CN104445219A - Preparation method of white carbon black - Google Patents
Preparation method of white carbon black Download PDFInfo
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- CN104445219A CN104445219A CN201410700622.5A CN201410700622A CN104445219A CN 104445219 A CN104445219 A CN 104445219A CN 201410700622 A CN201410700622 A CN 201410700622A CN 104445219 A CN104445219 A CN 104445219A
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- carbon black
- white carbon
- absorption
- preparation
- absorption tower
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Abstract
The invention relates to a preparation method of white carbon black. The preparation method comprises the following steps: decomposing albite, to be specific, reacting albite, fluorite and 98% of sulfuric acid at 100-200 DEG C and under self-generated pressure to obtain a silicon fluoride-containing gas product; absorbing gas, to be specific, filling the gas product into an absorption tower for hydrolyzing to obtain hydrolysate; ammonolyzing, to be specific, filling the hydrolysate into an ammonolyzing kettle, regulating pH value by adding ammonia water, neutralizing and then aging to obtain a suspension; roughing the white carbon black, to be specific, filtering, washing and drying the suspension to obtain a white carbon black crude product; refining the white carbon black, to be specific, mixing the white carbon black crude product and water, and stirring so as to sufficiently dissolve ammonium fluoride into water; filtering and drying to obtain the pure white carbon black. The preparation method is easy to operate and low in equipment requirement, and has the advantages of energy conservation, environment friendliness and low cost.
Description
Technical field
The present invention relates to a kind of preparation method of white carbon black, especially relate to a kind of method utilizing albite production of silica white.
Background technology
White carbon black is the general name of white powder X-ray amorphous silicic acid and silicate product, mainly refers to precipitated silica, aerosil and superfine silicon dioxide gel, also comprises Powdered synthetic aluminium silicate and Calucium Silicate powder etc.
The traditional preparation methods of white carbon black mainly contains vapor phase process and the precipitator method two kinds.
Vapor phase process adopts silicon tetrachloride gas under Hydrogen Oxygen air-flow high temperature, be hydrolyzed the silicon-dioxide of obtained smoke-like.Reaction formula is: SiCl
4+ 2H
2+ O
2=SiO
2+ 4HCl; The advantage of vapor phase process is reaction conditions easy to control, product purity is high, dispersity is high, particle is thin and formed spherical, surface hydroxyl is few, thus there is the nano effect of excellent reinforcement, thickening and thixotropic property and particle, its shortcoming is high expensive, and in fact also this point limits its widespread use just, therefore, at present as rubber industry, still use traditional precipitator method production of silica white a large amount of.
The precipitator method, namely adopt the method for soluble silicate and mineral acid neutralization-precipitation reaction to carry out production of silica white.Production technology, the equipment of preparing white carbon black by precipitation method are simple, dispersion agent and raw material are easy to get, and flow process is simple, and scale of investment is little, but energy consumption is high, higher to environmental requirement, Product Activity is not high, and particle is wayward, avidity is poor, reinforcing property is low, and the hydrophilic bonding of particle surface is serious, weakens the bonding force of product.Along with improving constantly of environmental consciousness, a large amount of losses of social resources, propose a kind of energy-saving and environmental protection, white carbon black preparation method that cost is low, more seem to have important positive effect.
Summary of the invention
The present invention is directed to prior art deficiency, propose a kind of method preparing white carbon black newly.
The technical solution adopted in the present invention is: a kind of preparation method of white carbon black, comprises the following steps:
Albite decomposes: by albite, fluorite, 98% sulfuric acid mix according to the mass ratio of 1:1.55 ~ 2.57:3.28 ~ 4.62, and under 100 DEG C ~ 200 DEG C and autogenous pressure, be obtained by reacting solid residue and the gaseous products containing silicon fluoride;
Gas absorption is hydrolyzed: lead in I and II absorption tower successively by the described gaseous products containing silicon fluoride, be hydrolyzed the hydrolyzed solution obtained containing silicofluoric acid;
Ammonia solution: passed into by described hydrolyzed solution in ammonia solution still, by adding the method adjust ph of ammoniacal liquor; Ripening after neutralization, obtains dirty solution;
Rough white carbon black: by described dirty solution, be transported in pressure filter and filter, obtain white carbon black, dry after washing, obtain white carbon black crude product;
Refining white carbon black: described white carbon black crude product and water are added in container according to the mass ratio being less than or equal to 1:1, is more than or equal to 40 DEG C in temperature and is uniformly mixed more than 1 hour under negative pressure state, make Neutral ammonium fluoride fully water-soluble; Filter, dry, obtained white carbon black finished product.
Based on the preparation method of above-mentioned white carbon black, described albite decomposition step comprises: at 100 DEG C ~ 200 DEG C, preheat 15 minutes ~ 30 minutes to described albite and described fluorite, and removing moisture wherein, obtains dry albite and fluorite raw material; Again the sulfuric acid of 98% is joined in the albite of described drying and fluorite raw material and react the solid residue obtained for 2 hours ~ 5 hours containing calcium sulfate, sodium sulfate and Tai-Ace S 150 and the gaseous products containing silicon fluoride.In this step, described temperature of reaction can be 100 DEG C, 150 DEG C, 180 DEG C, 200 DEG C, is preferably 120 DEG C ~ 200 DEG C; The described reaction times is preferably 2.5 hours ~ 4 hours.
Based on the preparation method of above-mentioned white carbon black, described gas absorption hydrolysing step comprises:
Described gaseous products leads to through entering in one-level concentrated phase receiving tank after absorption liquid absorption, hydrolysis in described first grade absorption tower in described first grade absorption tower after dust removal filter filters, and the concentrated phase thing that described one-level concentrated phase receiving tank is collected is transported in ammonia solution still and carries out ammonia solution and ripening;
The liquid flooding that described one-level concentrated phase receiving tank is collected, to first order absorption circulation groove, is returned in described first grade absorption tower through pump and is continued to absorb;
Enter described two-level absorption tower absorption liquid in described two-level absorption tower by described first grade absorption tower tail gas out to absorb, continue hydrolysis, liquid after described two-level absorption tower hydrolysis enters secondary concentrated phase absorption cell, and the concentrated phase thing that described secondary concentrated phase absorption cell is collected is transported in described ammonia solution still and carries out ammonia solution and ripening;
When the fluorinion concentration detected in the silicate fluoride solution in described first order absorption circulation groove, described secondary absorption cycle groove reaches 10mol/L, absorption liquid reaches capacity, and is also transported to by described absorption liquid in described ammonia solution still and carries out ammonia solution and ripening;
Wherein, the absorption liquid in described I and II absorption tower is respectively the aqueous ethanolic solution that mass concentration is 10% ~ 30%, and in described I and II absorption tower, hydrolysis temperature is respectively 70 DEG C ~ 90 DEG C.
Based on the preparation method of above-mentioned white carbon black, in described aminolysis step, the pH value of described hydrolyzed solution is regulated to be 7 ~ 8 by adding ammoniacal liquor.
Based on the preparation method of above-mentioned white carbon black, in described aminolysis step, the time of described ripening is 1 hour ~ 2 hours, and the temperature of described ripening controls at 70 DEG C ~ 85 DEG C.
Based on the preparation method of above-mentioned white carbon black, in the step of described refining white carbon black, the mass ratio of described white carbon black crude product and described water can be 1:1,1:2,1:3,1:4,1:5, and preferably, the mass ratio of described white carbon black crude product and described water is 1:2 ~ 5.
Based on the preparation method of above-mentioned white carbon black, in the step of described refining white carbon black, described temperature can be 40 DEG C, 50 DEG C, 55 DEG C, 60 DEG C, 65 DEG C, and preferably, described temperature is 50 DEG C ~ 65 DEG C.
Based on the preparation method of above-mentioned white carbon black, in the step of described refining white carbon black, described negative pressure is 10 handkerchief ~ 70 handkerchiefs, and preferably, described negative pressure is 40 handkerchiefs.
Based on the preparation method of above-mentioned white carbon black, in the step of described refining white carbon black, be uniformly mixed described in being undertaken by agitating vane, the rotating speed of described agitating vane is 50 revs/min ~ 350 revs/min, can be such as 50 revs/min, 100 revs/min, 150 revs/min, 200 revs/min, 250 revs/min, 300 revs/min, 350 revs/min, preferably, the rotating speed of described agitating vane is 150 revs/min ~ 350 revs/min.
Based on the preparation method of above-mentioned white carbon black, in the step of described refining white carbon black, described churning time can be 1 hour, 1.5 hours, 2.0 hours, 2.5 hours, 3.0 hours, 3.5 hours, and preferably, described churning time is 2.0 hours ~ 3.5 hours.
Compared with prior art, the gaseous products containing silicon fluoride that the present invention utilizes albite decomposition reaction to produce, through hydrolysis, ammonolysis reaction production of silica white, avoids the complicated processes be separated from solid phase, reduces environmental pollution; And utilize white carbon black water insoluble and the water-soluble characteristic of Neutral ammonium fluoride, white carbon black crude product is mixed with water again, while filtered and recycled Neutral ammonium fluoride, obtains the white carbon black product that purity is higher, aforesaid operations is simple, cost is low, environmental pollution is little.The temperature of reaction of described albite decomposition technique is at 100 DEG C ~ 200 DEG C, and reaction conditions is gentle, lower to the requirement of equipment, improves albite overall availability.
Embodiment
Below by embodiment, technical scheme of the present invention is described in further detail.
embodiment 1
The present embodiment provides a kind of preparation method of white carbon black, comprises the following steps:
Albite decomposes: first albite and fluorite are preheated 30 minutes at 100 DEG C, the sulfuric acid adding 98% again makes three react 5 hours under 100 DEG C and autogenous pressure, obtain the solid residue containing calcium sulfate, sodium sulfate and Tai-Ace S 150 and the gaseous products containing silicon fluoride, wherein, albite, fluorite, 98% the mass ratio of sulfuric acid be 1:1.55:3.28, reaction principle is:
CaF
2+ H
2SO
4= 2HF + CaSO
4,
2NaAlSi
3O
8+ 24HF + 4H
2SO
4= Na
2SO
4+ Al
2(SO
4)
3+ 6SiF
4↑ + 16H
2O;
Gas absorption is hydrolyzed: by described gaseous products after dust removal filter filters, pass in first grade absorption tower enters in one-level concentrated phase receiving tank after the absorption liquid absorption in described first grade absorption tower, hydrolysis, the concentrated phase thing that described one-level concentrated phase receiving tank is collected is transported in ammonia solution still and carries out ammonia solution and ripening, wherein, hydrolysis reaction principle is: 3SiF
4+ 2H
2o=2H
2siF
6+ SiO
2↓; The liquid flooding that described one-level concentrated phase receiving tank is collected, to first order absorption circulation groove, is returned in described first grade absorption tower through pump and is continued to absorb; Enter the absorption liquid of two-level absorption tower in described two-level absorption tower by described first grade absorption tower tail gas out to absorb, continue hydrolysis, liquid after described two-level absorption tower hydrolysis enters secondary concentrated phase absorption cell, and the concentrated phase thing that described secondary concentrated phase absorption cell is collected is transported in described ammonia solution still and carries out ammonia solution and ripening; The liquid flooding that described secondary concentrated phase receiving tank is collected, to secondary absorption cycle groove, is returned in described two-level absorption tower through pump and is continued to absorb; When the fluorinion concentration detected in the silicate fluoride solution in described first order absorption circulation groove, described secondary absorption cycle groove reaches 10mol/L, absorption liquid reaches capacity, described absorption liquid is also transported in described ammonia solution still and carries out ammonia solution and ripening, wherein, absorption liquid in described I and II absorption tower is respectively the aqueous ethanolic solution that mass concentration is 20%, and in described I and II absorption tower, hydrolysis temperature is respectively 75 DEG C;
Ammonia solution: described hydrolyzed solution is passed into ammonia solution still, by adding the method adjust ph of ammoniacal liquor, makes pH=7.2; After neutralization, under 80 DEG C of conditions, ageing 1.5 hours, obtains dirty solution; Reaction principle is: H
2siF
6+ 6NH
3+ 2H
2o=6NH
4f+SiO
2↓;
Rough white carbon black: by described dirty solution, be transported in pressure filter and filter, obtain white carbon black, dry after washing, obtain white carbon black crude product;
Refining white carbon black: white carbon black crude product and water are added in container according to the mass ratio of 1:1, under 40 DEG C and 10 handkerchief condition of negative pressure, rotating paddle is with the mixed solution of white carbon black described in the rotating speed Stirring of 350 revs/min and water, and Stirring 1 hour, makes Neutral ammonium fluoride fully water-soluble; Filter, dry obtained pure white carbon black.
embodiment 2
The present embodiment provides a kind of preparation method of white carbon black, comprises the following steps:
Albite decomposes: the embodiment that the embodiment of this step of the present embodiment is decomposed with albite in embodiment 1 is substantially identical, and difference is: described preheating temperature is 150 DEG C, and described warm up time is 20 minutes; Described temperature of reaction is 150 DEG C, and the reaction times is 3.5 hours; Wherein, albite, fluorite, 98% the mass ratio of sulfuric acid be 1:2:4;
Gas absorption is hydrolyzed: the embodiment of this step of the present embodiment is substantially identical with the embodiment of gas absorption in embodiment 1, and difference is: in described I and II absorption tower, hydrolysis temperature is respectively 80 DEG C;
Ammonia solution: the embodiment of this step of the present embodiment is substantially identical with the embodiment of ammonia solution in embodiment 1, and difference is: described hydrolyzed solution ammoniacal liquor regulates pH=7.4, and digestion time is 2 hours, and Aging Temperature controls at 85 DEG C;
Rough white carbon black: the embodiment of this step of the present embodiment is identical with the embodiment preparing white carbon black in embodiment 1;
Refining white carbon black: the embodiment of this step of the present embodiment is substantially identical with the embodiment of the removal of Neutral ammonium fluoride in white carbon black in embodiment 1, difference is: the mass ratio of white carbon black crude product and water is 1:3, temperature is 50 DEG C, negative pressure is 40 handkerchiefs, rotating speed is 150 revs/min, and churning time is 2.0 hours.
embodiment 3
The present embodiment provides a kind of preparation method of white carbon black, comprises the following steps:
Albite decomposes: the embodiment that the embodiment of this step of the present embodiment is decomposed with albite in embodiment 1 is substantially identical, and difference is: pre-warmed temperature is 200 DEG C, and the pre-warmed time is 15 minutes; The temperature of reaction is 200 DEG C, and the time of reaction is 2 hours;
Gas absorption is hydrolyzed: the embodiment of this step of the present embodiment is substantially identical with the embodiment of gas absorption in embodiment 1, and difference is: in described I and II absorption tower, temperature is respectively 85 DEG C;
Ammonia solution: the embodiment of this step of the present embodiment is substantially identical with the embodiment of ammonia solution in embodiment 1, and difference is: described hydrolyzed solution ammoniacal liquor adjusts pH=7.7, and digestion time is 1 hour, and Aging Temperature controls at 75 DEG C;
Rough white carbon black: the embodiment of this step of the present embodiment is identical with the embodiment preparing white carbon black in embodiment 1;
Refining white carbon black: the embodiment of this step of the present embodiment is substantially identical with the embodiment of the removal of Neutral ammonium fluoride in white carbon black in embodiment 1, difference is: the mass ratio of white carbon black crude product and water is 1:5, temperature is 65 DEG C, negative pressure is 70 handkerchiefs, rotating speed is 50 revs/min, and churning time is 3.5 hours.
Finally should be noted that: above embodiment is only in order to illustrate that technical scheme of the present invention is not intended to limit; Although with reference to preferred embodiment to invention has been detailed description, those of ordinary skill in the field are to be understood that: still can modify to the specific embodiment of the present invention or carry out equivalent replacement to portion of techniques feature; And not departing from the spirit of technical solution of the present invention, it all should be encompassed in the middle of the technical scheme scope of request of the present invention protection.
Claims (10)
1. a preparation method for white carbon black, comprises the following steps:
Albite decomposes: by albite, fluorite, 98% sulfuric acid mix according to the mass ratio of 1:1.55 ~ 2.57:3.28 ~ 4.62, and under 100 DEG C ~ 200 DEG C and autogenous pressure, be obtained by reacting solid residue and the gaseous products containing silicon fluoride;
Gas absorption is hydrolyzed: lead in I and II absorption tower successively by the described gaseous products containing silicon fluoride, be hydrolyzed the hydrolyzed solution obtained containing silicofluoric acid;
Ammonia solution: passed into by described hydrolyzed solution in ammonia solution still, by adding the method adjust ph of ammoniacal liquor; Ripening after neutralization, obtains dirty solution;
Rough white carbon black: be transported in pressure filter by described dirty solution and filter, obtains white carbon black precipitation, dry after washing, obtains white carbon black crude product;
Refining white carbon black: described white carbon black crude product and water are added in container according to the mass ratio being less than or equal to 1:1, is more than or equal to 40 DEG C in temperature and is uniformly mixed more than 1 hour under negative pressure state, make Neutral ammonium fluoride fully water-soluble; Filter, dry, obtained white carbon black finished product.
2. the preparation method of white carbon black according to claim 1, it is characterized in that: the step that described albite decomposes comprises: at 100 DEG C ~ 200 DEG C, preheat 15 minutes ~ 30 minutes to described albite and fluorite, removing moisture wherein, obtains dry albite and fluorite raw material; The sulfuric acid of 98% is joined reaction in the albite of described drying and fluorite raw material and within 2 hours ~ 5 hours, obtain solid residue containing calcium sulfate, sodium sulfate, Tai-Ace S 150 and ferric sulfate and the gaseous products containing silicon fluoride.
3. the preparation method of white carbon black according to claim 1, is characterized in that: the step of described gas absorption hydrolysis comprises:
Described gaseous products leads to through entering in one-level concentrated phase receiving tank after absorption liquid absorption, hydrolysis in described first grade absorption tower in described first grade absorption tower after dust removal filter filters, and the concentrated phase thing that described one-level concentrated phase receiving tank is collected is transported in ammonia solution still and carries out ammonia solution and ripening;
The liquid flooding that described one-level concentrated phase receiving tank is collected, to first order absorption circulation groove, is returned in described first grade absorption tower through pump and is continued to absorb;
Enter described two-level absorption tower absorption liquid in described two-level absorption tower by described first grade absorption tower tail gas out to absorb, continue hydrolysis, liquid after described two-level absorption tower hydrolysis enters secondary concentrated phase absorption cell, and the concentrated phase thing that described secondary concentrated phase absorption cell is collected is transported in described ammonia solution still and carries out ammonia solution and ripening;
When the fluorinion concentration detected in the silicate fluoride solution in described first order absorption circulation groove, described secondary absorption cycle groove reaches 10mol/L, absorption liquid reaches capacity, and is also transported to by described absorption liquid in described ammonia solution still and carries out ammonia solution and ripening;
Wherein, the absorption liquid in described I and II absorption tower is respectively the aqueous ethanolic solution that mass concentration is 10% ~ 30%, and in described I and II absorption tower, hydrolysis temperature is respectively 70 DEG C ~ 90 DEG C.
4. the preparation method of white carbon black according to claim 1, is characterized in that: in described aminolysis step, regulates the pH value of described hydrolyzed solution to be 7 ~ 8 by adding ammoniacal liquor.
5. the preparation method of white carbon black according to claim 1, is characterized in that: in described aminolysis step, and the time of described ripening is 1 hour ~ 2 hours, and the temperature of described ripening controls at 70 DEG C ~ 85 DEG C.
6. the preparation method of white carbon black according to claim 1, is characterized in that: in the step of described refining white carbon black, and the mass ratio of described white carbon black crude product and described water is 1:1 ~ 5.
7. the preparation method of white carbon black according to claim 1, is characterized in that: in the step of described refining white carbon black, and described temperature is 40 DEG C ~ 65 DEG C.
8. the preparation method of white carbon black according to claim 1, is characterized in that: in the step of described refining white carbon black, and described negative pressure is 10 handkerchief ~ 70 handkerchiefs.
9. the preparation method of the white carbon black according to claim 1 or 8, is characterized in that: in the step of described refining white carbon black, is uniformly mixed described in being undertaken by agitating vane, and the rotating speed of described agitating vane is 50 revs/min ~ 350 revs/min.
10. the preparation method of white carbon black according to claim 9, is characterized in that: in the step of described refining white carbon black, and described churning time is 1.0 hours ~ 3.5 hours.
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105036144A (en) * | 2015-07-10 | 2015-11-11 | 贵州远盛钾业科技有限公司 | Method for using acidic fluorine-containing silicon slag to prepare highly dispersable white carbon black |
CN107804851A (en) * | 2017-11-23 | 2018-03-16 | 达州励志环保科技有限公司 | The preparation method of white carbon |
CN108862287A (en) * | 2018-06-25 | 2018-11-23 | 确成硅化学股份有限公司 | The preparation method of high oil absorption high-dispersion white carbon black |
CN112143259A (en) * | 2020-10-16 | 2020-12-29 | 安徽锦华氧化锌有限公司 | Treatment process for improving reinforcing effect of white carbon black |
-
2014
- 2014-11-28 CN CN201410700622.5A patent/CN104445219A/en active Pending
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105036144A (en) * | 2015-07-10 | 2015-11-11 | 贵州远盛钾业科技有限公司 | Method for using acidic fluorine-containing silicon slag to prepare highly dispersable white carbon black |
CN105036144B (en) * | 2015-07-10 | 2017-06-16 | 贵州远盛钾业科技有限公司 | A kind of method that acid fluorine-containing white residue prepares high-dispersion white carbon black |
CN107804851A (en) * | 2017-11-23 | 2018-03-16 | 达州励志环保科技有限公司 | The preparation method of white carbon |
CN108862287A (en) * | 2018-06-25 | 2018-11-23 | 确成硅化学股份有限公司 | The preparation method of high oil absorption high-dispersion white carbon black |
CN112143259A (en) * | 2020-10-16 | 2020-12-29 | 安徽锦华氧化锌有限公司 | Treatment process for improving reinforcing effect of white carbon black |
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Application publication date: 20150325 |