CN102320613A - Method for hydrolyzing chlorosilane - Google Patents
Method for hydrolyzing chlorosilane Download PDFInfo
- Publication number
- CN102320613A CN102320613A CN201110149586A CN201110149586A CN102320613A CN 102320613 A CN102320613 A CN 102320613A CN 201110149586 A CN201110149586 A CN 201110149586A CN 201110149586 A CN201110149586 A CN 201110149586A CN 102320613 A CN102320613 A CN 102320613A
- Authority
- CN
- China
- Prior art keywords
- water
- chlorosilane
- milk sap
- solvent
- silicon tetrachloride
- 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
Abstract
The invention discloses a method for hydrolyzing chlorosilane. The method comprises the following steps of: (1) mixing emulsifier, water and water-insoluble solvent uniformly in a mass ratio of the emulsifier to the water of (0.005-0.2): 1 and a volume ratio of the water to the water-insoluble solvent of (0.05-0.9): 1 to form emulsion; (2) mixing the chlorosilane and the water-insoluble solvent in a volume of (1-25): 1 to form chlorosilane solution; and (3) mixing the emulsion prepared in the step (1) and the chlorosilane solution prepared in the step (2), reacting the mixture for 1 to 120 minutes, and generating silicon dioxide/silicate powder particles containing 60 weight percent of water and hydrogen chloride gas, wherein the mole number ratio of the water in the emulsion to the chlorosilane in the chlorosilane solution is 1: (0.2-2).
Description
Technical field
The invention belongs to the compound hydrolysis field, particularly a kind of method that chlorosilane is hydrolyzed.
Background technology
Wasserstoffatoms in the silane (SiH4) is generically and collectively referred to as chlorosilane after being replaced by the chlorine atom, and general formula is HnSiCl4-n, in the formula, and n=0,1,2,3, so chlorosilane comprises a chlorosilane, dichlorosilane, trichlorosilane (trichlorosilane) and silicon tetrachloride.Along with the development of China's polysilicon and organosilicon industry, the by product chlorosilane is owing to output is high, toxicity becomes serious environmental hidden danger greatly.Present said by product chlorosilane; Particularly the main processing approach of silicon tetrachloride is that to be used for the white carbon black of production gas phase, tetraethyl silicate, organosilicon and hydro-reduction be trichlorosilane; But these approach still are difficult to digest a large amount of silicon tetrachlorides, and investment is big, technical sophistication or cost are high.
Application number is that the one Chinese patent application of 200810044476.X discloses a kind of " recoverying and utilizing method of silicon tetrachloride in the production process of trichlorosilane ", and this method adopts Hydrogen chloride that silicon tetrachloride is hydrolyzed.Application number is that the one Chinese patent application of 200510043027.X discloses " a kind of preparation method of nanometer grade silica powder "; This method employing directly joins silicon tetrachloride reacts hydrolysis of silicon tetrachloride in the deionized water, and to the silicic acid grading extraction that generates, the silicon dioxide granule that drying obtains different size.Because hydrolysis obtains chlorosilane in water or Hydrogen chloride with wetting ability silicic acid is to contain a large amount of water (water cut surpasses 100wt%) in the master's deposition, therefore will obtain the higher energy consumption of exsiccant silicon-dioxide powdery needs.
Summary of the invention
The method that the purpose of this invention is to provide a kind of chlorosilane hydrolysis, reducing the water cut that the chlorosilane hydrolysis is obtained the silica/silicon acid sludge, thereby save energy reduces production costs.
The method of chlorosilane hydrolysis according to the invention, its process step is following:
(1) preparation milk sap
With emulsifying agent, water, with the immiscible solvent of water be raw material; Emulsifying agent quality: the quality of water=0.005～0.2: 1; The volume of water: with volume=0.05～0.9 of the immiscible solvent of water: 1; Under normal pressure, room temperature (indoor natural temperature),, promptly form milk sap with emulsifying agent, water, even with the immiscible solvent of water;
(2) preparation chlorosilane solution
With chlorosilane, with the immiscible solvent of water be raw material, chlorosilane volume:, under normal pressure, room temperature (indoor natural temperature), with chlorosilane, mix, promptly form chlorosilane solution with the immiscible solvent phase of water with volume=1: 1～25 of the immiscible solvent of water;
(3) hydrolysis reaction
With the milk sap of step (1) preparation and the chlorosilane solution of step (2) preparation is raw material; The proportioning of said milk sap and chlorosilane solution is the mole number of water in the milk sap: the mole number of chlorosilane in the chlorosilane solution=1: 0.2～2; Said milk sap is mixed with chlorosilane solution mutually; Normal pressure, room temperature (indoor natural temperature)～50 ℃ reaction 1 minute～120 minutes, promptly generate silica/silicon acid powder and the hydrogen chloride gas of water cut less than 60wt%.
The method of chlorosilane hydrolysis according to the invention; Preparation milk sap used emulsifying agent is at least a in the acid of hydrophile-lipophile balance value (being called for short HLB) less than 20, ester, the ether; Preferred hydrophile-lipophile balance value is 3～9 acid, ester, ether, is 5 Brij92, glyceryl monostearate etc. like Span series, HLB.
The method of chlorosilane hydrolysis according to the invention, preparation milk sap and preparation chlorosilane solution solvent for use are 30 ℃～250 ℃ organic solvent for depress boiling point at a standard atmosphere.Said organic solvent is at least a in pentane, normal hexane, hexanaphthene, heptane, octane, sherwood oil, petroleum naphtha, solvent oil, gasoline, kerosene, the diesel oil, preferred normal hexane, hexanaphthene, sherwood oil, solvent oil, kerosene.Preparation milk sap can be identical with the selected concrete organic solvent of preparation chlorosilane solution, also can be different, preferably identical.
The present invention has following beneficial effect:
The water cut of the silica/silicon acid powder that 1, the method for chlorosilane hydrolysis according to the invention, its hydrolysis directly produce is no more than 60wt%, compared with prior art, effectively reduces the water cut of the silica/silicon acid powder that the chlorosilane hydrolysis produced.
2, the method for the invention technology is simple, and equipment used is a conventional equipment, helps realizing suitability for industrialized production.
Embodiment
Through embodiment the method for chlorosilane hydrolysis according to the invention is described further below.
Embodiment 1
The process step of present embodiment is following:
(1) is raw material with 1.6 gram Span20 (emulsifying agent), 10mL tap water, 30mL normal hexane (solvent), under room temperature, normal pressure, Span20, tap water and normal hexane mixed, promptly form milk sap;
(2) be raw material with 40mL silicon tetrachloride and 50mL normal hexane (solvent), under room temperature, normal pressure, join silicon tetrachloride in the normal hexane and stir, promptly form silicon tetrachloride solution;
(3) under agitation the milk sap of step (1) preparation is joined in the silicon tetrachloride solution of step (2) preparation (mol ratio of water and silicon tetrachloride is about 1: 0.6); Refluxed 30 minutes in normal pressure, 50 ℃; After return time expires; From the reaction feed liquid, filter out silica/silicon acid powder, after the contained normal hexane volatilization of silica/silicon acid powder, recording its water cut is 20wt%, obtains SiO 2 powder 150～200 ℃ of oven dry.The hydrogen chloride gas that produces in reaction process water after removing silicon tetrachloride wherein absorbs the concentrated hydrochloric acid that obtains 31wt%.
Embodiment 2
The process step of present embodiment is following:
(1) is that 60～90 ℃ sherwood oil (solvent) is a raw material with 0.33 gram Span80 (emulsifying agent), 36mL tap water, 100mL boiling range, under room temperature, normal pressure, Span80 is dissolved in sherwood oil, tap water is joined in this solution mix again, promptly form milk sap;
(2) be raw material with 150mL silicon tetrachloride and 150mL normal hexane (solvent), under room temperature, normal pressure, join silicon tetrachloride in the normal hexane and stir, promptly form silicon tetrachloride solution;
(3) under agitation the milk sap of step (1) preparation is joined in the silicon tetrachloride solution of step (2) preparation (mol ratio of water and silicon tetrachloride is about 1: 0.7); Behind reinforced the finishing; Under agitation, after the reaction times expires, from the reaction feed liquid, filter out silica/silicon acid powder in normal pressure, room temperature reaction 30 minutes; After the contained organic solvent volatilization of silica/silicon acid powder, recording its water cut is 25wt%, obtains SiO 2 powder 150～200 ℃ of oven dry.The hydrogen chloride gas that produces in reaction process water after removing silicon tetrachloride wherein absorbs the concentrated hydrochloric acid that obtains 31wt%.
Embodiment 3
The process step of present embodiment is following:
(1) with 1 gram oleic acid (emulsifying agent), 36mL tap water, 100mL boiling range be 30～60 ℃ sherwood oil (solvent) be raw material, under room temperature, normal pressure, oleic acid is dissolved in sherwood oil, tap water is joined in this solution mix again, promptly form milk sap;
(2) be raw material with 100mL silicon tetrachloride and 200mL normal hexane (solvent), under room temperature, normal pressure, join silicon tetrachloride in the normal hexane and stir, promptly form silicon tetrachloride solution;
(3) under agitation the milk sap of step (1) preparation is joined in the silicon tetrachloride solution of step (2) preparation (mol ratio of water and silicon tetrachloride is about 1: 0.4); Behind reinforced the finishing; Under agitation, after the reaction times expires, from the reaction feed liquid, filter out silica/silicon acid powder in normal pressure, room temperature reaction 60 minutes; After the contained organic solvent volatilization of silica/silicon acid powder, recording its water cut is 28wt%, obtains SiO 2 powder 100～200 ℃ of oven dry.The hydrogen chloride gas that produces in reaction process water after removing silicon tetrachloride wherein absorbs the concentrated hydrochloric acid that obtains 31wt%.
Embodiment 4
The process step of present embodiment is following:
(1) is that 60～90 ℃ sherwood oil (solvent) is a raw material with 1.25 gram Span20 (emulsifying agent), 36mL tap water, 100mL boiling range, under room temperature, normal pressure, Span20 is dissolved in sherwood oil, tap water is joined in this solution mix again, promptly form milk sap;
(2) be raw material with 50mL silicon tetrachloride as by-product of polysilicon (containing a small amount of trichlorosilane) and 500mL normal hexane, under room temperature, normal pressure, join silicon tetrachloride as by-product of polysilicon in the normal hexane and stir, promptly form silicon tetrachloride solution;
(3) silicon tetrachloride solution of under normal pressure, room temperature, the milk sap and the step (2) of step (1) preparation being prepared is in the reaction vessel that joined continuously respectively 1: 4 (mol ratio of water and silicon tetrachloride and trichlorosilane total amount is about 1: 0.2) under stirring by volume; Behind reinforced the finishing; Under agitation continue reaction 20 minutes; After reaction times expires; From the reaction feed liquid, filter out silica/silicon acid powder, after the contained organic solvent volatilization of silica/silicon acid powder, recording its water cut is 60wt%, obtains SiO 2 powder 100～200 ℃ of oven dry.The hydrogen chloride gas that produces in the reaction process is collected after removing silicon tetrachloride and organic solvent wherein, obtains the gas that the hydrogen chloride gas body burden is 98v%.
Embodiment 5
The process step of present embodiment is following:
(1) is that 5 Brij92 (emulsifying agent), 40mL tap water, 100mL kerosene (solvent) are raw material with 2.0 gram HLB, under room temperature, normal pressure, said Brij92 and tap water joined in the kerosene and mix, promptly form milk sap;
(2) be raw material with 50mL silicon tetrachloride as by-product of polysilicon (containing a small amount of trichlorosilane) and 500mL normal hexane, under room temperature, normal pressure, join said silicon tetrachloride as by-product of polysilicon in the normal hexane and stir, promptly form silicon tetrachloride solution;
(3) silicon tetrachloride solution of under normal pressure, room temperature, the milk sap and the step (2) of step (1) preparation being prepared is in the reaction vessel that joined continuously respectively 1: 10 (mol ratio of water and silicon tetrachloride and trichlorosilane total amount is about 1: 0.5) under stirring by volume; Behind reinforced the finishing; Under agitation continue reaction 30 minutes; After reaction times expires; From the reaction feed liquid, filter out silica/silicon acid powder, after the contained organic solvent volatilization of silica/silicon acid powder, recording its water cut is 29wt%, obtains SiO 2 powder 150～200 ℃ of oven dry.The hydrogen chloride gas that produces in reaction process water after removing silicon tetrachloride and kerosene wherein absorbs the concentrated hydrochloric acid that obtains 31wt%.
Embodiment 6
The process step of present embodiment is following:
(1) with 2.5 gram glyceryl monostearates (emulsifying agent), 1 gram T 46155 oleyl alcohol (emulsifying agent), 40mL tap water, 100mL soybean extracting solvent no.6 (" GB 16629-1996 "; Solvent) is raw material; Under room temperature, normal pressure, said glyceryl monostearate, T 46155 oleyl alcohol and tap water joined in the soybean extracting solvent no.6 and mix, promptly form milk sap;
(2) be raw material with 50mL trichlorosilane silicon tetrachloride as by-product and 500mL normal hexane, under room temperature, normal pressure, join said trichlorosilane silicon tetrachloride as by-product in the normal hexane and stir, promptly form silicon tetrachloride solution;
(3) silicon tetrachloride solution of under normal pressure, room temperature, the milk sap and the step (2) of step (1) preparation being prepared is in the reaction vessel that joined continuously respectively 1: 10 (mol ratio of water and silicon tetrachloride is about 1: 0.5) under stirring by volume; Behind reinforced the finishing; Under agitation continue reaction 60 minutes; After reaction times expires; From the reaction feed liquid, filter out silica/silicon acid powder, after the contained organic solvent volatilization of silica/silicon acid powder, recording its water cut is 25wt%, obtains SiO 2 powder 150～200 ℃ of oven dry.The hydrogen chloride gas that produces in the reaction process is collected after removing silicon tetrachloride and solvent oil wherein, obtains the gas that the hydrogen chloride gas body burden is 98v%.
Embodiment 7
The process step of present embodiment is following:
(1) be that 1: 1: 1 normal hexane, hexanaphthene, the mixed solution (solvent) of heptane are raw material with 2.5 gram glyceryl monostearates (emulsifying agent), 40mL tap water, 100mL volume ratio; Under room temperature, normal pressure, said glyceryl monostearate and tap water joined in the said mixed solvent and mix, promptly form milk sap;
(2) be raw material with 50mL silicon tetrachloride as by-product of polysilicon (containing a small amount of trichlorosilane) and 500mL normal hexane, under room temperature, normal pressure, join said silicon tetrachloride as by-product of polysilicon in the normal hexane and stir, promptly form silicon tetrachloride solution;
(3) silicon tetrachloride solution of under normal pressure, room temperature, the milk sap and the step (2) of step (1) preparation being prepared is in the reaction vessel that joined continuously respectively 1: 10 (mol ratio of water and silicon tetrachloride and trichlorosilane total amount is about 1: 0.5) under stirring by volume; Behind reinforced the finishing; Under agitation continue reaction 60 minutes; After reaction times expires; From the reaction feed liquid, filter out silica/silicon acid powder, after the contained organic solvent volatilization of silica/silicon acid powder, recording its water cut is 28wt%, obtains SiO 2 powder 150～200 ℃ of oven dry.The hydrogen chloride gas that produces in the reaction process is collected after removing silicon tetrachloride and organic solvent wherein, obtains the gas that the hydrogen chloride gas body burden is 98v%.
Embodiment 8
The process step of present embodiment is following:
(1) is that 60～90 ℃ sherwood oil (solvent) is a raw material with 1.25 gram Span20 (emulsifying agent), 36mL tap water, 100mL boiling range, under room temperature, normal pressure, said Span20 is dissolved in said sherwood oil, add tap water again and mix, promptly form milk sap;
(2) be raw material with 40mL trichlorosilane silicon tetrachloride as by-product and 1000mL normal hexane, under room temperature, normal pressure, join said trichlorosilane silicon tetrachloride as by-product in the normal hexane and stir, promptly form silicon tetrachloride solution;
(3) silicon tetrachloride solution of under normal pressure, room temperature, the milk sap and the step (2) of step (1) preparation being prepared is in the reaction vessel that joined continuously respectively 1: 20 (mol ratio of water and silicon tetrachloride is about 1: 0.5) under stirring by volume; Behind reinforced the finishing; Under agitation continue reaction 20 minutes; After reaction times expires; From the reaction feed liquid, filter out silica/silicon acid powder, after the contained organic solvent volatilization of silica/silicon acid powder, recording its water cut is 30wt%, obtains SiO 2 powder 150～200 ℃ of oven dry.The hydrogen chloride gas that produces in the reaction process is collected after removing silicon tetrachloride and sherwood oil wherein, obtains the gas that the hydrogen chloride gas body burden is 98v%.
Embodiment 9
The process step of present embodiment is following:
(1) is that 60～90 ℃ sherwood oil (solvent) is a raw material with 1.25 gram Span80 (emulsifying agent), 18mL tap water, 100mL boiling range, under room temperature, normal pressure, said Span80 is dissolved in said sherwood oil, add tap water again and mix, promptly form milk sap;
(2) be raw material with 230mL silicon tetrachloride as by-product of polysilicon (containing a small amount of trichlorosilane) and 1000mL normal hexane, under room temperature, normal pressure, join said silicon tetrachloride as by-product of polysilicon in the normal hexane and stir, promptly form silicon tetrachloride solution;
(3) silicon tetrachloride solution of under normal pressure, room temperature, the milk sap and the step (2) of step (1) preparation being prepared is in the reaction vessel that joined continuously respectively 1: 10 (mol ratio of water and silicon tetrachloride and trichlorosilane total amount is about 1: 2) under stirring by volume; Behind reinforced the finishing; Under agitation continue reaction 120 minutes; After reaction times expires; From the reaction feed liquid, filter out silica/silicon acid powder, after the contained organic solvent volatilization of silica/silicon acid powder, recording its water cut is 15wt%, obtains SiO 2 powder 150～200 ℃ of oven dry.The hydrogen chloride gas that produces in the reaction process is collected after removing silicon tetrachloride and sherwood oil wherein, obtains the gas that the hydrogen chloride gas body burden is 98v%.
Embodiment 10
The process step of present embodiment is following:
(1) is that 60～90 ℃ sherwood oil (solvent) is a raw material with 0.5 gram Span80 (emulsifying agent), 10mL tap water, 100mL boiling range, under room temperature, normal pressure, said Span80 is dissolved in said sherwood oil, add tap water again and mix, promptly form milk sap;
(2) be raw material with 100mL silicon tetrachloride as by-product of polysilicon (containing a small amount of trichlorosilane) and 1000mL normal hexane, under room temperature, normal pressure, join said silicon tetrachloride as by-product of polysilicon in the normal hexane and stir, promptly form silicon tetrachloride solution;
(3) silicon tetrachloride solution of under normal pressure, room temperature, the milk sap and the step (2) of step (1) preparation being prepared is in the reaction vessel that joined continuously respectively 1: 10 (mol ratio of water and silicon tetrachloride and trichlorosilane total amount is about 1: 1.6) under stirring by volume; Behind reinforced the finishing; Under agitation continue reaction 30 minutes; After reaction times expires; From the reaction feed liquid, filter out silica/silicon acid powder, after the contained organic solvent volatilization of silica/silicon acid powder, recording its water cut is 21wt%, obtains SiO 2 powder 150～200 ℃ of oven dry.The hydrogen chloride gas that produces in reaction process water after removing silicon tetrachloride and sherwood oil wherein absorbs the concentrated hydrochloric acid that obtains concentration 31wt%.
Embodiment 11
The process step of present embodiment is following:
(1) is that 60～90 ℃ sherwood oil (solvent) is a raw material with 3.5 gram Span80 (emulsifying agent), 90mL tap water, 100mL boiling range, under room temperature, normal pressure, said Span80 is dissolved in said sherwood oil, add tap water again and mix, promptly form milk sap;
(2) be raw material with 100mL silicon tetrachloride as by-product of polysilicon (containing a small amount of trichlorosilane) and 1000mL normal hexane, under room temperature, normal pressure, join said silicon tetrachloride as by-product of polysilicon in the normal hexane and stir, promptly form silicon tetrachloride solution;
(3) silicon tetrachloride solution of under normal pressure, room temperature, the milk sap and the step (2) of step (1) preparation being prepared is in the reaction vessel that joined continuously respectively 1: 20 (mol ratio of water and silicon tetrachloride and trichlorosilane total amount is about 1: 0.6) under stirring by volume; Behind reinforced the finishing; Under agitation continue reaction 30 minutes; After reaction times expires; From the reaction feed liquid, filter out silica/silicon acid powder, after the contained organic solvent volatilization of silica/silicon acid powder, recording its water cut is 45wt%, obtains SiO 2 powder 150～200 ℃ of oven dry.The hydrogen chloride gas that produces in reaction process water after removing silicon tetrachloride and sherwood oil wherein absorbs the concentrated hydrochloric acid that obtains concentration 31wt%.
Embodiment 12
The process step of present embodiment is following:
(1) is that 60～90 ℃ sherwood oil (solvent) is a raw material with 0.1 gram Span60 (emulsifying agent), 20mL tap water, 100mL boiling range, under room temperature, normal pressure, said Span80 is dissolved in said sherwood oil, add tap water again and mix, promptly form milk sap;
(2) be raw material with 40mL silicon tetrachloride as by-product of polysilicon (containing a small amount of trichlorosilane) and 200mL normal hexane, under room temperature, normal pressure, join said silicon tetrachloride as by-product of polysilicon in the normal hexane and stir, promptly form silicon tetrachloride solution;
(3) silicon tetrachloride solution of under normal pressure, room temperature, the milk sap and the step (2) of step (1) preparation being prepared is in the reaction vessel that joined continuously respectively 1: 10 (mol ratio of water and silicon tetrachloride and trichlorosilane total amount is about 1: 1.4) under stirring by volume; Behind reinforced the finishing; Under agitation continue reaction 1 minute; After reaction times expires; From the reaction feed liquid, filter out silica/silicon acid powder, after the contained organic solvent volatilization of silica/silicon acid powder, recording its water cut is 40wt%, obtains SiO 2 powder 150～200 ℃ of oven dry.The hydrogen chloride gas that produces in reaction process water after removing silicon tetrachloride and sherwood oil wherein absorbs the concentrated hydrochloric acid that obtains concentration 31wt%.
Claims (6)
1. the method for a chlorosilane hydrolysis is characterized in that process step is following:
(1) preparation milk sap
With emulsifying agent, water, with the immiscible solvent of water be raw material; Emulsifying agent quality: the quality of water=0.005～0.2: 1; The volume of water: with volume=0.05～0.9 of the immiscible solvent of water: 1; Under normal pressure, room temperature,, promptly form milk sap with emulsifying agent, water, even with the immiscible solvent of water;
(2) preparation chlorosilane solution
With chlorosilane, with the immiscible solvent of water be raw material, chlorosilane volume:, under normal pressure, room temperature, with chlorosilane, mix, promptly form chlorosilane solution with the immiscible solvent phase of water with volume=1: 1～25 of the immiscible solvent of water;
(3) hydrolysis reaction
With the milk sap of step (1) preparation and the chlorosilane solution of step (2) preparation is raw material; The proportioning of said milk sap and chlorosilane solution is the mole number of water in the milk sap: the mole number of chlorosilane in the chlorosilane solution=1: 0.2～2; Said milk sap is mixed with chlorosilane solution mutually; Normal pressure, room temperature～50 ℃ reaction 1 minute～120 minutes, promptly generate silica/silicon acid powder and the hydrogen chloride gas of water cut less than 60wt%.
2. according to the method for the said chlorosilane hydrolysis of claim 1, it is characterized in that preparing the used emulsifying agent of milk sap and be at least a less than in 20 acid, ester, the ether of hydrophile-lipophile balance value,
3. according to the method for the said chlorosilane hydrolysis of claim 2, it is characterized in that preparing at least a in acid that the used emulsifying agent of milk sap is hydrophile-lipophile balance value=3～9, ester, the ether.
4. according to the method for the said chlorosilane hydrolysis of arbitrary claim in the claim 1 to 3, it is characterized in that preparing milk sap and preparation chlorosilane solution solvent for use is 30 ℃～250 ℃ organic solvent for depress boiling point at a standard atmosphere.
5. according to the method for the said chlorosilane hydrolysis of claim 4, it is characterized in that said organic solvent is at least a in pentane, normal hexane, hexanaphthene, heptane, octane, sherwood oil, petroleum naphtha, solvent oil, gasoline, kerosene, the diesel oil.
6. according to the method for the said chlorosilane hydrolysis of claim 5, it is characterized in that said organic solvent is at least a in normal hexane, hexanaphthene, sherwood oil, solvent oil, the kerosene.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110149586 CN102320613B (en) | 2011-06-04 | 2011-06-04 | Method for hydrolyzing chlorosilane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110149586 CN102320613B (en) | 2011-06-04 | 2011-06-04 | Method for hydrolyzing chlorosilane |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102320613A true CN102320613A (en) | 2012-01-18 |
| CN102320613B CN102320613B (en) | 2013-01-16 |
Family
ID=45448493
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201110149586 Expired - Fee Related CN102320613B (en) | 2011-06-04 | 2011-06-04 | Method for hydrolyzing chlorosilane |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102320613B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111647013A (en) * | 2020-06-12 | 2020-09-11 | 淄博市临淄齐泉工贸有限公司 | Device and method for preparing propyl silicate waterproof agent |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| NL8802119A (en) * | 1988-08-27 | 1990-03-16 | Stamicarbon | Method for preparing silicon dioxide particles and use thereof |
| CN1075154A (en) * | 1993-03-03 | 1993-08-11 | 复旦大学 | A kind of preparation method who is used for the filler-silicon dioxide of epoxy mold sealing material |
| CN101613108A (en) * | 2009-07-10 | 2009-12-30 | 长春理工大学 | A kind of preparation method of silicon dioxide ultrafine powder |
| CN102009953A (en) * | 2010-10-29 | 2011-04-13 | 四川永祥股份有限公司 | Method for recycling byproduct during production of polycrystalline silicon |
-
2011
- 2011-06-04 CN CN 201110149586 patent/CN102320613B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| NL8802119A (en) * | 1988-08-27 | 1990-03-16 | Stamicarbon | Method for preparing silicon dioxide particles and use thereof |
| CN1075154A (en) * | 1993-03-03 | 1993-08-11 | 复旦大学 | A kind of preparation method who is used for the filler-silicon dioxide of epoxy mold sealing material |
| CN101613108A (en) * | 2009-07-10 | 2009-12-30 | 长春理工大学 | A kind of preparation method of silicon dioxide ultrafine powder |
| CN102009953A (en) * | 2010-10-29 | 2011-04-13 | 四川永祥股份有限公司 | Method for recycling byproduct during production of polycrystalline silicon |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111647013A (en) * | 2020-06-12 | 2020-09-11 | 淄博市临淄齐泉工贸有限公司 | Device and method for preparing propyl silicate waterproof agent |
| CN111647013B (en) * | 2020-06-12 | 2023-05-16 | 淄博市临淄齐泉工贸有限公司 | Device and method for preparing propyl silicate waterproof agent |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102320613B (en) | 2013-01-16 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103864455B (en) | Method for yellow phosphorus slag base aerated building blocks | |
| CN105060307A (en) | High-specific-area white carbon black and production method thereof | |
| CN102001671A (en) | Method for preparing white carbon black by using silicon tetrachloride | |
| CN1764600A (en) | Pyrogenic silicon dioxide powder and dispersion thereof | |
| CN101798088A (en) | Method for preparing white carbon black by utilizing silicon tetrachloride | |
| CN104910649A (en) | Quartz powder surface active composite modification method | |
| CN102198942A (en) | Preparation method of silicon dioxide | |
| CN101708976A (en) | Liquid composition used for reinforcing concrete, preparation method thereof and application thereof | |
| CN102320613B (en) | Method for hydrolyzing chlorosilane | |
| CN103936015A (en) | Method for preparing white carbon black slurry by using spraying method | |
| CN102976659A (en) | Chemical-waste compounded cement grinding aid | |
| CN1458061A (en) | Process for extracting CaF2 and SiO2 from fluorite tailing and producing fluorosilicic acid further | |
| CN104445219A (en) | Preparation method of white carbon black | |
| CN101838005B (en) | Method for producing sodium chloride and carbon powder and co-producing superfine light calcium carbonate and white carbon black | |
| CN109179429B (en) | Method for preparing mesoporous nano-silica from chlorosilane residual liquid | |
| JP2010121083A (en) | Production method of consolidating material for grouting | |
| CN103213992B (en) | Method for preparing nano white carbon black by taking wollastonite as raw material | |
| US20180044188A1 (en) | Method for producing organically modified aerogels | |
| CN103272564B (en) | Method for rapidly preparing efficient adsorbent with low cost by adopting organosilicone high-boiling residue | |
| CN1308401C (en) | Method for preparing hydrophobic inorganic and organic composite corpuscle | |
| CN109824055A (en) | The method for preparing nano-sheet zinc silicate compound adsorbent using iron tailings | |
| CN115957891A (en) | Phosphogypsum flotation purification method | |
| CN101691226B (en) | Method for comprehensively utilizing polysilicon by-product with low cost | |
| CN101823746B (en) | Method for producing fine precipitated calcium carbonate and white carbon black coproduction sodium chloride and powdered carbon | |
| CN102627324A (en) | Preparation method of nanometer antimony oxide |
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 | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20130116 Termination date: 20130604 |