata.This intermediate processing, silicon powder finished product stammerer is serious, is difficult to take out before being dried, can only be with the container heat drying.And calcium iron contamination content is higher, contains the high-quality super-fine silicon micro-powder in the waste pulp of solid content up to 12-25%, arrange behind water body environment, and the one, cause water pollution, the 2nd, cause the finished product waste.
2, embodiment of the present invention and principle
When (1) embodiment of the present invention silicon powder slurries discharge from ball mill, add bicarbonate of ammonia or volatile salt, addition is the 1.0-2.0% of slurries by weight.With Armco magnetic iron row culture stirring rod, carry out stirring in ten minutes, stir evenly the back and propose stirring rod, standby after the flushing with clean water.Slurries precipitate 6-12 hour under normal temperature, normal pressure, sedimentation time is decided with the silicon powder fineness.Fineness is the general precipitation of 200 order silicon powders 6 hours, and 600 order silicon powders generally need precipitate 12 hours, tell upper solution after, lower floor's slurries are with clear water washing precipitation surface gently, and remove scrubber layer, and lower sediment is after mechanical separation, dry under normal pressure and 600-650 ℃ of temperature, fragmentation.
Aforesaid method also is used for the recovery of natural sedimentation waste pulp.Adding weight ratio in the waste pulp of natural sedimentation after 24 hours is bicarbonate of ammonia or the volatile salt of 1.0-2.0%, stirs 10 minutes with the magnetic iron bar, after sedimentation 6-12 hour, with a small amount of clear water washing precipitation surface and removing gently, after layering and machinery are centrifugal, 600-650 ℃ of drying, fragmentation.
(2), principle of the invention the present invention main effect of adding bicarbonate of ammonia or volatile salt has two aspects; The one, as helping precipitation additives, quicken settling velocity.When the silicon powder granularity attenuated, silicon-dioxide easily formed colloid, and influences settling velocity, after adding bicarbonate of ammonia or volatile salt, because bicarbonate of ammonia or volatile salt all belong to strong electrolyte, helped destroying colloidal and formed, thereby can accelerate settling velocity.
The 2nd, the bicarbonate ion in the bicarbonate of ammonia can form the processable Calcium hydrogen carbonate with the calcium ion in the silicon powder;
Help precipitation additives bicarbonate of ammonia and volatile salt, can both accelerate settling velocity, and the latter help settling velocity faster than the former, but the former is better than the latter removal of impurity effect, test shows after deliberation, helps precipitation agent to make precipitation agent than with volatile salt with bicarbonate of ammonia, and purity improves about 1%.
The present invention is to remove iron contamination with the effect of Armco magnetic iron row culture stirring rod, generally stirs ten minutes before sedimentation, and iron contamination is attracted to magnetic iron bar surface, reaches the purpose of removing iron contamination.The method of another iron impurity is after layering, with clear water washing precipitation surface gently, because the Fe (OH) of chemical combination attitude
3Easily form colloid, the postprecipitation phenomenon takes place, major part is attracted to the surface of silicon powder, therefore after layering, centrifugal before, fine laundering silicon powder precipitation surface helps the raising of finished product purity.Test shows, gently behind the washing precipitation surface, purity improves more than 0.5% with clear water.
Help sinking agent weight ratio 1.0% and 2.0% relatively, the former is after sedimentation in 6-12 hour, and the solid content of upper strata waste liquid is at 5-6%, but lower floor's slurry solid content is higher, reaches more than 60%, and purity is higher, reaches more than 99%.2% weight ratio help sinking agent, settling velocity is very fast, upper strata waste liquid solid content is low, less than 1%, but lower floor's slurries are loose, solid content is less than 60%, purity is more than 98%.
3, creative the present invention of the present invention adds in natural sedimentation method after bicarbonate of ammonia (or volatile salt) helps precipitation additives, compares with classical natural sedimentation technology, and new depositing technology is obviously superior.
(1) sedimentation speed adds and helps precipitation agent, and through 6 hours post precipitations, upper strata waste pulp solid content was less than 6.5% (less than more than 50% of natural sedimentation method), and the solid content of lower sediment thing reaches 70%.
(2) overcome precipitation stammerer and add bicarbonate of ammonia (or volatile salt) after, precipitation is loose, easily stirs, and has realized the characteristics that aftertreatment is easy.
(3) the product purity silicon powder that improves the wet ball grinding explained hereafter greatly contains iron contamination and lime carbonate impurity, bicarbonate of ammonia can increase the dissolution of calcium carbonate degree among the present invention, magnetic iron bar stirring rod can be adsorbed iron contamination, thereby has reduced lime carbonate and iron contamination content, and silicon powder purity is improved.No matter be virgin pulp liquid, or the classical approach precipitation waste pulp after 24 hours, adopt technology of the present invention after, the product dioxide-containing silica is all more than 98% and 99%.
4, the conventional intermediate processing of novelty silicon-dioxide of the present invention is to add acid back and water sepn
[1] [2], or add acid back interpolation organic solvent
[3] [4]The former easily brings acid ion in the silicon powder finished product, dry preceding must the washing, and operation is longer.It is higher that the latter is precipitated cost.And the precipitation additives that the present invention adopts, the one, inexpensive, the 2nd, easily decompose volatilization during heat drying, do not influence throw out purity, and can be without the washing convection drying.Through looking into new affirmation, there are not same or similar technology and similar precipitation additives.
5, practicality the present invention of the present invention can be on the production basis of former silicon powder, and increasing simple steps and cheap cost can realize, it is slow to have overcome in the production process sedimentation speed, and finished product is the difficult problem of stammerer easily.The present invention also can be used for the recycling of silicon powder waste pulp, has both prevented environmental pollution, has reclaimed the high-quality super-fine silicon micro-powder again, has good practicality.
6, technical field the invention belongs to the technical matters transformation in the field of inorganic materials, mainly solve problems such as the medium-term and long-term settling velocity that exists of silicon powder production technique is slow, easily stammerer, purity be low, and solved in the original production process waste pulp effectively the pollution of environment.
5, reference;
(1), Xu Menglei, high purity SiO 2 superfine powder and production method thereof (P), Chinese patent; CN 1186772,1998-07-08
(2), Yang Baotian, yellow gram, Zhang Shumei etc., the production method of white carbon black (P), Chinese patent; CN 1120016,1996-04-10
(3), Yuan Weiping, the preparation method of superfine silicon dioxide (P), Chinese patent; CN1186044,1998-07-01
(4), thatch-capital Truex, Ka Ermai Yale, A Site Reed Miller etc., partially hydrophobic precipitated silicas (P), Chinese patent: CN1167078,1997-12-10 are consolidated in the sea
Claims (1)
- A kind of precipitation of silica technology adopts the natural subsidence method, adds and helps precipitation agent.Comprise in the settling process:A, add people's bicarbonate of ammonia (or volatile salt) for helping precipitation agent, addition is the 1.0-2.0% of slurries by weight.B, mix rod, slurries are stirred propose outside the container after 10 minutes with the magnetic iron staff, totally standby with flushing with clean water.Behind C, the precipitated and separated, lower sediment is with clear water fine laundering precipitation surface 2 times, remove scrubber layer after, lower sediment is after mechanical separation, dry under normal pressure and 600-650 ℃ of temperature, pulverizing the back slightly is finished product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03135010 CN1233556C (en) | 2003-09-17 | 2003-09-17 | Silicon dioxide rapid precipitation process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03135010 CN1233556C (en) | 2003-09-17 | 2003-09-17 | Silicon dioxide rapid precipitation process |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1524787A true CN1524787A (en) | 2004-09-01 |
| CN1233556C CN1233556C (en) | 2005-12-28 |
Family
ID=34286258
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 03135010 Expired - Fee Related CN1233556C (en) | 2003-09-17 | 2003-09-17 | Silicon dioxide rapid precipitation process |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1233556C (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102762498A (en) * | 2010-02-19 | 2012-10-31 | 株式会社德山 | Method for producing inorganic oxide particles |
| CN111017932A (en) * | 2019-12-30 | 2020-04-17 | 无锡恒诚硅业有限公司 | Large-aperture white carbon black and preparation method and application thereof |
-
2003
- 2003-09-17 CN CN 03135010 patent/CN1233556C/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102762498A (en) * | 2010-02-19 | 2012-10-31 | 株式会社德山 | Method for producing inorganic oxide particles |
| US9000202B2 (en) | 2010-02-19 | 2015-04-07 | Tokuyama Corporation | Method for producing inorganic oxide particles |
| US9079777B2 (en) | 2010-02-19 | 2015-07-14 | Tokuyama Corporation | Method for producing inorganic oxide particles |
| CN102762498B (en) * | 2010-02-19 | 2015-11-25 | 株式会社德山 | The manufacture method of inorganic oxide particle |
| CN111017932A (en) * | 2019-12-30 | 2020-04-17 | 无锡恒诚硅业有限公司 | Large-aperture white carbon black and preparation method and application thereof |
| CN111017932B (en) * | 2019-12-30 | 2023-02-21 | 无锡恒诚硅业有限公司 | Large-aperture white carbon black and preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1233556C (en) | 2005-12-28 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Li et al. | Removal of copper from aqueous solution by carbon nanotube/calcium alginate composites | |
| US20220219142A1 (en) | Polymeric lanthanum nanocomposite, and preparation method and application thereof | |
| CN111804930A (en) | Nano zero-valent ferro-manganese bimetal and preparation method and application thereof | |
| CN104307866B (en) | A kind of method that chemical oxidation strengthens chemical leaching restoration of soil polluted by heavy metal | |
| CN107963704B (en) | Multi-element flocculation settling agent for titanium-rich material acidolysis titanium liquid and preparation and use methods thereof | |
| CN102249386B (en) | Preparation method of modified kaoline alga flocculating agent and application thereof | |
| CN105709684B (en) | A kind of ferro manganese composite oxides arsenic removal material and its methods for making and using same | |
| CN1524787A (en) | Silicon dioxide rapid precipitation process | |
| CN104971688A (en) | Preparation method of nanometer magnetic particle adsorbent | |
| CN105214618B (en) | Quercetin calcium alginate nano gel system and its preparation method and application | |
| CN116274328A (en) | Method for mineralizing heavy metal contaminated soil by carbonate through nanomaterial-enhanced enzyme | |
| CN115779847B (en) | In-situ adsorption material and preparation method and application thereof | |
| CN104289175B (en) | A kind of preparation method of polymerizing cationically type thermal activation micropore bimetallic filler | |
| CN101269841B (en) | Manganese oxide for dephenolization and method for processing high concentration phenol wastewater | |
| CN114873649A (en) | Synthesis method of nano Shi mineral for repairing arsenic-polluted soil | |
| CN113952923B (en) | Modified micron zeolite and application thereof | |
| CN112591842B (en) | Preparation of NZVI-carbon sphere/soapstone composite material and application thereof in sewage treatment field | |
| CN114192109A (en) | Graphene copper-iron oxide composite adsorbent for removing arsenic in water and preparation method thereof | |
| CN110975798B (en) | Preparation method, application and regeneration method of FeO (OH) -diatomite composite adsorbent | |
| CN103740329A (en) | Cerium oxide polishing powder and preparation method thereof | |
| CN111849505A (en) | Soil remediation agent and preparation method and application thereof | |
| Keren et al. | Effect of pH on Permeability of Clay‐Sand Mixture Containing Hydroxy Polymers | |
| CN205398137U (en) | Retrieve tertiary gunbarrel of strontium carbonate granule | |
| CN116120941A (en) | Lead and arsenic combined polluted soil eluting agent and use method thereof | |
| CN114621599B (en) | Nano ferrihydrite-spent grain composite colloidal material and preparation and application thereof |
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 | ||
| ASS | Succession or assignment of patent right |
Owner name: HUZHOU JINTAI SCIENCE CO., LTD. Free format text: FORMER OWNER: HAN ZHIPING Effective date: 20080919 |
|
| C41 | Transfer of patent application or patent right or utility model | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20080919 Address after: No. 1888 Jintai Road, Zhejiang, Huzhou Patentee after: Huzhou Jintai Science and Technology Co., Ltd. Address before: Room 216, building 203, tide garden, Huzhou District, Zhejiang Patentee before: Han Zhiping |
|
| EE01 | Entry into force of recordation of patent licensing contract |
Assignee: Huzhou Jintai holds Limited by Share Ltd Assignor: Han Zhiping Contract fulfillment period: 2006.11.1 to 2012.11.1 Contract record no.: 2008330000757 Denomination of invention: Silicon dioxide rapid precipitation process Granted publication date: 20051228 License type: Exclusive license Record date: 20080928 |
|
| LIC | Patent licence contract for exploitation submitted for record |
Free format text: EXCLUSIVE LICENCE; TIME LIMIT OF IMPLEMENTING CONTACT: 2006.11.1 TO 2012.11.1 Name of requester: HUZHOU JINTAIKECHI CO., LTD. Effective date: 20080928 |
|
| C57 | Notification of unclear or unknown address | ||
| DD01 | Delivery of document by public notice |
Addressee: Han Hong Document name: Notification of Passing Examination on Formalities |
|
| ASS | Succession or assignment of patent right |
Owner name: HUZHOU BIAOLI ENERGY-SAVING TECHNOLOGY CO., LTD. Free format text: FORMER OWNER: HUZHOU JINTAI SCIENCE AND TECHNOLOGY CO., LTD. Effective date: 20150304 |
|
| C41 | Transfer of patent application or patent right or utility model | ||
| COR | Change of bibliographic data |
Free format text: CORRECT: ADDRESS; FROM: 313001 HUZHOU, ZHEJIANG PROVINCE TO: 313028 HUZHOU, ZHEJIANG PROVINCE |
|
| TR01 | Transfer of patent right |
Effective date of registration: 20150304 Address after: 313028 1 building, No. seven, 999 fortune road, Zhejiang, Huzhou Patentee after: HUZHOU BIAOLI ENERGY SAVING TECHNOLOGY CO., LTD. Address before: 313001 No. 1888 Jintai Road, Zhejiang, Huzhou Patentee before: Huzhou Jintai Science and Technology Co., Ltd. |
|
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20051228 Termination date: 20150917 |
|
| EXPY | Termination of patent right or utility model |