CN114805422B - Method for recycling silicon ether from alkylamine kettle residues - Google Patents
Method for recycling silicon ether from alkylamine kettle residues Download PDFInfo
- Publication number
- CN114805422B CN114805422B CN202210537827.0A CN202210537827A CN114805422B CN 114805422 B CN114805422 B CN 114805422B CN 202210537827 A CN202210537827 A CN 202210537827A CN 114805422 B CN114805422 B CN 114805422B
- Authority
- CN
- China
- Prior art keywords
- octamethyltrisiloxane
- kettle
- alkylamine
- purity
- ether
- 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.)
- Active
Links
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 150000003973 alkyl amines Chemical class 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 title claims abstract description 17
- 238000004064 recycling Methods 0.000 title claims abstract description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims description 23
- 229910052710 silicon Inorganic materials 0.000 title claims description 23
- 239000010703 silicon Substances 0.000 title claims description 23
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 72
- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000006227 byproduct Substances 0.000 claims abstract description 24
- 238000010992 reflux Methods 0.000 claims abstract description 23
- 238000006243 chemical reaction Methods 0.000 claims abstract description 22
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical compound [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000007787 solid Substances 0.000 claims abstract description 14
- 238000005904 alkaline hydrolysis reaction Methods 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000003513 alkali Substances 0.000 claims abstract description 9
- 229920000642 polymer Polymers 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 5
- 229910052799 carbon Inorganic materials 0.000 claims description 5
- 239000003054 catalyst Substances 0.000 claims description 5
- 238000004821 distillation Methods 0.000 claims description 5
- 238000002390 rotary evaporation Methods 0.000 claims description 5
- 238000005070 sampling Methods 0.000 claims description 5
- 239000012044 organic layer Substances 0.000 claims description 4
- JRMUNVKIHCOMHV-UHFFFAOYSA-M tetrabutylammonium bromide Chemical compound [Br-].CCCC[N+](CCCC)(CCCC)CCCC JRMUNVKIHCOMHV-UHFFFAOYSA-M 0.000 claims description 4
- 239000003444 phase transfer catalyst Substances 0.000 abstract description 7
- 239000012074 organic phase Substances 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 229920001296 polysiloxane Polymers 0.000 abstract 4
- 238000011282 treatment Methods 0.000 description 11
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 description 6
- 239000012071 phase Substances 0.000 description 6
- 239000002994 raw material Substances 0.000 description 5
- VHYFNPMBLIVWCW-UHFFFAOYSA-N 4-Dimethylaminopyridine Chemical group CN(C)C1=CC=NC=C1 VHYFNPMBLIVWCW-UHFFFAOYSA-N 0.000 description 4
- 238000009835 boiling Methods 0.000 description 4
- 239000002920 hazardous waste Substances 0.000 description 3
- 229960000549 4-dimethylaminophenol Drugs 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- GLDOVTGHNKAZLK-UHFFFAOYSA-N octadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCCCO GLDOVTGHNKAZLK-UHFFFAOYSA-N 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- XEZNGIUYQVAUSS-UHFFFAOYSA-N 18-crown-6 Chemical compound C1COCCOCCOCCOCCOCCO1 XEZNGIUYQVAUSS-UHFFFAOYSA-N 0.000 description 1
- SZKKRCSOSQAJDE-UHFFFAOYSA-N Schradan Chemical group CN(C)P(=O)(N(C)C)OP(=O)(N(C)C)N(C)C SZKKRCSOSQAJDE-UHFFFAOYSA-N 0.000 description 1
- HMDDXIMCDZRSNE-UHFFFAOYSA-N [C].[Si] Chemical compound [C].[Si] HMDDXIMCDZRSNE-UHFFFAOYSA-N 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000012700 ceramic precursor Substances 0.000 description 1
- 150000003983 crown ethers Chemical class 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 239000000543 intermediate Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000012450 pharmaceutical intermediate Substances 0.000 description 1
- 229920000548 poly(silane) polymer Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/0834—Compounds having one or more O-Si linkage
- C07F7/0838—Compounds with one or more Si-O-Si sequences
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/0834—Compounds having one or more O-Si linkage
- C07F7/0838—Compounds with one or more Si-O-Si sequences
- C07F7/0872—Preparation and treatment thereof
- C07F7/0874—Reactions involving a bond of the Si-O-Si linkage
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/20—Purification, separation
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Silicon Polymers (AREA)
Abstract
The invention relates to a method for recycling alkylamine kettle residues, which comprises the steps of adding potassium hydroxide and a phase transfer catalyst into a silicone ether kettle residue containing 70% of byproduct octamethyltrisiloxane, and thoroughly decomposing octamethyltrisiloxane into silicone ether with the purity of about 92% by an alkaline hydrolysis reflux mode, wherein the obtained silicone ether can be subjected to normal pressure rectification to obtain qualified silicone ether which can be continuously used for reaction; after the residual kettle residue is hydrolyzed by adding water, the upper organic phase is a small amount of high-heat-value polymer, and the lower alkali liquor can be directly decolorized and evaporated to dryness to obtain solid potassium hydroxide for reuse; the method solves the problem that the alkylamine byproduct is difficult to treat, recovers a large amount of silyl ether, and increases the production benefit.
Description
Technical Field
The invention relates to a method for recycling residue of an alkylamine kettle, in particular to a method for recycling octamethyltrisiloxane byproduct generated in the production process of hexamethyldisilazane.
Background
Hexamethyldisilazane is an important pharmaceutical intermediate raw material and also a base raw material for organosilicon products. In recent years, applications in photoelectric materials, ceramic precursors, photovoltaic materials, carbon-silicon materials, polysilane intermediates and the like are attracting more and more attention. However, corresponding byproducts are generated in the process of producing hexamethyldisilazane, wherein octamethyltrisiloxane and a small amount of silyl ether are contained, the treatment of the high-boiling byproduct octamethyltrisiloxane always puzzles related enterprises, the existing treatment method for the alkylamine byproduct octamethyltrisiloxane is mostly directly carried out incineration treatment or directly used as hazardous waste for transferring, a large amount of silicon dioxide solids are generated in the incineration treatment, the environment is damaged, and the hazardous waste transfer can cause waste of raw materials and increase the cost. In regard to the cleaning treatment method of the alkylamine byproduct octamethyltrisiloxane, no relevant report is found by referring to the domestic and foreign documents, and in view of the situation that the current state gradually trends in the supervision of hazardous waste treatment, development and research on a cleaning treatment method are urgently needed.
Disclosure of Invention
In order to solve the problems, the invention provides that the silicon ether kettle residue containing 70% by-product octamethyltrisiloxane is added with potassium hydroxide and a phase transfer catalyst, octamethyltrisiloxane is thoroughly decomposed and reacted into silicon ether with the purity of about 92% by an alkaline hydrolysis reflux mode, and the obtained silicon ether can be subjected to normal pressure rectification to obtain qualified silicon ether which can be continuously used for reaction; after the residual kettle residue is hydrolyzed by adding water, the upper organic phase is a small amount of high-heat-value polymer, and the lower alkali liquor can be directly decolorized and evaporated to dryness to obtain solid potassium hydroxide for reuse; the method solves the problem that the alkylamine byproduct is difficult to treat, recovers a large amount of silyl ether, and increases the production benefit.
In view of the above, the invention provides a method for obtaining qualified silyl ether from alkylamine kettle residues by processing octamethyltrisiloxane to be hydrolyzed into silyl ether and rectifying the silyl ether.
The strong alkaline potassium hydroxide has the best alkaline hydrolysis effect, the alkaline of sodium hydroxide is weaker than that of potassium hydroxide, the alkaline hydrolysis reaction by sodium hydroxide is incomplete, and the alkaline hydrolysis effect is poor.
The technical scheme of the invention is realized as follows: adding alkylamine kettle residues, potassium hydroxide and a phase transfer catalyst into a reaction kettle, thoroughly reacting octamethyltrisiloxane into silicon ether with the purity of 92% in an alkaline hydrolysis reflux mode, and obtaining qualified silicon ether which can be continuously used in a normal pressure rectification mode; after the residual kettle is hydrolyzed by adding water, the upper organic phase is a small amount of polymer with high heat value, the polymer can be directly burnt, the lower alkali liquor can be directly decolored and evaporated to dryness to obtain solid potassium hydroxide for reuse.
The technical scheme of the invention is as follows:
(1) Adding alkylamine kettle residues and potassium hydroxide solids into a reaction kettle, and heating by adding a phase transfer catalyst until reflux reaction;
(2) As the reaction proceeds, the temperature is reduced from 124 ℃ to 102 ℃, and the reflux reaction is stabilized for 6 hours;
The early reflux temperature is 124 ℃ and is high-boiling octamethyltrisiloxane, the octamethyltrisiloxane is reacted into silicon ether through the reaction group trisiloxane octamethyl, the boiling point of the mixed solution is reduced from 124 ℃ to about 102 ℃ of the boiling point of the silicon ether, and the stable reflux at 102 ℃ is started.
(3) Sampling and detecting the reaction condition every 1h, wherein the octamethyltrisiloxane can completely react after 6 h;
(4) At this time, the purity of the distilled silyl ether is 92% under normal pressure;
(5) The residual kettle is hydrolyzed by adding water, the upper organic phase is a small amount of high heat value polymer, the upper organic phase can be directly burnt, the lower alkali liquor is decolored by adding active carbon, and the solid potassium hydroxide can be reused after rotary evaporation and drying;
(6) Rectifying the silyl ether obtained in the step (4) at normal pressure, and collecting fractions at about 100 ℃ to obtain qualified fractions;
(7) After the reaction is finished, the purity of the obtained qualified fraction silyl ether is over 99 percent, the moisture is below 0.05 percent, the obtained silyl ether is qualified silyl ether, subsequent experiments can be carried out, and a qualified product can be obtained.
The amount of potassium hydroxide added in step (1) is determined by the amount of octamethyltrisiloxane, the molar ratio of octamethyltrisiloxane to potassium hydroxide ranging from 1:1 to 1:3, preferably from 1:1.2 to 1:1.8. The phase transfer catalyst is selected from DMAP, octadecanohexa (1, 4,7,10,13, 16-hexaoxacyclooctadecane, which is a crown ether), tetrabutylammonium bromide, and the molar ratio of octamethyltrisiloxane to the phase transfer catalyst is 1:0.001.
The invention has the following beneficial effects:
(1) The method is different from the conventional treatment method, before rectification treatment, alkali and phase transfer catalyst are reinforced by the residue of the alkylamine kettle, and alkaline hydrolysis reaction is carried out until the byproduct octamethyltrisiloxane is completely reacted into silicon ether, and then the silicon ether with the purity of 92% is distilled out at normal pressure;
(2) The invention can recover the silicon ether with 92% purity by normal pressure distillation to obtain the silicon ether with high purity and low moisture content, the silicon ether purity is above 99% and the moisture content is below 0.05%.
Detailed Description
The following description of the embodiments of the present application will clearly and fully describe the technical aspects of the embodiments of the present application, and it is apparent that the described embodiments are only some embodiments of the present application, and not all embodiments of the present application. Given the embodiments of the present application, all other embodiments that may be obtained by one of ordinary skill in the art without undue burden are within the scope of the present application. It is also to be understood that various changes and modifications may be made by one skilled in the art after reading the teachings of the application, and that these equivalents are intended to fall within the scope of the application as defined in the appended claims
The alkylamine residue containing octamethyltrisiloxane as a byproduct produced in a production plant was treated, and the alkylamine residue used in the example of the present invention contained octamethyltrisiloxane as a byproduct by about 70%.
Example 1:
(1) Adding alkylamine kettle residues and solid potassium hydroxide (the molar ratio of octamethyltrisiloxane to potassium hydroxide is 1:1.2) into a reaction kettle, and adding a proper amount of DMAP (the molar ratio of octamethyltrisiloxane to catalyst is 1:0.001);
(2) Slowly heating to reflux state for alkaline hydrolysis, and reducing the reflux temperature from 124 ℃ to 102 ℃ to keep stable reflux reaction for 6 hours;
(3) Sampling and detecting after 6 hours, and carrying out basic full reaction on the byproduct octamethyltrisiloxane;
(4) Adopting an atmospheric distillation mode, and distilling out the silicon ether with the purity of about 92 percent;
(5) The residual kettle is hydrolyzed by adding water, is kept stand for layering, the upper organic layer is a small amount of high-heat-value polymer, can be directly burnt, and the lower alkali liquor is decolored by adding active carbon and is evaporated to dryness by rotary evaporation to obtain solid potassium hydroxide for repeated use;
(6) Rectifying the silicon ether with the purity of 92% at normal pressure;
(7) Starting rectification and adjusting the reflux ratio to 3:1;
(8) Heating to gas phase temperature of 60deg.C to start collecting the pre-fraction, and stopping collecting the pre-fraction to 99.5deg.C; the front fraction is the silyl ether with lower purity, and can participate in the mechanically continuous rectification during the next batch of rectification;
(9) Continuously heating, and collecting the gas phase temperature of 99.5-100 ℃ as qualified fraction;
(10) And detecting the purity, the moisture and byproducts of the silyl ether by using the qualified fraction sample.
Example 2:
(1) Adding alkylamine kettle residues and solid potassium hydroxide (the molar ratio of octamethyltrisiloxane to potassium hydroxide is 1:1.2) into a reaction kettle, and adding a proper amount of octadecanol hexa (the molar ratio of octamethyltrisiloxane to catalyst is 1:0.001);
(2) Slowly heating to reflux state for alkaline hydrolysis, and reducing the reflux temperature from 124 ℃ to 102 ℃ to keep stable reflux reaction for 6 hours;
(3) Sampling and detecting after 6 hours, and carrying out basic full reaction on the byproduct octamethyltrisiloxane;
(4) Adopting an atmospheric distillation mode, and distilling out the silicon ether with the purity of about 92 percent;
(5) The residual kettle is hydrolyzed by adding water, is kept stand for layering, the upper organic layer is a small amount of high-heat-value polymer, can be directly burnt, and the lower alkali liquor is decolored by adding active carbon and is evaporated to dryness by rotary evaporation to obtain solid potassium hydroxide for repeated use;
(6) Rectifying the silicon ether with the purity of 92% at normal pressure;
(7) Starting rectification and adjusting the reflux ratio to 3:1;
(8) Heating to gas phase temperature of 60deg.C to start collecting the pre-fraction, and stopping collecting the pre-fraction to 99.5deg.C;
(9) Continuously heating, and collecting the gas phase temperature of 99.5-100 ℃ as qualified fraction;
(10) And detecting the purity, the moisture and byproducts of the silyl ether by using the qualified fraction sample.
Example 3:
(1) Adding alkylamine kettle residues and solid potassium hydroxide (the molar ratio of octamethyltrisiloxane to potassium hydroxide is 1:1.2) into a reaction kettle, and adding a proper amount of tetrabutylammonium bromide (the molar ratio of octamethyltrisiloxane to catalyst is 1:0.001);
(2) Slowly heating to reflux state for alkaline hydrolysis, and reducing the reflux temperature from 124 ℃ to 102 ℃ to keep stable reflux reaction for 6 hours;
(3) Sampling and detecting after 6 hours, and carrying out basic full reaction on the byproduct octamethyltrisiloxane;
(4) Adopting an atmospheric distillation mode, and distilling out the silicon ether with the purity of about 92 percent;
(5) The residual kettle is hydrolyzed by adding water, is kept stand for layering, the upper organic layer is a small amount of high-heat-value polymer, can be directly burnt, and the lower alkali liquor is decolored by adding active carbon and is evaporated to dryness by rotary evaporation to obtain solid potassium hydroxide for repeated use;
(6) Rectifying the silicon ether with the purity of 92% at normal pressure;
(7) Starting rectification and adjusting the reflux ratio to 3:1;
(8) Heating to gas phase temperature of 60deg.C to start collecting the pre-fraction, and stopping collecting the pre-fraction to 99.5deg.C;
(9) Continuously heating, and collecting the gas phase temperature of 99.5-100 ℃ as qualified fraction;
(10) And detecting the purity, the moisture and byproducts of the silyl ether by using the qualified fraction sample.
The following data were obtained by gas chromatography detection of the raw material alkylamine residue and the silyl ether produced in examples 1 to 3, respectively:
| Project | Residue of raw material alkylamine kettle | Example 1 | Example 2 | Example 3 |
| Silyl ether purity/% | 26.14 | 99.46 | 99.51 | 99.53 |
| By-product octa-methyl/% | 70.19 | Not detected | Not detected | Not detected |
| Moisture/% | -- | 0.02 | 0.03 | 0.02 |
The data show that the treatment method can obtain high-purity silyl ether, and the byproduct octamethyltrisiloxane can be reacted completely, so that the treatment method is simpler and the recovery rate is high.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.
Claims (1)
1. A method for recycling alkylamine kettle residues, the purity of silyl ether in the alkylamine kettle residues is 26.14 percent, the byproduct octamethyltrisiloxane is 70.19%, and is characterized by comprising the following steps:
(1) Adding alkylamine kettle residues and solid potassium hydroxide into a reaction kettle, wherein the molar ratio of octamethyltrisiloxane to potassium hydroxide is 1:1.2, and adding a proper amount of catalyst tetrabutylammonium bromide, wherein the molar ratio of octamethyltrisiloxane to catalyst tetrabutylammonium bromide is 1:0.001;
(2) Slowly heating to reflux state for alkaline hydrolysis, and reducing the reflux temperature from 124 ℃ to 102 ℃ to keep stable reflux reaction for 6 hours;
(3) Sampling and detecting after 6 hours, and carrying out basic full reaction on the byproduct octamethyltrisiloxane;
(4) Adopting an atmospheric distillation mode, and distilling out the silicon ether with the purity of about 92 percent;
(5) The residual kettle is hydrolyzed by adding water, is kept stand for layering, the upper organic layer is a small amount of high-heat-value polymer, can be directly burnt, and the lower alkali liquor is decolored by adding active carbon and is evaporated to dryness by rotary evaporation to obtain solid potassium hydroxide for repeated use;
(6) Rectifying the silicon ether with the purity of 92% at normal pressure;
(7) Starting rectification and adjusting the reflux ratio to 3:1;
(8) Heating to gas phase temperature of 60deg.C to start collecting the pre-fraction, and stopping collecting the pre-fraction to 99.5deg.C;
(9) Continuously heating, and collecting the gas phase temperature of 99.5-100 ℃ as a qualified fraction;
(10) And detecting the purity of the silyl ether, the water content and byproducts of the qualified fraction, wherein the purity of the silyl ether is 99.53%, the water content is 0.02%, and the byproducts of the octamethyltrisiloxane are not detected.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210537827.0A CN114805422B (en) | 2022-05-17 | 2022-05-17 | Method for recycling silicon ether from alkylamine kettle residues |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210537827.0A CN114805422B (en) | 2022-05-17 | 2022-05-17 | Method for recycling silicon ether from alkylamine kettle residues |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114805422A CN114805422A (en) | 2022-07-29 |
| CN114805422B true CN114805422B (en) | 2024-08-27 |
Family
ID=82516109
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210537827.0A Active CN114805422B (en) | 2022-05-17 | 2022-05-17 | Method for recycling silicon ether from alkylamine kettle residues |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114805422B (en) |
Family Cites Families (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5250791B2 (en) * | 1972-12-30 | 1977-12-27 | ||
| US3846464A (en) * | 1973-11-27 | 1974-11-05 | Gen Electric | Process for preparing cyclic methylvinylsiloxanes |
| US4111973A (en) * | 1977-12-01 | 1978-09-05 | General Electric Company | Process for producing a cyclotrisiloxane in a cracking reaction |
| DE3108235A1 (en) * | 1981-03-05 | 1982-09-30 | Dynamit Nobel Ag, 5210 Troisdorf | "METHOD FOR PURIFYING HEXAMETHYLDISILOXANE AND THE AZEOTROPIC MIXTURES INCLUDING IT" |
| JPS63190891A (en) * | 1987-02-03 | 1988-08-08 | Toray Silicone Co Ltd | Purification of hexamethyldisiloxane |
| JPH07126269A (en) * | 1993-11-05 | 1995-05-16 | Shin Etsu Chem Co Ltd | Method for producing hexamethyldisiloxane |
| JPH10251276A (en) * | 1997-03-07 | 1998-09-22 | Kanegafuchi Chem Ind Co Ltd | Production of demethoxymethylsilane |
| DE19934374C1 (en) * | 1999-07-22 | 2000-10-19 | Ge Bayer Silicones Gmbh & Co | Continuous production of cyclic dimethylsiloxanes, e.g. octamethylcyclotetrasiloxane used in silicone elastomer production, includes removal of monomethylsiloxy compounds before recycling unwanted homologues |
| CN1092200C (en) * | 2000-05-19 | 2002-10-09 | 清华大学 | Preparation of hexamethl disilamine from hexamethyl disiloxane |
| CN101723964A (en) * | 2009-11-26 | 2010-06-09 | 浙江胡涂硅有限公司 | Preparation method of hexamethyl disilazane alkyl |
| JP6375946B2 (en) * | 2013-01-09 | 2018-08-22 | 東レ株式会社 | Laminated film |
| CN105384763A (en) * | 2014-09-04 | 2016-03-09 | 上海楚青新材料科技有限公司 | 1,1,1,3,3,5,5-heptamethyltrisiloxane preparation method |
| CN105061483A (en) * | 2015-08-19 | 2015-11-18 | 湖北兴瑞化工有限公司 | Method for preparing hexamethyldisiloxane by using organic silicon by-product |
| CN107652315A (en) * | 2017-08-24 | 2018-02-02 | 常州润联化工有限公司 | The synthetic method of hexamethyldisilane |
| CN108129509A (en) * | 2017-12-25 | 2018-06-08 | 湖北泓肽生物科技有限公司 | It is a kind of to recycle the method for waste generated in protected silane reaction process |
| CN109748932B (en) * | 2019-01-09 | 2021-06-08 | 浙江新化化工股份有限公司 | Continuous synthesis method of hexamethyldisilazane |
-
2022
- 2022-05-17 CN CN202210537827.0A patent/CN114805422B/en active Active
Non-Patent Citations (1)
| Title |
|---|
| Cleavage of silicon-oxygen bonds in the presence of triethyl orthoformate;Zhurkina, I. P等，;《Osn. Organ. Sintez i Neftekhimiya》;第161-7页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114805422A (en) | 2022-07-29 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN100999442B (en) | Pseudo-azeotropic composition containing dichloropropanol and process for producing the same | |
| US8283139B2 (en) | Method of producing xylitol using hydrolysate containing xylose and arabinose prepared from byproduct of tropical fruit biomass | |
| JP3841834B2 (en) | Malonic acid and its esters | |
| CN1104254A (en) | Process for the production of lactic acid and lactic acid esters | |
| CN1057291C (en) | Process for the manufacture of butyl acrylate by direct esterification | |
| WO2011084002A2 (en) | Method for producing organic acids from biomass | |
| CN105111232B (en) | A kind of preparation technology of MTES | |
| CN114805422B (en) | Method for recycling silicon ether from alkylamine kettle residues | |
| EP0881248A2 (en) | Continuous hydrolysis of organochlorosilanes | |
| CN101638235A (en) | A method for preparing silicon-containing product from plant | |
| WO2012002648A2 (en) | Method for preparing chlorohydrins and method for preparing epichlorohydrin using chlorohydrins prepared thereby | |
| CN103408474B (en) | High purity N-acetyl-D, the high-efficiency method for producing of L-Methionine | |
| WO2019027222A1 (en) | Method for decolorizing and deodorizing polyhydric alcohol | |
| CN117861252A (en) | Separation and purification process for waste solvent in liquid crystal panel production | |
| CN111004131A (en) | A kind of recovery method of sucralose by-product salt | |
| CN114671859B (en) | Preparation method of rosuvastatin calcium and intermediate thereof | |
| CN110357921A (en) | A kind of industrialized process for preparing of high-purity three (butoxyethyl group) phosphate | |
| WO2012002651A2 (en) | Method for preparing chlorohydrins composition and method for preparing epichlorohydrin using chlorohydrins composition prepared thereby | |
| CN210826005U (en) | 1, 2-benzisothiazole-3-ketone production system | |
| WO2012002649A2 (en) | Method for preparing chlorohydrins and method for preparing epichlorohydrin using chlorohydrins prepared thereby | |
| CN111675918B (en) | Preparation method of disperse red 60 | |
| CN1045077C (en) | Tail gas recovery method and device in production of silicon carbide fibre | |
| CN109928993A (en) | A kind of commercial recovery method that the fluorescent whitening agent kettle of phosphorous diethyl phthalate is residual | |
| JP2010265455A (en) | Method for producing treated coal and silica from fly ash-including coal | |
| CN118480180B (en) | Low-oxygen-content polydimethylsilane and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |