CN1053044A - A kind of method for preparing precipitated hydrated silica - Google Patents
A kind of method for preparing precipitated hydrated silica Download PDFInfo
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- CN1053044A CN1053044A CN 90106136 CN90106136A CN1053044A CN 1053044 A CN1053044 A CN 1053044A CN 90106136 CN90106136 CN 90106136 CN 90106136 A CN90106136 A CN 90106136A CN 1053044 A CN1053044 A CN 1053044A
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- wollastonite
- filtration
- reaction
- hydrochloric acid
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Abstract
A kind of method for preparing precipitated hydrated silica, this method is with wollastonite, hydrochloric acid or nitric acid are raw material, make the finished product hydrated SiO 2 by reaction, filtration, drying and crushing, the former filtrate that it filters out obtains byproduct calcium chloride or nitrocalcite by neutralization, adjusting pH, clarification filtration, concentrate drying.
This method uses raw material sources wide, and price is low, technology is simple, does not have " three wastes " and pollutes.
Description
The present invention relates to a kind of method of producing hydrated SiO 2 of domain of inorganic chemistry.
Whole world white carbon black (silicon-dioxide) throughput was 720,000 tons/year in 1988, and wherein precipitator method throughput is 660,000 tons/year.Existing precipitated silica is to adopt water glass and diluted acid reaction to make, and the main drawback of this technology is the cost of material height.Invented technology for the Chinese patent CN1036746A of Chongqing City Chemical Engineering Inst. number with silica sand and Neutral ammonium fluoride direct production precipitated silica, but this technology is raw material with the Neutral ammonium fluoride, and its raw material sources difficulty has severe corrosive to equipment, poisonous to human body, environmental pollution is big.
The objective of the invention is to create that a kind of (main component is calcium metasilicate CaSiO with natural wollastonite
3) for raw material (replacing the industrial chemicals water glass in the old technology) and hydrochloric acid or nitric acid single step reaction obtain precipitated hydrated silica, reclaim the novel process of byproduct calcium chloride or nitrocalcite simultaneously.
Technological process of the present invention comprises: reaction, filtration, rinsing filtration, drying and crushing and byproduct reclaim plurality of processes, it is characterized in that reaction is to be raw material with wollastonite, hydrochloric acid or nitric acid, its raw material weight ratio is: wollastonite: it is 100% that hydrochloric acid=1: 0.65～0.75(hydrochloric acid is amounted to HCL); Wollastonite: nitric acid=1: 1.14～1.30(nitric acid is amounted to HNO
3Be 100%).
Saliferous acidic solution after batch rinsing product filtered on this method had also added in reactor.
The byproduct removal process be meant will reaction after-filtration gained former filtrate, by neutralization, clarification, filter, concentrate, dry five stages obtain byproduct calcium chloride or nitrocalcite.
The invention has the advantages that with natural wollastonite to replace water glass, raw material sources are wide, low price; Reclaimed byproduct simultaneously, production cost is low, does not have " three wastes " and pollutes.
Present method be described in detail for: in reaction flask, drop into 10～36% hydrochloric acid, add an amount of acid filtrate that contains calcium chloride of going up batch rinsing after-filtration gained.Weight ratio 1: 0.65～0.75 by wollastonite and hydrochloric acid (amounting to HCL is 100%) under agitation slowly joins the wollastonite powder in the reaction flask.Continued stirring reaction again 1～4 hour after adding wollastonite powder, allow raw material fully react, its chemical equation is as follows:
CaSiO
3(wollastonite)+2HCL → SiO
2+ H
2O+CaCL
2
The reaction after-filtration is neutralized to filtrate about PH6 with calcite in powder, regulates PH8～9 with milk of lime again, clarification filtration, is concentrated into driedly, can get calcium chloride.Filter cake is used and its equivalent tap water rinsing, stirs 15 minutes, filters (wash water contains a large amount of calcium chloride and hydrochloric acid for the first time, as following batch mother liquor) continuous rinsing 3～5 times, contains Ca until wash water
2+ below 50PPM, more once, be filtered to driedly with rinsed with deionized water, 140～160 ℃ are dried to water content less than 7%.
Nitric acid with 20% above concentration replaces hydrochloric acid.Wollastonite and nitric acid (are amounted to HNO
3Be 100%) weight ratio be 1: 1.14～1.30, operation comes to the same thing with same with hydrochloric acid, just by product is a nitrocalcite, its chemical equation is as follows:
Accompanying drawing prepares the process flow diagram of precipitated hydrated silica with wollastonite for the present invention.
The precipitated hydrated silica quality standard that makes by technique of the present invention is as follows:
SiO
2〉=92% burning decrement≤7%
PH value 6～7 oil factors 〉=1.70ml/g
200 screen residues≤0.009%
Index of refraction 1.4590～1.4610
Above indices all meets or exceeds the precipitated hydrated silica quality index with produced in conventional processes, and the present invention is owing to reclaimed calcium chloride or the calcium nitrate in the production process, so whole technical process, nothing " three wastes " is discharged.
Embodiment one: drop into 31% technical hydrochloric acid 130 grams in the 500ml there-necked flask, go up crowd rear filtrate of rinsing for the first time 120ml, under vigorous stirring 58 grams, 200 purpose wollastonite powder (are contained SiO
244～52%) gradation slowly joins in the flask.Rely on the reaction heating, temperature of reaction rises to 60 ℃ gradually by room temperature, continues to stir 2 hours after adding wollastonite powder.Filter, filtrate is as reclaiming calcium chloride, and filter cake stirs filtration in 15 minutes with tap water 120ml rinsing, and filtrate is made the mother liquor of batch reaction down.Continue to use the tap water rinsing, the filtrate after rinsing adds the Na of 1m
2CO
3Solution does not have till the turbid phenomenon, uses the rinsed with deionized water filter cake more once, is filtered to anhydrous dripping, and filter cake was got major product white porous hydrated SiO 2 30 grams in 3 hours 160 ℃ of oven dry, pulverizes and is the white carbon black finished product.
Former filtrate after the filtration is neutralized to about PH6 with calcite in powder, adds milk of lime again and regulates PH8～9, and clarification filtration promptly gets byproduct hydration calcium chloride 55 grams with the filtrate concentrate drying.
Embodiment two: drop into 65% nitric acid 107 grams in the 500ml there-necked flask, upward the filtrate 120ml after batch rinsing for the first time (contains SiO with 58 grams, 200 purpose wollastonite powder under vigorous stirring
244～52%) gradation slowly joins in the flask.Rely on the reaction heating, temperature of reaction rises to 60 ℃ gradually by room temperature.After adding wollastonite powder, continue to stir 2 hours, filter, filtrate is as reclaiming nitrocalcite.Filter cake stirred 15 minutes with tap water 120ml rinsing, filtered, and filtrate is made batch reaction mother liquor down.Continue to use the tap water rinsing, the filtrate after rinsing adds the Na of 1M
2CO
3Till the no turbid phenomenon, use the rinsed with deionized water filter cake more once in the solution, be filtered to anhydrous dripping.Filter cake 160 ℃ of oven dry 3 hours, is got white porous hydrated SiO 2 30 grams, pulverize and be the white carbon black finished product.
Byproduct reclaims according to embodiment one, can get nitric hydrate calcium 95 grams.
Claims (4)
1, a kind of method for preparing precipitated hydrated silica comprises that reaction, filtration, rinsing filtration, drying and crushing and byproduct reclaim plurality of processes; It is characterized in that reaction is to be raw material with wollastonite, hydrochloric acid, the weight ratio of wollastonite and hydrochloric acid is 1: 0.65～0.75 (it is 100% that hydrochloric acid is amounted to HCL).
2, method according to claim 1 is characterized in that reaction can be with wollastonite, and nitric acid is raw material, and the weight ratio of wollastonite and nitric acid is that 1: 1.14～1.30(nitric acid is amounted to HNO
3Be 100%).
3, method according to claim 1 and 2 is characterized in that adding in the reactor saliniferous acidic solution of going up after batch rinsing product filters.
4, method according to claim 1 and 2 is characterized in that the byproduct removal process is: the former filtrate that will react the filtration gained obtains byproduct by neutralization, clarification, filtration, concentrated, dry five stages.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 90106136 CN1053044A (en) | 1990-12-07 | 1990-12-07 | A kind of method for preparing precipitated hydrated silica |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 90106136 CN1053044A (en) | 1990-12-07 | 1990-12-07 | A kind of method for preparing precipitated hydrated silica |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1053044A true CN1053044A (en) | 1991-07-17 |
Family
ID=4879838
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 90106136 Pending CN1053044A (en) | 1990-12-07 | 1990-12-07 | A kind of method for preparing precipitated hydrated silica |
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| CN (1) | CN1053044A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1039219C (en) * | 1993-12-21 | 1998-07-22 | 冯中一 | Technology for combination production of sodium silicate, aquation silica acid and zeolite catalyst by mirabilite method |
| NL1007131C2 (en) * | 1997-09-26 | 1999-03-29 | Geochem Research B V | Silica with high silanol group content |
| CN102502662A (en) * | 2011-11-09 | 2012-06-20 | 段甲明 | Method for preparing precipitated white carbon black by using waste slag for producing ferrovanadium |
| CN104609436A (en) * | 2015-02-11 | 2015-05-13 | 四川西冶新材料有限公司 | Method for preparing water glass from aedelforsite by virtue of decomposition with hydrochloric acid and curing with curing agent |
| CN106145128A (en) * | 2016-08-18 | 2016-11-23 | 柳州市亿廷贸易有限责任公司 | The method preparing nano silicon for raw material with wollastonite |
-
1990
- 1990-12-07 CN CN 90106136 patent/CN1053044A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1039219C (en) * | 1993-12-21 | 1998-07-22 | 冯中一 | Technology for combination production of sodium silicate, aquation silica acid and zeolite catalyst by mirabilite method |
| NL1007131C2 (en) * | 1997-09-26 | 1999-03-29 | Geochem Research B V | Silica with high silanol group content |
| CN102502662A (en) * | 2011-11-09 | 2012-06-20 | 段甲明 | Method for preparing precipitated white carbon black by using waste slag for producing ferrovanadium |
| CN102502662B (en) * | 2011-11-09 | 2013-09-11 | 段甲明 | Method for preparing precipitated white carbon black by using waste slag for producing ferrovanadium |
| CN104609436A (en) * | 2015-02-11 | 2015-05-13 | 四川西冶新材料有限公司 | Method for preparing water glass from aedelforsite by virtue of decomposition with hydrochloric acid and curing with curing agent |
| CN104609436B (en) * | 2015-02-11 | 2016-01-20 | 四川西冶新材料有限公司 | Adopt hydrochloric acid to decompose with wollastonite and solidifying agent slaking legal system for the method for water glass |
| CN106145128A (en) * | 2016-08-18 | 2016-11-23 | 柳州市亿廷贸易有限责任公司 | The method preparing nano silicon for raw material with wollastonite |
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