CN101712476A - Method for preparing precipitated silica from tetrachlorosilane - Google Patents
Method for preparing precipitated silica from tetrachlorosilane Download PDFInfo
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Abstract
The invention belongs to a preparation method of inorganic materials, and in particular relates to a method for preparing precipitated silica from tetrachlorosilane, which comprises the following steps: enabling the tetrachlorosilane to directly react with water or alkaline water solution to generate precipitated silica hydrate pulp, and carrying out processes of solid-liquid separating, washing, drying and pulverizing on the obtained pulp to prepare the precipitated silica products with different applications, wherein the reaction temperature is 0-100 DEG C, the tetrachlorosilane accounts for 5%-70% of the total weight, the alkaline water solution is prepared by dissolving an alkaline matter in water, the mole ratio of the alkaline matter to the tetrachlorosilane is 1:0.25-2, a functional additive is also matched in the water or alkaline water solution, and the adding amount of the functional additive is 0-5% of the total amount. The invention has the characteristics of simple production processes, less equipment investment and low product cost, and the obtained product can be widely applied to the fields of rubber, food, plastics, daily health products and the like.
Description
Affiliated technical field: the invention belongs to the preparation method of inorganic materials, be specifically related to a kind of method for preparing precipitated silica with silicon tetrachloride.
Background technology: along with China's photovoltaic industry extra normal development in recent years, polysilicon approximately can form 20,000 tons/year throughput.And 1 ton of polysilicon of every production will produce 10-15 ton silicon tetrachloride byproduct.These silicon tetrachloride byproducts become waste owing to can not find " outlet ".How handling these wastes becomes the difficult problem of production of polysilicon enterprise.
Guangzhou Science and Technology Ji Sheng Industrial Co is the raw material production gas-phase silica with the silicon tetrachloride, is a better method of processing silicon chloride waste.But this method facility investment is big, and the products production cost is higher, thereby has restricted its product promotion.Therefore, also must look for another way, it is simple to find out a kind of production technique, and facility investment is little, and the novel method that product cost is low solves the problem of silicon tetrachloride waste.
Domestic most of manufacturing enterprise adopts the precipitator method (being the water glass acidization again) to produce precipitated silica, promptly adopts water glass solution and acid-respons, through precipitation, filter, washing, dry, calcine and obtain white carbon black.In recent years, also having reported many novel methods of producing precipitated silica, mainly is with nonmetalliferous ore and extension thereof to be the silicon source, adopts the precipitator method to prepare white carbon black.
Up to now, yet there are no the report for preparing precipitated silica with silicon tetrachloride.
Summary of the invention: the objective of the invention is in order to overcome the existing existing facility investment of silicon tetrachloride refuse processing method big, the technical barrier that the products production cost is higher, for people provide a kind of production technique simple, facility investment is little, and what product cost was low prepares the method for precipitated silica with silicon tetrachloride.
The objective of the invention is to realize by following technical proposals.
Of the present inventionly prepare the precipitated silica method of (claiming precipitated hydrated silica again) with silicon tetrachloride, be direct and water or alkaline aqueous solution reaction with silicon tetrachloride, generate the precipitated hydrated silica slurry, the slurry that obtains makes the precipitated silica product that satisfies different purposes through solid-liquid separation, washing, drying, disintegrating process; Temperature of reaction is generally 0-100 ℃ of scope, more fortunately 0-50 ℃ of scope.It is relatively good to consider that from the cost aspect temperature of reaction is controlled at room temperature.
In the such scheme, described alkaline aqueous solution is to be dissolved in the water by alkaline matter to form, used alkaline matter comprises mineral alkali and the organic bases that all can be water-soluble, as: ammonia, amine, water glass, sodium hydroxide, lime carbonate, silicate etc., preferably water glass and silicate; Count alkaline matter: silicon tetrachloride=1: 0.25～2 in molar ratio.
In the such scheme, is furnished with functional agent in described water or the alkaline aqueous solution, described functional agent can be stablizer, tensio-active agent, defoamer, properties-correcting agent etc., as: glycerine, polyoxyethylene glycol, Soxylat A 25-7, organic silicon emulsion etc., to regulate the performance of precipitated silica product.
In the such scheme, when described silicon tetrachloride directly reacted with water, silicon tetrachloride accounted for the 5%-70% of water and silicon tetrachloride gross weight, is preferably 15%-35%.
In the such scheme, when described silicon tetrachloride directly reacted with alkaline aqueous solution, silicon tetrachloride accounted for the 5%-70% of water, alkaline matter and silicon tetrachloride total mass, is preferably 15%-35%.
In the such scheme, the addition of described functional agent is 0～5% of a total amount, is preferably 0～1%; Described total amount is the total amount of water, silicon tetrachloride and functional agent or the total amount of water, alkaline matter, silicon tetrachloride and functional agent.
The present invention utilize produce in polysilicon and other industrial production byproduct---silicon tetrachloride is a raw material, by generating precipitated silica with the reaction of water or alkaline aqueous solution, following two kinds of different production technique are arranged: silicon tetrachloride is directly with the production technique of water prepared in reaction precipitated silica with silicon tetrachloride is direct and the production technique of alkaline aqueous solution prepared in reaction precipitated silica.
(1) silicon tetrachloride production technique direct and water prepared in reaction precipitated silica is as follows:
1. raw material and equipment:
(1) water can be all water such as underground water, rivers water, tap water, deionized water, distilled water.Take all factors into consideration from quality product and cost, preferentially select deionized water for use.
(2) required equipment, container and pipeline can be selected acidproof materials such as plastics, stainless steel, enamel, glass reinforced plastic for use in the production process, preferentially select enamel and glass reinforced plastic material for use.
(3) for regulating the performance of precipitated silica product, can in water, allocate some functional agents (comprising: stablizer, tensio-active agent, defoamer, properties-correcting agent etc.) into as glycerine, polyoxyethylene glycol, Soxylat A 25-7, organic silicon emulsion etc.
(4) when silicon tetrachloride and water hybrid reaction, silicon tetrachloride accounts for the mass percent of mixture (containing silicon tetrachloride, water) total mass between 5%-70%, preferred 15%-35%.
2. production technique:
(1) with silicon tetrachloride and water (can contain some functional agents) hybrid reaction by a certain percentage, feed way can take to drip, static mixed, spray one or more forms such as mixed.
(2) will go up step gained silicon-dioxide pulpous state liquid and carry out solid-liquid separation, can adopt filtration, precipitation, one or more forms such as centrifugal.Solid (precipitated silica crude product) changes next-step operation over to, and liquid (dilute hydrochloric acid) changes other containers store over to, treats the simmer down to concentrated hydrochloric acid.
(3) step gained precipitated silica crude product be will go up and neutrality or approaching neutral (pH value 5-8) will be washed with water to.Can directly wash with water, the waste water after washing reclaims as dilute hydrochloric acid.Also available buck (as one or more aqueous solution such as ammonia, sodium hydroxide, lime carbonate, silicate, yellow soda ash) washing, the waste water reclamation after washing or enter the environment protection emission program.
(4) will go up the precipitated silica drying that goes on foot after washing, one or more modes such as drying mode can adopt and bake and bank up with earth, calcining, hot gas flow drying.
(5) product of last step is pulverized, can be adopted one or more modes such as grinding, ball milling, comminution by gas stream, to regulate the performances such as specific surface area of precipitated silica product.
(6) packing.
(2) silicon tetrachloride directly prepares the production technique of precipitated silica with the reactant aqueous solution that shows alkalescence:
1. raw material and equipment:
(1) water can be all water such as underground water, rivers water, tap water, deionized water, distilled water.Take all factors into consideration from quality product and cost, preferentially select deionized water for use.
(2) used alkaline matter comprises mineral alkali and the organic bases that all can be water-soluble, as: ammonia, amine, water glass, sodium hydroxide, lime carbonate, silicate etc., preferably water glass and silicate.
(3) alkali in (2) is dissolved in (1) described water is alkaline aqueous solution.
(4) required equipment, container and pipeline can be selected acidproof materials such as plastics, stainless steel, enamel, glass reinforced plastic for use in the production process, preferentially select enamel and glass reinforced plastic material for use.
(5) for regulating the performance of precipitated silica product, can in water, allocate some functional agents (comprising: stablizer, tensio-active agent, defoamer, properties-correcting agent etc.) into as glycerine, polyoxyethylene glycol, Soxylat A 25-7, organic silicon emulsion etc.
When (6) silicon tetrachloride reacted with the aqueous solution that shows alkalescence, silicon tetrachloride accounted for mixture
The mass percent of (contain silicon tetrachloride, show the aqueous solution and the functional agent of alkalescence) total mass between 5%-70%, preferred 15%-35%.
2 production technique:
(1) with silicon tetrachloride and the aqueous solution (can contain some functional agents) that shows alkalescence hybrid reaction by a certain percentage, feed way can take to drip, static mixed, spray one or more forms such as mixed.
(2) will go up step gained silicon-dioxide pulpous state liquid and carry out solid-liquid separation, can adopt filtration, precipitation, one or more forms such as centrifugal.Solid (precipitated silica crude product) changes next-step operation over to, and liquid (salts solution) changes other containers store over to, waits to be recycled or environment protection emission.
(3) step gained precipitated silica crude product be will go up and neutrality or approaching neutral (pH value 5-8) will be washed with water to.Can directly wash also available buck (as one or more aqueous solution such as ammonia, sodium hydroxide, lime carbonate, silicate, yellow soda ash) washing, the waste water reclamation after washing or enter the environment protection emission program with water.
(4) will go up the precipitated silica drying that goes on foot after washing, one or more modes such as drying mode can adopt and bake and bank up with earth, calcining, hot gas flow drying.
(5) product of last step is pulverized, can be adopted one or more modes such as grinding, ball milling, comminution by gas stream, to regulate the performances such as specific surface area of precipitated silica product.
(6) packing.
The present inventor is through research, discovery is direct and water or apparent alkaline reactant aqueous solution with silicon tetrachloride, can prepare precipitated silica easily, compared with prior art, it is simple that it has production technique, facility investment is little, the characteristics that product cost is low, for in polysilicon and other industrial production byproduct---silicon tetrachloride has solved " three wastes " and has utilized problem, technology is simply suitable, the precipitated silica of producing (precipitated hydrated silica) product cost low, products obtained therefrom can be widely used in fields such as rubber, food, plastics, daily use chemicals.
Embodiment:
The invention is further illustrated by the following examples, and the present invention is not limited only to described embodiment.
Embodiment one
Add 640 kilograms of deionized waters in 1000 liters of enamel stills, start stirring, control still temperature is no more than 50 ℃, drips silicon tetrachloride gradually, through 3 hours, adds 160 kilograms of silicon tetrachlorides altogether.Then above-mentioned soup compound is put into 1000 liters of plastic tanks, left standstill 24 hours.Filter with 60 order copper mesh, gained liquid is sent into storage tank as dilute hydrochloric acid.Solid after filtering in a plastics rinse bath, was used rinsed with deionized water 15 minutes while stirring, until pH value near 7.Filter with 60 order copper mesh, gained filter cake centrifuge dewatering is transported in the pneumatic drier dry more again.Products obtained therefrom, after tested, its physical and chemical performance is as follows:
(1) dioxide-containing silica: 93%; (2) screenings (45um) 0.1;
(3) weight loss on heating: 2%; (4) burning decrement: 6%;
(5) pH value: 6-7; (6) total iron-holder: 12mg/kg;
Embodiment two
Add 640 kilograms of bucks (contain 115 kilograms of water glass, all the other are deionized water) in 1000 liters of enamel stills, start stirring, control still temperature is no more than 50 ℃, drips silicon tetrachloride gradually, through 3 hours, adds 80 kilograms of silicon tetrachlorides altogether.Count water glass: silicon tetrachloride=1: 0.5 in molar ratio.Then above-mentioned soup compound is put into 1000 liters of plastic tanks, left standstill 24 hours.Filter with 60 order copper mesh, the solid after filtering in a plastics rinse bath, used rinsed with deionized water 15 minutes while stirring, until pH value near 7.Filter with 60 order copper mesh, gained filter cake centrifuge dewatering is transported in the pneumatic drier dry more again.Products obtained therefrom, after tested, its physical and chemical performance is as follows:
(1) dioxide-containing silica: 93%; (2) screenings (45um) 0;
(3) weight loss on heating: 2%; (4) burning decrement: 6%;
(5) pH value: 6-7; (6) total iron-holder: 125mg/kg.
Embodiment three
The consumption that dewaters is 760 kilograms, and the silicon tetrachloride consumption is outside 40 kilograms, and all the other are with embodiment one.Products obtained therefrom, after tested, its physical and chemical performance is as follows:
(1) dioxide-containing silica: 93%; (2) screenings (45um) 0;
(3) weight loss on heating: 2%; (4) burning decrement: 6%;
(5) pH value: 6-7; (6) total iron-holder: 12mg/kg;
Embodiment four
The consumption that dewaters is 240 kilograms, and the silicon tetrachloride consumption is outside 560 kilograms, and all the other are with embodiment one.Products obtained therefrom, after tested, its physical and chemical performance is as follows:
(1) dioxide-containing silica: 90%; (2) screenings (45um) 0.5;
(3) weight loss on heating: 3%; (4) burning decrement: 8%;
(5) pH value: 6-7; (6) total iron-holder: 13mg/kg;
Embodiment five
The consumption that dewaters is 680 kilograms, and the silicon tetrachloride consumption is outside the 120 kg, and all the other are with embodiment one.Products obtained therefrom, after tested, its physical and chemical performance is as follows:
(1) dioxide-containing silica: 92%; (2) screenings (45um) 0.1;
(3) weight loss on heating: 2%; (4) burning decrement: 6%;
(5) pH value: 6-7; (6) total iron-holder: 12mg/kg;
Embodiment six
The consumption that dewaters is 520 kilograms, and the silicon tetrachloride consumption is outside 280 kilograms, and all the other are with embodiment one.Products obtained therefrom, after tested, its physical and chemical performance is as follows:
(1) dioxide-containing silica: 91%; (2) screenings (45um) 0.3;
(3) weight loss on heating: 2%; (4) burning decrement: 7%;
(5) pH value: 6-7; (6) total iron-holder: 13mg/kg;
Embodiment seven
The consumption that dewaters is 600 kilograms, and the silicon tetrachloride consumption is 160 kilograms, and the consumption of glycerine is outside 40 kilograms, and all the other are with embodiment one.Products obtained therefrom, after tested, its physical and chemical performance is as follows:
(1) dioxide-containing silica: 93%; (2) screenings (45um) 0;
(3) weight loss on heating: 2%; (4) burning decrement: 6%;
(5) pH value: 6-7; (6) total iron-holder: 12mg/kg;
Embodiment eight
The consumption that dewaters is 616 kilograms, and the silicon tetrachloride consumption is 160 kilograms, and the consumption of polyoxyethylene glycol is outside 24 kilograms, and all the other are with embodiment one.Products obtained therefrom, after tested, its physical and chemical performance is as follows:
(1) dioxide-containing silica: 93%; (2) screenings (45um) 0;
(3) weight loss on heating: 2%; (4) burning decrement: 6%;
(5) pH value: 6-7; (6) total iron-holder: 12mg/kg;
Embodiment nine
The consumption that dewaters is 632 kilograms, and the silicon tetrachloride consumption is 160 kilograms, and the consumption of Soxylat A 25-7 is outside 8 kilograms, and all the other are with embodiment one.Products obtained therefrom, after tested, its physical and chemical performance is as follows:
(1) dioxide-containing silica: 93%; (2) screenings (45um) 0;
(3) weight loss on heating: 2%; (4) burning decrement: 6%;
(5) pH value: 6-7; (6) total iron-holder: 12mg/kg;
Embodiment ten
The consumption that dewaters is 624 kilograms, and the silicon tetrachloride consumption is 160 kilograms, and the consumption of organic silicon emulsion is outside 16 kilograms, and all the other are with embodiment one.Products obtained therefrom, after tested, its physical and chemical performance is as follows:
(1) dioxide-containing silica: 92%; (2) screenings (45um) 0;
(3) weight loss on heating: 2%; (4) burning decrement: 6%;
(5) pH value: 6-7; (6) total iron-holder: 12mg/kg;
Embodiment 11
The consumption that removes buck (contain 112 kilograms of ammonia, all the other are deionized water) is 504 kilograms, and the silicon tetrachloride consumption is 280 kilograms, and the consumption of Soxylat A 25-7 is outside 16 kilograms, and all the other are with embodiment two.Count ammonia: silicon tetrachloride=1: 0.25 in molar ratio.Products obtained therefrom, after tested, its physical and chemical performance is as follows:
(1) dioxide-containing silica: 93%; (2) screenings (45um) 0.5;
(3) weight loss on heating: 2%; (4) burning decrement: 6%;
(5) pH value: 6-7; (6) total iron-holder: 220mg/kg;
Embodiment 12
The consumption that removes buck (contain 28 kilograms of quadrols, all the other are deionized water) is 640 kilograms, and the silicon tetrachloride consumption is 80 kilograms, and the consumption of polyoxyethylene glycol is outside 1 kilogram, and all the other are with embodiment two.Count quadrol: silicon tetrachloride=1: 1 in molar ratio.Products obtained therefrom, after tested, its physical and chemical performance is as follows:
(1) dioxide-containing silica: 93%; (2) screenings (45um) 0;
(3) weight loss on heating: 2%; (4) burning decrement: 6%;
(5) pH value: 6-7; (6) total iron-holder: 163mg/kg;
Embodiment 13
The consumption that removes buck (contain 38 kilograms of sodium hydroxide, all the other are deionized water) is 744 kilograms, and the silicon tetrachloride consumption is 40 kilograms, and the consumption of glycerine is outside 16 kilograms, and all the other are with embodiment two.Count sodium hydroxide: silicon tetrachloride=1: 0.25 in molar ratio.Products obtained therefrom, after tested, its physical and chemical performance is as follows:
(1) dioxide-containing silica: 93%; (2) screenings (45um) 0;
(3) weight loss on heating: 2%; (4) burning decrement: 6%;
(5) pH value: 6-7; (6) total iron-holder: 80mg/kg;
Embodiment 14
Add 640 kilograms of deionized waters in 1000 liters of enamel stills, start stirring, control still temperature is no more than 5 ℃, drips silicon tetrachloride gradually, through 6 hours, adds 160 kilograms of silicon tetrachlorides altogether.Then above-mentioned soup compound is put into 1000 liters of plastic tanks, left standstill 24 hours.Filter with 60 order copper mesh, gained liquid is sent into storage tank as dilute hydrochloric acid.Solid after filtering in a plastics rinse bath, was used rinsed with deionized water 15 minutes while stirring, until pH value near 7.Filter with 60 order copper mesh, gained filter cake centrifuge dewatering is transported in the pneumatic drier dry more again.Products obtained therefrom, after tested, its physical and chemical performance is as follows:
(1) dioxide-containing silica: 92%; (2) screenings (45um) 0;
(3) weight loss on heating: 3%; (4) burning decrement: 7%;
(5) pH value: 6-7; (6) total iron-holder: 12mg/kg;
Embodiment 15
Add 640 kilograms of deionized waters in 1000 liters of enamel stills, start stirring, control still temperature drips silicon tetrachloride (hydrogen chloride gas is discharged special disposal by pipeline) gradually between 95 ℃-100 ℃, through 6 hours, add 160 kilograms of silicon tetrachlorides altogether.With putting into 1000 liters of plastic tanks after the above-mentioned soup compound cooling, left standstill 24 hours then.Filter with 60 order copper mesh, gained liquid is sent into storage tank as dilute hydrochloric acid.Solid after filtering in a plastics rinse bath, was used rinsed with deionized water 15 minutes while stirring, until pH value near 7.Filter with 60 order copper mesh, gained filter cake centrifuge dewatering is transported in the pneumatic drier dry more again.Products obtained therefrom, after tested, its physical and chemical performance is as follows:
(1) dioxide-containing silica: 93%; (2) screenings (45um) 0.5;
(3) weight loss on heating: 3%; (4) burning decrement: 6%;
(5) pH value: 6-7; (6) total iron-holder: 12mg/kg;
Embodiment 16
Remove outside the buck (water glass that contains 200 kilograms of degree Beaume 40, all the other are deionized water),
All the other are with embodiment two.Temperature of reaction is 0 ℃.Products obtained therefrom, after tested, its physical and chemical performance is as follows:
(1) dioxide-containing silica: 93%; (2) screenings (45um) 0;
(3) weight loss on heating: 2%; (4) burning decrement: 6%;
(5) pH value: 6-7; (6) total iron-holder: 106mg/kg.
Claims (10)
1. method for preparing precipitated silica with silicon tetrachloride, it is characterized in that it being direct and water or alkaline aqueous solution reaction with silicon tetrachloride, generate the precipitated hydrated silica slurry, the slurry that obtains makes the precipitated silica product that satisfies different purposes through solid-liquid separation, washing, drying, disintegrating process; Temperature of reaction is 0-100 ℃.
2. according to claim 1ly prepare the method for precipitated silica, it is characterized in that described temperature of reaction is 0-50 ℃ with silicon tetrachloride.
3. according to claim 1ly prepare the method for precipitated silica with silicon tetrachloride, when it is characterized in that described silicon tetrachloride directly reacts with water, silicon tetrachloride accounts for the 5%-70%. of water and silicon tetrachloride gross weight
4. according to claim 1ly prepare the method for precipitated silica with silicon tetrachloride, when it is characterized in that described silicon tetrachloride directly reacts with water, silicon tetrachloride accounts for the 15%-35% of water and silicon tetrachloride gross weight.
5. according to claim 1ly prepare the method for precipitated silica with silicon tetrachloride, when it is characterized in that described silicon tetrachloride directly reacts with alkaline aqueous solution, silicon tetrachloride accounts for the 5%-70% of water, alkaline matter and silicon tetrachloride total mass.
6. according to claim 1ly prepare the method for precipitated silica with silicon tetrachloride, when it is characterized in that described silicon tetrachloride directly reacts with alkaline aqueous solution, silicon tetrachloride accounts for the 15%-35% of water, alkaline matter and silicon tetrachloride total mass.
7. the method for preparing precipitated silica with silicon tetrachloride according to claim 1, it is characterized in that described alkaline aqueous solution is to be dissolved in the water by alkaline matter to form, used alkaline matter comprises mineral alkali and the organic bases that all can be water-soluble, count alkaline matter: silicon tetrachloride=1: 0.25～2 in molar ratio.
8. according to claim 7ly prepare the method for precipitated silica, it is characterized in that described mineral alkali and organic bases are ammonia, amine, water glass, sodium hydroxide, lime carbonate, silicate with silicon tetrachloride.
9. the method for preparing precipitated silica with silicon tetrachloride according to claim 1, it is characterized in that being furnished with functional agent in described water or the alkaline aqueous solution, described functional agent is stablizer, tensio-active agent, defoamer, properties-correcting agent, and the addition of described functional agent is 0～5% of a total amount.
10. according to claim 9ly prepare the method for precipitated silica with silicon tetrachloride, it is characterized in that described functional agent specifically is meant glycerine, polyoxyethylene glycol, Soxylat A 25-7, organic silicon emulsion, addition is 0～1% of a total amount.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101891213A (en) * | 2010-07-20 | 2010-11-24 | 乌洪涛 | Method for preparing water glass from byproduct silicon tetrachloride |
| CN101898764A (en) * | 2010-07-30 | 2010-12-01 | 天津大学 | Method for transforming silicon tetrachloride to fine silica powder |
| CN101973556A (en) * | 2010-10-26 | 2011-02-16 | 昊华宇航化工有限责任公司 | Method for preparing white carbon black by precipitation method |
| CN102001671A (en) * | 2010-12-15 | 2011-04-06 | 湘潭大学 | Method for preparing white carbon black by using silicon tetrachloride |
| CN102180470A (en) * | 2011-04-07 | 2011-09-14 | 赵志军 | Method for recycling silicon tetrachloride as by-product of polycrystalline silicon |
| CN102432026A (en) * | 2011-10-21 | 2012-05-02 | 安徽祥源安全环境科学技术有限公司 | Method for preparing white carbon black from polysilicon byproduct silicon tetrachloride |
| CN102659118A (en) * | 2012-04-24 | 2012-09-12 | 湖南工业大学 | Method for producing food grade white carbon black by silicon tetrachloride |
| CN104477923A (en) * | 2014-11-28 | 2015-04-01 | 新沂市天悦石英有限公司 | Method for preparing silicon dioxide powder from silicon tetrachloride |
| CN109336121A (en) * | 2018-12-11 | 2019-02-15 | 怀化学院 | Overcritical white carbon black and preparation method thereof |
| CN113731415A (en) * | 2021-09-28 | 2021-12-03 | 江苏金聚合金材料有限公司 | Preparation method and application of ethylene glycol catalyst |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101891213A (en) * | 2010-07-20 | 2010-11-24 | 乌洪涛 | Method for preparing water glass from byproduct silicon tetrachloride |
| CN101898764A (en) * | 2010-07-30 | 2010-12-01 | 天津大学 | Method for transforming silicon tetrachloride to fine silica powder |
| CN101973556B (en) * | 2010-10-26 | 2012-10-03 | 昊华宇航化工有限责任公司 | Method for preparing white carbon black by precipitation method |
| CN101973556A (en) * | 2010-10-26 | 2011-02-16 | 昊华宇航化工有限责任公司 | Method for preparing white carbon black by precipitation method |
| CN102001671A (en) * | 2010-12-15 | 2011-04-06 | 湘潭大学 | Method for preparing white carbon black by using silicon tetrachloride |
| CN102180470A (en) * | 2011-04-07 | 2011-09-14 | 赵志军 | Method for recycling silicon tetrachloride as by-product of polycrystalline silicon |
| CN102180470B (en) * | 2011-04-07 | 2012-11-21 | 赵志军 | Method for recycling silicon tetrachloride as by-product of polycrystalline silicon |
| CN102432026B (en) * | 2011-10-21 | 2013-08-14 | 安徽祥源安全环境科学技术有限公司 | Method for preparing white carbon black from polysilicon byproduct silicon tetrachloride |
| CN102432026A (en) * | 2011-10-21 | 2012-05-02 | 安徽祥源安全环境科学技术有限公司 | Method for preparing white carbon black from polysilicon byproduct silicon tetrachloride |
| CN102659118A (en) * | 2012-04-24 | 2012-09-12 | 湖南工业大学 | Method for producing food grade white carbon black by silicon tetrachloride |
| CN104477923A (en) * | 2014-11-28 | 2015-04-01 | 新沂市天悦石英有限公司 | Method for preparing silicon dioxide powder from silicon tetrachloride |
| CN109336121A (en) * | 2018-12-11 | 2019-02-15 | 怀化学院 | Overcritical white carbon black and preparation method thereof |
| CN113731415A (en) * | 2021-09-28 | 2021-12-03 | 江苏金聚合金材料有限公司 | Preparation method and application of ethylene glycol catalyst |
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