CN114805422A - Method for recovering silicon ether from alkylamine kettle residue - Google Patents
Method for recovering silicon ether from alkylamine kettle residue Download PDFInfo
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- CN114805422A CN114805422A CN202210537827.0A CN202210537827A CN114805422A CN 114805422 A CN114805422 A CN 114805422A CN 202210537827 A CN202210537827 A CN 202210537827A CN 114805422 A CN114805422 A CN 114805422A
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- octamethyltrisiloxane
- alkylamine
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- potassium hydroxide
- silicon ether
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- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 title claims abstract description 58
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 30
- 239000010703 silicon Substances 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 26
- 150000003973 alkyl amines Chemical class 0.000 title claims abstract 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 34
- 238000006243 chemical reaction Methods 0.000 claims abstract description 23
- 238000010992 reflux Methods 0.000 claims abstract description 21
- 239000007787 solid Substances 0.000 claims abstract description 15
- 239000003444 phase transfer catalyst Substances 0.000 claims abstract description 10
- 239000003513 alkali Substances 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229920000642 polymer Polymers 0.000 claims abstract description 8
- 239000012074 organic phase Substances 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 10
- VHYFNPMBLIVWCW-UHFFFAOYSA-N 4-Dimethylaminopyridine Chemical group CN(C)C1=CC=NC=C1 VHYFNPMBLIVWCW-UHFFFAOYSA-N 0.000 claims description 6
- 238000005070 sampling Methods 0.000 claims description 5
- 238000001704 evaporation Methods 0.000 claims description 4
- 230000008020 evaporation Effects 0.000 claims description 4
- 238000002390 rotary evaporation Methods 0.000 claims description 4
- 229960000549 4-dimethylaminophenol Drugs 0.000 claims description 3
- 238000011084 recovery Methods 0.000 claims description 3
- JRMUNVKIHCOMHV-UHFFFAOYSA-M tetrabutylammonium bromide Chemical compound [Br-].CCCC[N+](CCCC)(CCCC)CCCC JRMUNVKIHCOMHV-UHFFFAOYSA-M 0.000 claims description 3
- 230000007062 hydrolysis Effects 0.000 claims 1
- 238000006460 hydrolysis reaction Methods 0.000 claims 1
- 239000006227 byproduct Substances 0.000 abstract description 20
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical compound [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 abstract description 18
- 238000005904 alkaline hydrolysis reaction Methods 0.000 abstract description 11
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 238000004064 recycling Methods 0.000 abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 239000012071 phase Substances 0.000 description 6
- 239000002994 raw material Substances 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 238000009835 boiling Methods 0.000 description 4
- 230000003301 hydrolyzing effect Effects 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 3
- 238000004821 distillation Methods 0.000 description 3
- 239000002920 hazardous waste Substances 0.000 description 3
- -1 hexamethyldisilane amine Chemical class 0.000 description 3
- 239000012044 organic layer Substances 0.000 description 3
- 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
- 239000000543 intermediate Substances 0.000 description 2
- 239000010410 layer Substances 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
- 239000000047 product Substances 0.000 description 2
- XEZNGIUYQVAUSS-UHFFFAOYSA-N 18-crown-6 Chemical compound C1COCCOCCOCCOCCOCCO1 XEZNGIUYQVAUSS-UHFFFAOYSA-N 0.000 description 1
- HMDDXIMCDZRSNE-UHFFFAOYSA-N [C].[Si] Chemical compound [C].[Si] HMDDXIMCDZRSNE-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000012700 ceramic precursor Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000003983 crown ethers Chemical class 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 229920000548 poly(silane) polymer Polymers 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
- ZQTYRTSKQFQYPQ-UHFFFAOYSA-N trisiloxane Chemical compound [SiH3]O[SiH2]O[SiH3] ZQTYRTSKQFQYPQ-UHFFFAOYSA-N 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 still residue of alkylamine, the still residue of silyl ether containing 70% byproduct octamethyltrisiloxane is added with potassium hydroxide and phase transfer catalyst, through the way of alkaline hydrolysis reflux, octamethyltrisiloxane is decomposed completely and reacts into silyl ether with purity about 92%, the silyl ether obtained can get qualified silyl ether that can continue to be used for reacting through the way of atmospheric pressure rectification; after the residual kettle residue in the reaction is hydrolyzed by water, the upper layer organic phase is a small amount of high-heat-value polymer, and the lower layer alkali liquor can be directly decolorized and then evaporated to dryness to obtain solid potassium hydroxide for reuse; the method not only solves the problem that the alkylamine byproduct is difficult to treat, but also recycles a large amount of silicon ether and increases the production benefit.
Description
Technical Field
The invention relates to a method for recycling alkylamine kettle residue, in particular to a method for recycling byproduct octamethyltrisiloxane generated in the production process of hexamethyldisilane amine.
Background
Hexamethyldisilane amine is an important medical intermediate raw material and is also a basic raw material of an organic silicon product. In recent years, the application of the composite material in photoelectric materials, ceramic precursors, photovoltaic materials, carbon silicon materials, polysilane intermediates and the like is attracting more and more attention. However, corresponding byproducts are generated in the process of producing hexamethyldisilane amine, wherein the byproducts contain octamethyltrisiloxane and a small amount of silicon ether, the treatment of the high-boiling point byproduct octamethyltrisiloxane always troubles related enterprises, most of the existing treatment methods for the alkylamine byproduct octamethyltrisiloxane are directly subjected to incineration treatment or directly transferred as hazardous waste, a large amount of silicon dioxide solid is generated in the incineration treatment, the environment is damaged, and the hazardous waste transfer causes the waste of raw materials and increases the cost. However, as for the cleaning treatment method of octamethyltrisiloxane as a byproduct of alkylamine, no relevant report is found in reference to domestic and foreign documents, and in view of the situation that the supervision on hazardous waste treatment is gradually stricter in the current country, the cleaning treatment method is urgently needed to be developed and researched.
Disclosure of Invention
In order to solve the problems, the invention provides that the silyl ether kettle residue containing 70% of byproduct octamethyltrisiloxane is added with potassium hydroxide and a phase transfer catalyst, the octamethyltrisiloxane is thoroughly decomposed and reacted into silyl ether with the purity of about 92% in an alkaline hydrolysis reflux mode, and the obtained silyl ether can be subjected to normal pressure rectification to obtain qualified silyl ether which can be continuously used for reaction; after the residual kettle residue in the reaction is hydrolyzed by water, the upper layer organic phase is a small amount of high-heat-value polymer, and the lower layer alkali liquor can be directly decolorized and then evaporated to dryness to obtain solid potassium hydroxide for reuse; the method not only solves the problem that the alkylamine byproduct is difficult to treat, but also recycles a large amount of silicon ether and increases the production benefit.
In view of the above, the invention provides a method for obtaining qualified silyl ether by carrying out alkaline hydrolysis on octamethyltrisiloxane into silyl ether through treatment from alkylamine kettle residue and rectifying the silyl ether.
The alkaline potassium hydroxide has the best alkaline hydrolysis effect, the alkalinity of the sodium hydroxide is weaker than that of the potassium hydroxide, the alkaline hydrolysis reaction is incomplete by using the sodium hydroxide, and the alkaline hydrolysis effect is poor.
The technical scheme of the invention is realized as follows: adding the alkylamine kettle residue, potassium hydroxide and a phase transfer catalyst into a reaction kettle, and completely reacting octamethyltrisiloxane into silyl ether with the purity of 92% in an alkaline hydrolysis reflux mode, wherein the obtained silyl ether can be rectified under normal pressure to obtain qualified and continuously-used silyl ether; after the residual kettle residue in the reaction is hydrolyzed by water, the upper organic phase is a small amount of high-heat-value polymer and can be directly incinerated, and the lower alkali liquor can be directly decolorized and evaporated to dryness to obtain solid potassium hydroxide for reuse.
The technical scheme of the invention is as follows:
(1) adding the alkylamine kettle residue and the potassium hydroxide solid into a reaction kettle, adding a phase transfer catalyst, and heating to reflux reaction;
(2) the temperature is reduced from 124 ℃ to 102 ℃ along with the reaction, and the reaction is carried out for 6 hours under stable reflux;
the early stage reflux temperature is 124 ℃ and is high boiling point octamethyltrisiloxane, octamethyltrisiloxane is reacted into silicon ether through reaction group trisiloxane, the boiling point of the mixed solution is reduced from 124 ℃ to about 102 ℃ of the boiling point of the silicon ether, and stable reflux is started to be maintained at 102 ℃.
(3) Sampling every 1h to detect the reaction condition, and after 6h, the octamethyltrisiloxane can completely react;
(4) the purity of the silicon ether evaporated at normal pressure is 92 percent;
(5) hydrolyzing the residual kettle residue with water, wherein the upper organic phase is a small amount of high-heat-value polymer and can be directly incinerated, and the lower alkali solution is decolorized by adding activated carbon and then is rotary-evaporated to dryness to obtain solid potassium hydroxide which can be reused;
(6) rectifying the silicon 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 silicon ether is more than 99%, the moisture content is less than 0.05%, the obtained silicon ether is qualified, subsequent experiments can be carried out, and qualified products can be obtained.
The amount of potassium hydroxide added in step (1) is determined according to the amount of octamethyltrisiloxane, and the molar ratio of octamethyltrisiloxane to potassium hydroxide is in the range of 1:1 to 1:3, preferably 1:1.2 to 1: 1.8. The phase transfer catalyst is selected from DMAP, octadeca-coronene (1,4,7,10,13, 16-hexaoxacyclooctadecane, which is crown ether), tetrabutyl ammonium 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, the residual alkylamine kettle is added with solid alkali and a phase transfer catalyst to carry out alkaline hydrolysis reaction until all byproduct octamethyltrisiloxane is reacted into silicon ether, and then the silicon ether with the purity of 92 percent is evaporated under normal pressure;
(2) the method can completely recover the crude distilled silyl ether with the purity of 92 percent by rectifying under normal pressure to obtain the directly used high-purity and low-moisture silyl ether, wherein the purity of the silyl ether is more than 99 percent, and the moisture is less than 0.05 percent.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. Given the embodiments of the present invention, all other embodiments that can be obtained by a person of ordinary skill in the art without inventive faculty are within the scope of the present invention. Furthermore, it should be understood that various changes and modifications can be made by those skilled in the art after reading the teachings of the present invention, and such equivalents also fall within the scope of the appended claims
The alkylamine kettle residue containing byproduct octamethyltrisiloxane produced in a certain production workshop is taken as a treatment object, and the alkylamine kettle residue used in the embodiment of the invention contains byproduct octamethyltrisiloxane about 70%.
Example 1:
(1) adding alkylamine kettle residue 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 a catalyst is 1: 0.001);
(2) slowly heating to a 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 basically fully reacting the byproduct octamethyltrisiloxane;
(4) the purity of the silicon ether is about 92 percent by adopting a normal pressure distillation mode;
(5) hydrolyzing the residual kettle residue with water, standing for layering, wherein the upper organic layer is a small amount of high-heat-value polymer and can be directly incinerated, and the lower alkali solution is decolorized by adding activated carbon and then is subjected to rotary evaporation and evaporation to dryness to obtain solid potassium hydroxide which can be repeatedly used;
(6) rectifying the silicon ether with the purity of about 92 percent at normal pressure;
(7) starting rectification, and adjusting the reflux ratio to be 3: 1;
(8) heating to the gas phase temperature of 60 ℃ to start collecting front distillate, and stopping collecting the front distillate at the temperature of 99.5 ℃; the front fraction is silicon ether with lower purity, and can participate in the next batch of rectification to continue rectification;
(9) continuously heating, and collecting qualified fraction with the gas phase temperature of 99.5-100 ℃;
(10) and (4) sending the qualified fractions to a sample to detect the purity, the moisture and byproducts of the silicon ether.
Example 2:
(1) adding alkylamine kettle residue 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 octadecanohexa (the molar ratio of octamethyltrisiloxane to a catalyst is 1: 0.001);
(2) slowly heating to a 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 basically fully reacting the byproduct octamethyltrisiloxane;
(4) the purity of the silicon ether is about 92 percent by adopting a normal pressure distillation mode;
(5) hydrolyzing the residual kettle residue with water, standing for layering, wherein the upper organic layer is a small amount of high-heat-value polymer and can be directly incinerated, and the lower alkali solution is decolorized by adding activated carbon and then is subjected to rotary evaporation and evaporation to dryness to obtain solid potassium hydroxide which can be repeatedly used;
(6) rectifying the silicon ether with the purity of about 92 percent at normal pressure;
(7) starting rectification, and adjusting the reflux ratio to be 3: 1;
(8) heating to the gas phase temperature of 60 ℃ to start collecting front distillate, and stopping collecting the front distillate at the temperature of 99.5 ℃;
(9) continuously heating, and collecting qualified fraction with gas phase temperature of 99.5-100 ℃;
(10) and (4) sending the qualified fractions to a sample to detect the purity, the moisture and byproducts of the silicon ether.
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 a catalyst is 1: 0.001);
(2) slowly heating to a 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 basically fully reacting the byproduct octamethyltrisiloxane;
(4) the purity of the silicon ether is about 92 percent by adopting a normal pressure distillation mode;
(5) hydrolyzing the residual kettle residue with water, standing for layering, wherein the upper organic layer is a small amount of high-heat-value polymer and can be directly incinerated, and the lower alkali solution is decolorized by adding activated carbon and then is subjected to rotary evaporation and evaporation to dryness to obtain solid potassium hydroxide which can be repeatedly used;
(6) rectifying the silicon ether with the purity of about 92 percent at normal pressure;
(7) starting rectification, and adjusting the reflux ratio to be 3: 1;
(8) heating to the gas phase temperature of 60 ℃ to start collecting front distillate, and stopping collecting the front distillate at the temperature of 99.5 ℃;
(9) continuously heating, and collecting qualified fraction with the gas phase temperature of 99.5-100 ℃;
(10) and (4) sending the qualified fractions to a sample to detect the purity, the moisture and byproducts of the silicon ether.
The raw material alkylamine still residue and the generated silyl ether of the embodiment 1-3 are respectively detected by gas chromatography, and the following data are obtained:
| item | Raw material of alkylamine still residue | Example 1 | Example 2 | Example 3 |
| Silicon ether purity/%) | 26.14 | 99.46 | 99.51 | 99.53 |
| By-production of octa A/%) | 70.19 | Not detected out | Not detected out | Not detected out |
| Water content/%) | -- | 0.02 | 0.03 | 0.02 |
The data show that the treatment method can obtain high-purity silicon ether, simultaneously the byproduct octamethyltrisiloxane can be completely reacted, the treatment method is simpler, and the recovery rate is high.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (6)
1. The method for recovering the alkylamine kettle residue is characterized by comprising the following steps of:
(1) adding the alkylamine kettle residue containing octamethyltrisiloxane and potassium hydroxide solid into a reaction kettle, adding a phase transfer catalyst, and heating to reflux reaction;
(2) the temperature is reduced from 124 ℃ to 102 ℃ along with the reaction, and the reaction is carried out for 6 hours under stable reflux;
(3) sampling every 1h to detect the reaction condition, and after 6h, completely reacting the octamethyltrisiloxane;
(4) the purity of the silicon ether evaporated at normal pressure is 92 percent;
(5) and (4) rectifying the silicon ether obtained in the step (4) at normal pressure, and collecting the fraction at 99.5-100 ℃ to obtain qualified fraction silicon ether.
2. The process of claim 1, wherein the process comprises: and (4) adding water into the residual kettle residue in the step (4) for hydrolysis, wherein the upper layer organic phase is a small amount of high-heat-value polymer and can be directly subjected to incineration treatment, and the lower layer alkali liquor is decolorized by adding activated carbon and then is subjected to rotary evaporation and evaporation to dryness to obtain solid potassium hydroxide which can be repeatedly used.
3. The process of claim 1, wherein the process comprises: the molar ratio of the octamethyltrisiloxane to the potassium hydroxide in step (1) is in the range of 1:1 to 1: 3.
4. The process of claim 1, wherein the process comprises: the phase transfer catalyst is selected from DMAP, octodecahexa-crown and tetrabutylammonium bromide.
5. The process for the recovery of the alkylamine still residue according to claim 1 to 4, wherein: the molar ratio of octamethyltrisiloxane to phase transfer catalyst was 1: 0.001.
6. The process for the recovery of the alkylamine still residue according to claim 1 to 4, wherein: the purity of the qualified fraction silicon ether is more than 99%, and the moisture content is less than 0.05%.
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| CN202210537827.0A CN114805422A (en) | 2022-05-17 | 2022-05-17 | Method for recovering silicon ether from alkylamine kettle residue |
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| CN202210537827.0A CN114805422A (en) | 2022-05-17 | 2022-05-17 | Method for recovering silicon ether from alkylamine kettle residue |
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