CN114349783B - Method for preparing neutral alkoxy disilane by taking organosilicon high-boiling-point substances as raw materials - Google Patents
Method for preparing neutral alkoxy disilane by taking organosilicon high-boiling-point substances as raw materials Download PDFInfo
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- -1 alkoxy disilane Chemical compound 0.000 title claims abstract description 46
- 238000000034 method Methods 0.000 title claims abstract description 41
- 230000007935 neutral effect Effects 0.000 title claims abstract description 39
- 239000000126 substance Substances 0.000 title claims abstract description 28
- 239000002994 raw material Substances 0.000 title claims abstract description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 68
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 29
- 238000005406 washing Methods 0.000 claims abstract description 25
- 238000006136 alcoholysis reaction Methods 0.000 claims abstract description 22
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000004202 carbamide Substances 0.000 claims abstract description 21
- 238000009835 boiling Methods 0.000 claims abstract description 18
- 238000003756 stirring Methods 0.000 claims abstract description 13
- 150000001412 amines Chemical class 0.000 claims abstract description 11
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 10
- 239000010703 silicon Substances 0.000 claims abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 5
- 239000003929 acidic solution Substances 0.000 claims abstract description 4
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 4
- 238000009833 condensation Methods 0.000 claims abstract description 4
- 230000005494 condensation Effects 0.000 claims abstract description 4
- 238000010992 reflux Methods 0.000 claims abstract description 4
- 239000002253 acid Substances 0.000 claims description 55
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 20
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 16
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 4
- 239000000460 chlorine Substances 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims description 2
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims 2
- 229920001296 polysiloxane Polymers 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 7
- 238000003860 storage Methods 0.000 abstract description 5
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- 239000003795 chemical substances by application Substances 0.000 abstract description 2
- 230000003472 neutralizing effect Effects 0.000 abstract 1
- 239000000047 product Substances 0.000 description 20
- 239000003921 oil Substances 0.000 description 19
- 125000001301 ethoxy group Chemical group [H]C([H])([H])C([H])([H])O* 0.000 description 17
- 238000006243 chemical reaction Methods 0.000 description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 239000002699 waste material Substances 0.000 description 5
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 4
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 4
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- YGZSVWMBUCGDCV-UHFFFAOYSA-N chloro(methyl)silane Chemical compound C[SiH2]Cl YGZSVWMBUCGDCV-UHFFFAOYSA-N 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 229920000180 alkyd Polymers 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 239000013049 sediment Substances 0.000 description 2
- 229910000077 silane Inorganic materials 0.000 description 2
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 2
- 235000017557 sodium bicarbonate Nutrition 0.000 description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 description 2
- 229910003849 O-Si Inorganic materials 0.000 description 1
- 229910003872 O—Si Inorganic materials 0.000 description 1
- 229910008045 Si-Si Inorganic materials 0.000 description 1
- 229910006411 Si—Si Inorganic materials 0.000 description 1
- 125000003545 alkoxy group Chemical group 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 229910021419 crystalline silicon Inorganic materials 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 238000004078 waterproofing Methods 0.000 description 1
Abstract
The invention provides a method for preparing neutral alkoxy disilane by taking an organosilicon high-boiling residue as a raw material, belonging to the field of organosilicon material synthesis. Adding the organic silicon high-boiling-point substances into a device with stirring and condensation reflux, and dropwise adding alcohol to carry out alcoholysis reaction; adding the acidic solution obtained by alcoholysis into a rectifying device, and then adding alcohol for alcohol washing; after the alcohol washing is finished, the neutral alkoxy disilane is obtained through two-stage neutralization at normal temperature, the first-stage urea neutralization and the second-stage organic amine reagent neutralization. The invention has the advantages that: the recovered alcohol can be subjected to alcoholysis to form alcohol circulation, so that the material loss is reduced, the consumption of a neutralizing agent is reduced, water is not generated in the neutralization process, and the storage stability of the neutral alkoxy disilane is not damaged.
Description
Technical Field
The invention belongs to the technical synthesis field of organosilicon materials, and particularly relates to a method for preparing neutral alkoxy disilane by taking organosilicon high-boiling residues as raw materials.
Background
The high-boiling-point substances are byproducts generated in the methyl chlorosilane monomer synthesis process, have a certain practical value, are used as a silane mixture taking Si-Si, si-O-Si and Si-C-Si as main chains, and are difficult to store and use due to HCl corrosive gas generated by easy hydrolysis of silicon-chlorine bonds contained in the silane mixture, meanwhile, a method for simply preparing the high-boiling-point substances into products with a higher practical value is not available, a great deal of backlog causes serious resource waste, environmental protection problems and potential safety hazards, and the development of the methyl chlorosilane in industrial scale is hindered. Therefore, the high-efficiency treatment of the high-boiling-point substances has important significance for the development of the methylchlorosilanes industry in China.
At present, the domestic treatment methods for the organic silicon high-boiling-point substances include the following methods: alcoholysis to prepare alkoxy disilane, hydrolysis to prepare waterproofing agent and silicone resin, cracking to prepare monosilane, and the like. The preparation of alkoxy disilane by an alcoholysis method is important, and the product has wide application, simple process, circular economy and less secondary pollution, but has some problems: the waste alkyd solution can not be recycled, a large amount of three wastes are generated, the alkoxy disilane is difficult to neutralize, the oil yield is low, the acid return is easy, the molecular weight is difficult to control, and the like. Known methods for the production of alkoxy disilanes are described in chinese patents CN102408568A, CN101456955A, CN102516543a, CN105713033B.
Disclosure of Invention
The invention aims to solve the problems in the prior art, and provides a method for preparing neutral alkoxy disilane by taking organosilicon high-boiling substances as raw materials, which has the advantages of reduced three-waste emission, stable product quality, high oil yield and simple process in the production process.
A method for preparing neutral alkoxy disilane by taking organosilicon high-boiling residues as raw materials comprises the following steps:
(1) Alcoholysis: adding the organic silicon high-boiling-point substances into a device with stirring and condensation reflux, dropwise adding alcohol, carrying out alcoholysis reaction, and circularly absorbing the generated HCl tail gas by using absorption tower water;
(2) Alcohol washing: adding the acidic solution obtained by alcoholysis into a rectifying device, and then adding alcohol for alcohol washing;
(3) And (3) neutralization: after the alcohol washing is finished, the neutral alkoxy disilane is obtained through two-stage neutralization at normal temperature, the first-stage urea neutralization and the second-stage organic amine reagent neutralization.
The organic silicon high-boiling-point substance is as follows: the boiling point range is 120-160 ℃, and the main chain contains silicon-silicon bonds and at least two silicon-chlorine bonds; the molecular formula of the high-boiling-point substance component is as follows: r is R m Si 2 Cl 6-m M is an integer of 0 to 4, and R is methyl.
The mass ratio of the organic silicon high-boiling-point substance to the alcohol is 2:1-4.
The alcoholysis reaction temperature is 30-60 ℃, and the stirring speed is 200-300r/min in the alcoholysis process.
The alcohol is methanol or ethanol.
In the alcohol washing process, the adding amount of the alcohol is 1-3 times of the mass of the organic silicon high-boiling-point substances, the alcohol is distilled at the temperature of 80-100 ℃ and the stirring speed of 200-300r/min, and the acid value of the alkoxy disilane is reduced to 80-100mgKOH/g.
In the step (3), the organic amine is an alcohol amine, more specifically one or a mixture of triethanolamine, diethanolamine and monoethanolamine, the urea dosage is 10-15% of the mass of the organic silicon high-boiling-point substances, and the organic amine dosage is 5-10% of the mass of the organic silicon high-boiling-point substances.
In the step (3), the acid value of the first-stage urea neutralized alkoxy disilane is 25-40mgKOH/g, and the acid value of the second-stage organic amine reagent neutralized alkoxy disilane is 0.2-1.0mgKOH/g.
Compared with the prior art, the invention has the following advantages:
1. the recovered alcohol can be subjected to alcoholysis to form alcohol circulation, HCl gas absorbed by the absorption tower can be prepared into hydrochloric acid solution, waste alkyd solution generated by other invention is avoided, and material loss is reduced.
2. The neutralization is easier, the consumption of the neutralizer is reduced, the generated solid waste is reduced, the urea is economical, the organic amine is easy to disperse in the system, and the acid value can be reduced to below 0.5.
3. No water is produced during the neutralization process and the storage stability of the neutral alkoxysilane is not impaired.
Detailed Description
Example 1
200kg of organosilicon high-boiling-point substances (molecular formula: R) m Si 2 Cl 6-m M is an integer of 0-4, R is methyl), adding a device with stirring and condensation reflux, dropwise adding 100kg of ethanol to start alcoholysis, controlling the temperature at 35 ℃, stirring at 200R/min, and circularly absorbing the generated HCl tail gas by using an absorption tower water. Adding the brown yellow transparent acidic solution obtained by alcoholysis into a condensing and rectifying device, adding 300kg of ethanol in the alcohol washing step, rectifying and recovering the ethanol at the temperature of 100 ℃, and stirring at the rotating speed of 200r/min. After the alcohol washing is finished, the acid value of the alkoxy disilane is reduced to 99mgKOH/g, the normal temperature is maintained, 30kg of urea is added for neutralization, the stirring speed is 200r/min, the stirring is carried out for 60min, white sediment is generated, the filtering is carried out, the acid value of the alkoxy disilane is reduced to 36mgKOH/g, 18kg of triethanolamine is added for neutralization, the stirring is carried out for 60min, the white sediment is generated, and the light yellow transparent neutral alkoxy disilane is obtained after the filtering.
The alkoxy disilane (formula: R) m Si 2 X 6-m M is an integer from 0 to 4, R is methyl and X is ethoxy) product: viscosity (25 ℃ C., mm) 2 /s）2.5，The acid value (mgKOH/g) was 0.4, and the oil yield was 88.2%.
Example 2
The procedure was as in example 1, except that the alcohol washing step was not carried out, the acid value of the alkoxysilane was lowered to 520mgKOH/g, kept at ordinary temperature, neutralized by adding 157kg of urea, the acid value of the alkoxysilane was lowered to 36mgKOH/g, and then neutralized by adding 19kg of triethanolamine, to give a pale yellow transparent neutral alkoxysilane.
The alkoxy disilane (formula: R) m Si 2 X 6-m M is an integer from 0 to 4, R is methyl and X is ethoxy) product: the viscosity (25 ℃ C., mm 2/s) was 4.3, the acid value (mgKOH/g) was 0.7, and the oil yield was 12.6%.
Example 3
The procedure was as in example 1 except that the ethanol was added in the alcohol washing step to 100kg, the acid value of the alkoxysilane was lowered to 192mgKOH/g, the reaction was kept at room temperature, the acid value of the neutralized alkoxysilane was lowered to 48mgKOH/g by adding 52kg of urea, and then the neutral alkoxysilane was obtained by neutralization by adding 24kg of triethanolamine.
The alkoxy disilane (formula: R) m Si 2 X 6-m M is an integer from 0 to 4, R is methyl and X is ethoxy) product: the viscosity (25 ℃ C., mm 2/s) was 3.4, the acid value (mgKOH/g) was 0.3, and the oil yield was 39.6%.
Example 4
The procedure was as in example 1 except that 200kg of ethanol was added in the alcohol washing step, the acid value of the alkoxysilane was reduced to 145mgKOH/g, the reaction was kept at room temperature, the acid value of the neutralized alkoxysilane was reduced to 42mgKOH/g by adding 43kg of urea, and then the neutral alkoxysilane was obtained by neutralization by adding 26kg of triethanolamine.
The alkoxy disilane (formula: R) m Si 2 X 6-m M is an integer from 0 to 4, R is methyl and X is ethoxy) product: the viscosity (25 ℃ C., mm 2/s) was 3.3, the acid value (mgKOH/g) was 0.5, and the oil yield was 63.7%.
Example 5
The procedure was as in example 1 except that the ethanol was added in the alcohol washing step to 400kg, the acid value of the alkoxysilane was reduced to 76mgKOH/g, the reaction was kept at room temperature, the acid value of the neutralized alkoxysilane was reduced to 33mgKOH/g by adding 22kg of urea, and then the neutral alkoxysilane was obtained by neutralization by adding 16kg of triethanolamine.
The alkoxy disilane (formula: R) m Si 2 X 6-m M is an integer from 0 to 4, R is methyl and X is ethoxy) product: the viscosity (25 ℃ C., mm 2/s) was 2.4, the acid value (mgKOH/g) was 0.9, and the oil yield was 84.5%.
Example 6
The procedure was as in example 1 except that the ethanol was added in the alcohol washing step to 500kg, the acid value of the alkoxysilane was reduced to 61mgKOH/g, the reaction was kept at room temperature, the acid value of the neutralized alkoxysilane was reduced to 30mgKOH/g by adding 18kg of urea, and then the neutral alkoxysilane was obtained by neutralization by adding 16kg of triethanolamine.
The alkoxy disilane (formula: R) m Si 2 X 6-m M is an integer from 0 to 4, R is methyl and X is ethoxy) product: the viscosity (25 ℃ C., mm 2/s) was 2.7, the acid value (mgKOH/g) was 0.2, and the oil yield was 79.4%.
Example 7
The procedure was as in example 1 except that the ethanol was added in the alcohol washing step to 600kg, the acid value of the alkoxysilane was reduced to 51mgKOH/g, the reaction was kept at room temperature, the acid value of the neutralized alkoxysilane was reduced to 29mgKOH/g by adding 16kg of urea, and then the neutral alkoxysilane was obtained by neutralization by adding 15kg of triethanolamine.
The alkoxy disilane (formula: R) m Si 2 X 6-m M is an integer from 0 to 4, R is methyl and X is ethoxy) product: the viscosity (25 ℃ C., mm 2/s) was 2.1, the acid value (mgKOH/g) was 0.8, and the oil yield was 72.8%.
Example 8
The procedure was as in example 1 except that the ethanol was added in the alcohol washing step to 700kg, the acid value of the alkoxysilane was reduced to 43mgKOH/g, the reaction was kept at room temperature, the acid value of the neutralized alkoxysilane was reduced to 26mgKOH/g by adding 14kg of urea, and then the neutral alkoxysilane was obtained by neutralization by adding 14kg of triethanolamine.
The alkoxy disilane (formula: R) m Si 2 X 6-m M is an integer from 0 to 4, R is methyl and X is ethoxy) product: the viscosity (25 ℃ C., mm 2/s) was 2.4, the acid value (mgKOH/g) was 1.0, and the oil yield was 67.4%.
Example 9
The procedure was as in example 1, except that urea alone was used in the neutralization step, 200kg of urea was used to neutralize the alkoxysilane acid value down to 11mgKOH/g, and no neutral alkoxysilane was obtained.
The alkoxy disilane (formula: R) m Si 2 X 6-m M is an integer from 0 to 4, R is methyl and X is ethoxy) product: the viscosity (25 ℃ C., mm 2/s) was 15.6, the acid value (mgKOH/g) was 11, and the oil yield was 25.7%.
Example 10
The procedure was as in example 1 except that only triethanolamine was used in the neutralization step, and 74kg triethanolamine was used to neutralize the alkoxysilane acid number down to 0.8mgKOH/g to give a pale yellow transparent neutral alkoxysilane.
The alkoxy disilane (formula: R) m Si 2 X 6-m M is an integer from 0 to 4, R is methyl and X is ethoxy) product: the viscosity (25 ℃ C., mm 2/s) was 6.7, the acid value (mgKOH/g) was 0.8, and the oil yield was 32.9%.
Example 11
The procedure was as in example 1 except that only sodium carbonate was added in the neutralization step, and 70kg of sodium carbonate was added to neutralize the alkoxysilane acid value down to 0.8mgKOH/g, to obtain a neutral alkoxysilane having a pale yellow transparent water content (deterioration of the storage stability of the neutral alkoxysilane).
The alkoxy disilane (formula: R) m Si 2 X 6-m M is an integer from 0 to 4, R is methyl and X is ethoxy) product: the viscosity (25 ℃ C., mm 2/s) was 4.3, the acid value (mgKOH/g) was 0.8, and the oil yield was 24.6%.
Example 12
The procedure was as in example 1 except that only sodium hydrogencarbonate was added in the neutralization step, and 92kg of sodium hydrogencarbonate was added to neutralize the alkoxysilane acid value down to 1.0mgKOH/g, to give a neutral alkoxysilane having a pale yellow transparent water content (impairing the storage stability of the neutral alkoxysilane).
The alkoxy disilane (formula: R) m Si 2 X 6-m M is an integer from 0 to 4, R is methyl and X is ethoxy) product: the viscosity (25 ℃ C., mm 2/s) was 3.4, the acid value (mgKOH/g) was 1.0, and the oil yield was 20.8%.
Example 13
The procedure was as in example 1 except that only sodium hydroxide was added in the neutralization step, and that the acid value of the neutralized alkoxysilane was reduced to 0.7mgKOH/g by adding 51kg of sodium hydroxide, to obtain a neutral alkoxysilane having a pale yellow transparent water content (deterioration of the storage stability of the neutral alkoxysilane).
The alkoxy disilane (formula: R) m Si 2 X 6-m M is an integer from 0 to 4, R is methyl and X is ethoxy) product: the viscosity (25 ℃ C., mm 2/s) was 2.9, the acid value (mgKOH/g) was 0.7, and the oil yield was 31.4%.
Example 14
The procedure was the same as in example 1, except that 100kg of ethanol in the alcoholysis step was changed to 100kg of acid ethanol recovered in the alcohol washing step, the acid value of the alkoxysilane after alcohol washing was reduced to 131mgKOH/g, the reaction was maintained at room temperature, the acid value of the neutralized alkoxysilane by adding 47kg of urea was reduced to 34mgKOH/g, and then the reaction was further neutralized by adding 17kg of triethanolamine, to give pale yellow transparent neutral alkoxysilane.
The alkoxy disilane (formula: R) m Si 2 X 6-m M is an integer from 0 to 4, R is methyl and X is ethoxy) product: the viscosity (25 ℃ C., mm 2/s) was 2.3, the acid value (mgKOH/g) was 0.5, and the oil yield was 80.7%.
Example 15
The procedure was as in example 14 except that the acid value of the alkoxysilane was reduced to 106mgKOH/g by the alcohol washing in the alcoholysis step alone, the normal temperature was maintained, the acid value of the neutralized alkoxysilane was reduced to 37mgKOH/g by the addition of 39kg of urea, and the neutral alkoxysilane was obtained by the neutralization of 18kg of triethanolamine.
The alkoxy disilane (formula: R) m Si 2 X 6-m M is an integer from 0 to 4, R is methyl and X is ethoxy) product: the viscosity (25 ℃ C., mm 2/s) was 2.2, the acid value (mgKOH/g) was 0.6, and the oil yield was 77.6%.
Example 16
The procedure was as in example 14 except that the acid value of the alkoxysilane was reduced to 86mgKOH/g by the alcohol washing in the alcoholysis step alone, the normal temperature was maintained, the acid value of the neutralized alkoxysilane was reduced to 31mgKOH/g by adding 31kg of urea, and then the neutral alkoxysilane was obtained by neutralization by adding 16kg of triethanolamine.
The alkoxy disilane (formula: R) m Si 2 X 6-m M is an integer from 0 to 4, R is methyl and X is ethoxy) product: the viscosity (25 ℃ C., mm 2/s) was 1.9, the acid value (mgKOH/g) was 0.7, and the oil yield was 72.8%.
Example 17
The procedure was as in example 14 except that the acid value of the alkoxysilane was reduced to 71mgKOH/g by alcohol washing in the alcoholysis step alone, and the acid value of the neutralized alkoxysilane was reduced to 32mgKOH/g by adding 24kg of urea, followed by adding 16kg of triethanolamine, thereby obtaining a pale yellow transparent neutral alkoxysilane.
The alkoxy disilane (formula: R) m Si 2 X 6-m M is an integer from 0 to 4, R is methyl and X is ethoxy) product: the viscosity (25 ℃ C., mm 2/s) was 1.9, the acid value (mgKOH/g) was 0.6, and the oil yield was 64.4%.
Claims (8)
1. The method for preparing the neutral alkoxy disilane by taking the organosilicon high-boiling-point substances as raw materials is characterized by comprising the following steps:
(1) Alcoholysis: adding the organic silicon high-boiling-point substances into a device with stirring and condensation reflux, and dropwise adding alcohol to carry out alcoholysis reaction;
(2) Alcohol washing: adding the acidic solution obtained by alcoholysis into a rectifying device, adding alcohol for alcohol washing, wherein the adding amount of the alcohol is 1-3 times of the mass of the organic silicon high-boiling substances in the alcohol washing process, rectifying at 80-100 ℃ at the stirring speed of 200-300r/min, and alcohol washing until the acid value of the alkoxy disilane is reduced to 80-100mgKOH/g;
(3) And (3) neutralization: after the alcohol washing is finished, the neutral alkoxy disilane is obtained through two-stage neutralization at normal temperature, the first-stage urea neutralization and the second-stage organic amine reagent neutralization.
2. The method for preparing neutral alkoxy disilane by using organosilicon high-boiling substances as raw materials according to claim 1, wherein the organosilicon high-boiling substances are as follows: the boiling point range is 120-160 ℃, and the main chain contains silicon-silicon bonds and at least two silicon-chlorine bonds; the molecular formula of the high-boiling-point substance component is as follows: r is R m Si 2 Cl 6-m M is an integer of 0 to 4, and R is methyl.
3. The method for preparing neutral alkoxy disilane by using the organosilicon high-boiling point compound as a raw material according to claim 1, wherein the mass ratio of the organosilicon high-boiling point compound to the alcohol in the step (1) is 2:1-4.
4. The method for preparing neutral alkoxy disilane by using organosilicon high-boiling substances as raw materials according to claim 1, wherein the alcoholysis reaction temperature is 30-60 ℃, and the stirring speed in the alcoholysis process is 200-300r/min.
5. The method for preparing neutral alkoxy disilane by using organosilicon high-boiling substances as raw materials according to claim 1, wherein the alcohol is methanol or ethanol.
6. The method for preparing neutral alkoxy disilane by using the organosilicon high-boiling substances as the raw material according to claim 1, wherein in the step (3), the organic amine is an alcohol amine, the urea is 10-15% of the mass of the organosilicon high-boiling substances, and the organic amine is 5-10% of the mass of the organosilicon high-boiling substances.
7. The method for producing neutral alkoxysilane using high boiling point silicone material according to claim 1, wherein in step (3), the acid value of the first urea-neutralized alkoxysilane is 25 to 40mgKOH/g, and the acid value of the second organic amine reagent-neutralized alkoxysilane is 0.2 to 1.0mgKOH/g.
8. The method for preparing neutral alkoxy disilane by using organosilicon high-boiling point substances as raw materials according to claim 6, wherein the organic amine is one of triethanolamine, diethanolamine, monoethanolamine or a mixture thereof.
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| DE4033156A1 (en) * | 1990-10-12 | 1992-04-16 | Nuenchritz Chemie Gmbh | Prepn. of methyl:alkoxy:oligo(di:silyl)-siloxane cpds. - by two stage alkoxylation of distn. residue from methyl:chlorosilane synthesis or di:silane(s) from residue |
| CN101016383A (en) * | 2007-01-24 | 2007-08-15 | 吉林市凇泰化工有限责任公司 | Method of producing high boiling point silicon oil |
| CN102153752A (en) * | 2010-12-03 | 2011-08-17 | 湖北新四海化工股份有限公司 | Method and device for preparing high-boiling-point silicone oil |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| DE4033156A1 (en) * | 1990-10-12 | 1992-04-16 | Nuenchritz Chemie Gmbh | Prepn. of methyl:alkoxy:oligo(di:silyl)-siloxane cpds. - by two stage alkoxylation of distn. residue from methyl:chlorosilane synthesis or di:silane(s) from residue |
| CN101016383A (en) * | 2007-01-24 | 2007-08-15 | 吉林市凇泰化工有限责任公司 | Method of producing high boiling point silicon oil |
| CN102153752A (en) * | 2010-12-03 | 2011-08-17 | 湖北新四海化工股份有限公司 | Method and device for preparing high-boiling-point silicone oil |
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