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Synthesis method and application of 1, 3-bis (isocyanate alkyl)-1, 1, 3, 3-tetramethyldisiloxane

A technology of tetramethyldisiloxane and alkyl carbamate silane, which is applied in the field of compound synthesis, can solve the problems of low yield of alkyl carbamate, difficult separation of products, large amount of raw materials, etc., so as to reduce the input of raw materials. The effect of cost, short synthesis time and simple process

Pending Publication Date: 2021-08-24
唐山三孚新材料有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing process prepares the alkyl carbamate with a low yield by reacting 1,3-bis(chloropropyl)-1,1,3,3-tetramethyldisiloxane with dimethyl carbonate, and the initial investment The amount of raw materials is large, and there are many by-products in the cracking process, and the products are difficult to separate
The yield of the alkyl carbamate prepared by the reaction is low

Method used

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  • Synthesis method and application of 1, 3-bis (isocyanate alkyl)-1, 1, 3, 3-tetramethyldisiloxane
  • Synthesis method and application of 1, 3-bis (isocyanate alkyl)-1, 1, 3, 3-tetramethyldisiloxane
  • Synthesis method and application of 1, 3-bis (isocyanate alkyl)-1, 1, 3, 3-tetramethyldisiloxane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] A kind of synthetic method of 1,3-bis(isocyanatoalkyl)-1,1,3,3-tetramethyldisiloxane, the steps are as follows:

[0032] The first step: chloropropyldimethylmethoxysilane, sodium cyanate and methanol were reacted at 130° C. and a pressure of 0.1 MPa for 13 hours at a molar ratio of 1:2.5:3 to synthesize methyl carbamate silane.

[0033] The second step: Add methyl carbamate silane dropwise to water at 80°C for hydrolysis, wherein the volume ratio of water to methyl carbamate silane is 3:1, to obtain 1,3-bis(carbamate methyl propyl base)-1,1,3,3-tetramethyldisiloxane, the end of the dropwise addition means the end of the second step reaction.

[0034] The third step: first add triethylamine to 1,3-bis(carbamate propyl)-1,1,3,3-tetramethyldisiloxane, and then add Add trimethylchlorosilane dropwise to 1,3-bis(carbamate propyl)-1,1,3,3-tetramethyldisiloxane, and the addition is completed in 4 hours to obtain trimethylsilyl methyl carbamate silane. Wherein, the molar rati...

Embodiment 2

[0037] A kind of synthetic method of 1,3-bis(isocyanatoalkyl)-1,1,3,3-tetramethyldisiloxane, the steps are as follows:

[0038] The first step: chloropropyldimethylmethoxysilane, potassium cyanate and ethanol were reacted at 180° C. and a pressure of 0.2 MPa for 11 hours at a molar ratio of 1:2.5:3 to synthesize urethane silane.

[0039] The second step: Add urethane silane dropwise to water at 100°C for hydrolysis, wherein the volume ratio of water to urethane silane is 5:1.5 to obtain 1,3-bis(urethane propyl base)-1,1,3,3-tetramethyldisiloxane, the end of the dropwise addition means the end of the second step reaction.

[0040] The third step: first add triethylamine to 1,3-bis(carbamate ethyl propyl)-1,1,3,3-tetramethyldisiloxane, and then add triethylamine to 1 at 50°C , 3-bis(carbamate ethyl propyl)-1,1,3,3-tetramethyldisiloxane was added dropwise with trimethylchlorosilane, and the addition was completed in 4 hours to obtain trimethylsilyl carbamic acid ethyl silane. ...

Embodiment 3

[0043] A kind of synthetic method of 1,3-bis(isocyanatoalkyl)-1,1,3,3-tetramethyldisiloxane, the steps are as follows:

[0044] The first step: chloropropyldimethylethoxysilane, magnesium cyanate and tert-butanol were reacted at 80°C and a pressure of 0.1MPa for 14 hours at a molar ratio of 1:2.5:3 to synthesize tert-butyl carbamate silane.

[0045] Step 2: Add tert-butyl carbamate silane dropwise to water at 25°C for hydrolysis, wherein the volume ratio of water to tert-butyl carbamate silane is 4:1 to obtain 1,3-bis(tert-butyl carbamate Butylcarboxypropyl)-1,1,3,3-tetramethyldisiloxane, the end of the dropwise addition means the end of the second step reaction.

[0046]The third step: first add triethylamine to 1,3-bis(tert-butylcarbamate propyl)-1,1,3,3-tetramethyldisiloxane, and then Add trimethylchlorosilane dropwise to 1,3-bis(tert-butylcarbamate propyl)-1,1,3,3-tetramethyldisiloxane, and the addition is completed in 4 hours to obtain trimethyl Silyl tert-butyl carbama...

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Abstract

The invention discloses a synthesis method and application of 1, 3-bis (isocyanate alkyl)-1, 1, 3, 3-tetramethyldisiloxane, which relates to the technical field of compound synthesis. According to the synthesis method, cyanate, alkyl alcohol and chloralkane silane react to obtain carbamic acid alkyl ester silane, so that the raw material input cost is effectively reduced; trimethylchlorosilane is used as a protective agent to protect secondary amine on the alkyl carbamate double end socket, so that polymerization reaction phenomena such as by-products and the like are prevented from occurring again in the cracking process. The synthesis method is simple in process, short in synthesis time and high in synthesis efficiency, the yield of a finished product can reach 95% or above, and industrial mass production is facilitated. The 1, 3-bis (isocyanate alkyl)-1, 1, 3, 3-tetramethyldisiloxane is mostly applied as a preparation raw material in polyurethane, coatings, sealants and polyether modified products.

Description

technical field [0001] The invention relates to the technical field of compound synthesis, in particular to a synthesis method and application of 1,3-bis(isocyanatoalkyl)-1,1,3,3-tetramethyldisiloxane. Background technique [0002] In the existing related technology, mostly adopt dimethyl carbonate and 1,3-bis(chloropropyl)-1,1,3,3-tetramethyldisiloxane to react to produce alkyl carbamate, and then crack Get subsequent corresponding products. The existing process prepares the alkyl carbamate with a low yield by reacting 1,3-bis(chloropropyl)-1,1,3,3-tetramethyldisiloxane with dimethyl carbonate, and the initial investment The amount of raw materials is large, and there are many by-products in the cracking process, and the products are difficult to separate. The yield of the alkyl carbamate prepared by the reaction is low. [0003] Therefore, on the basis of reducing the input cost of raw materials, a new synthesis process that can further increase the yield of alkyl carba...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/10C08G18/77C08G65/336
CPCC07F7/0889C08G18/778C08G65/336
Inventor 高胜波刘嵚陈辉李庆李越祁拥军郑泽
Owner 唐山三孚新材料有限公司
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