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A kind of preparation method of alkynyl polyether

An alkynyl polyether and alkynyl technology are applied in the preparation of alkynyl polyethers and in the field of alkynyl polyethers, which can solve the problems of difficulty in realizing industrialized production, difficulty in realizing industrialization, complicated procedures, etc., and achieve cheap methods and low equipment requirements. , the effect of simple formula

Active Publication Date: 2022-03-25
SHANGHAI MAIPU NEW MATERIAL TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the need to prepare the catalyst twice, the method is complicated and difficult to realize industrialization
[0007] In the above polyether synthesis, sodium hydroxide and potassium hydroxide are often used as catalysts, and sodium hydroxide, potassium hydroxide and alcoholic hydroxyl groups react to produce water, and water further reacts with ethylene oxide and propylene oxide to generate by-products dihydroxyl Polyether; when using sodium methoxide and potassium methoxide as catalyst, sodium methoxide and potassium methoxide react with alcoholic hydroxyl group to generate methanol, and methanol further reacts with ethylene oxide and propylene oxide to generate by-product methyl alkoxylate, And in this process, although methanol is relatively easy to remove, sodium methylate and potassium methylate are highly flammable chemicals, and the methanol generated is a flammable and toxic liquid, which pollutes the environment; using metallic sodium or potassium as a catalyst, although it can Avoid the production of by-products, but metal sodium or potassium is flammable, and the hydrogen generated with unsaturated alcohol is flammable gas, and industrial production is difficult to achieve

Method used

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  • A kind of preparation method of alkynyl polyether
  • A kind of preparation method of alkynyl polyether
  • A kind of preparation method of alkynyl polyether

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Synthesis of alkynyl polyether with phenylacetylene as raw material:

[0030]

[0031] Under a nitrogen atmosphere, add 10 parts by weight of phenylacetylene, 1 part by weight of triethylamine and 0.5 parts by weight of CuI in the reactor, stir at room temperature for 10 minutes, add 500 parts by weight of ethylene oxide and 450 parts by weight of propylene oxide, and heat up Polymerize at 50°C, control the reaction pressure to 0.05-0.20Mpa, react for 3 hours, lower to room temperature and pour into post-treatment tank, after treatment with polyether adsorbent, filter to obtain the product.

Embodiment 2

[0033] Synthesis of alkynyl polyether with p-methylphenylacetylene as raw material:

[0034]

[0035] Under a nitrogen atmosphere, 11 parts by weight of p-methylphenylacetylene, 1 part by weight of DBU (1,8-diazabicycloundec-7-ene) and 0.6 parts by weight of Cu(OAc) were added to the reactor 2 , after stirring at room temperature for 10 minutes, add 600 parts by weight of ethylene oxide and 300 parts by weight of propylene oxide, heat up to 60°C for polymerization, control the reaction pressure at 0.05-0.20Mpa, react for 3 hours, cool down to room temperature and pour in post-treatment Kettle, treated with polyether adsorbent, and filtered to obtain the product.

Embodiment 3

[0037] Synthesis of alkynyl polyethers from 2-ethynyl-1,3,5-trimethylbenzene:

[0038]

[0039] Under a nitrogen atmosphere, add 13 parts by weight of 2-ethynyl-1,3,5-trimethylbenzene, 1 part by weight of Cs 2 CO 3 and 0.7 parts by weight Cu(OTf) 2, after stirring at room temperature for 10 minutes, add 600 parts by weight of ethylene oxide and 400 parts by weight of propylene oxide, heat up to 80 ° C for polymerization, control the reaction pressure 0.05 ~ 0.20Mpa, after 4 hours of reaction, cool down to room temperature and pour in post-treatment Kettle, treated with polyether adsorbent, and filtered to obtain the product.

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Abstract

The invention belongs to the field of chemical industry and provides a method for preparing an alkynyl polyether. The invention utilizes the nucleophilic ring-opening reaction of an alkynyl group on an epoxy compound under the action of a copper catalyst and an alkali to realize the synthesis of an alkynyl polyether . Compared with the prior art, the method of the invention is cheaper, the formula is simpler, and the operation is more convenient. At the same time, it is green, safe, efficient and environmentally friendly, and is suitable for industrial production. Since the alkyne bond is more reactive than the double bond, compared with the allyl polyether, the alkynyl polyether has higher activity, and its addition reaction conditions with organosilane hydrogen compounds are milder and require less equipment. Therefore, through The alkynyl polyether synthesized by the method of the invention has broader application prospects.

Description

technical field [0001] The invention belongs to the field of chemical industry and relates to an alkynyl polyether, in particular to a preparation method of an alkynyl polyether. Background technique [0002] Traditional unsaturated polyethers are polyethers obtained by reacting alcohols containing unsaturated double bonds as initiators with epoxy monomers such as ethylene oxide (EO) and propylene oxide (PO). Alcohols containing unsaturated double bonds include allyl alcohol, methallyl alcohol, and the like. The main application of unsaturated polyether is to use its unsaturated double bond to react with hydrogen-containing silicone oil to prepare polyether-modified silicone surfactant. [0003] The polyether structures used in the hydrosilylation reaction are different, and polyether-modified silicones with different molecular structures are obtained. At present, allyl polyoxyethylene ether, allyl polyoxyethylene polyoxypropylene atactic polyether and methallyl alcohol po...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/14
CPCC08G65/14
Inventor 张文凯谢卫炜龚国安
Owner SHANGHAI MAIPU NEW MATERIAL TECH CO LTD
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