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Steric hindrance type amino-terminated polyether, preparation method of steric hindrance type amino-terminated polyether and preparation method of slow reaction type polyurea

A technology of amino-terminated polyether and reaction type, which is applied in the field of preparation of slow-reaction polyurea, can solve the problems of single product, restriction of polyurea product promotion and application, and high price, and achieve the effect of high production efficiency

Pending Publication Date: 2022-07-12
山西省建筑科学研究院集团有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] However, currently available steric-hindered low-activity amino-terminated polyether products on the market have disadvantages such as high price and single product, which greatly restrict the promotion and application of polyurea products.

Method used

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  • Steric hindrance type amino-terminated polyether, preparation method of steric hindrance type amino-terminated polyether and preparation method of slow reaction type polyurea
  • Steric hindrance type amino-terminated polyether, preparation method of steric hindrance type amino-terminated polyether and preparation method of slow reaction type polyurea
  • Steric hindrance type amino-terminated polyether, preparation method of steric hindrance type amino-terminated polyether and preparation method of slow reaction type polyurea

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preparation example Construction

[0053] According to another aspect of the present invention, a preparation method of sterically hindered amino-terminated polyether is provided, and the method comprises the following steps:

[0054] a) In the presence of an esterification catalyst, the polyether polyol is reacted with p-nitrobenzoyl chloride or p-nitrophenyl chloroformate to obtain a polyether polyol terminated at both ends by p-nitrobenzoyl chloride Alcohols or polyether polyols terminated at both ends with p-nitrophenyl chloroformate; and

[0055] b) reacting the product of step a) with hydrogen in the presence of a palladium-carbon catalyst to obtain the sterically hindered amino-terminated polyether.

[0056] Preferably, the sterically hindered amino-terminated polyether has a structure represented by the following general formula (1):

[0057]

[0058] Wherein, X is a divalent residue obtained after removing two hydroxyl groups from the polyether polyol; and Y is a direct bond or O.

[0059] Accordi...

Embodiment 1

[0106] 100 g of polytetramethylene ether glycol (PTMG1000 produced by Mitsubishi Chemical Corporation, Japan) having a hydroxyl functionality of 2 and a molecular weight of 1000 was added to a four-necked flask equipped with a stirrer, thermometer, nitrogen inlet and reflux device. , 0.01 g of 4-dimethylaminopyridine (produced by Hubei Wonder Chemical Co., Ltd.) and 37.5 g of p-nitrobenzoyl chloride (produced by Shandong Kaisheng New Materials Co., Ltd.) The reaction was carried out at 110° C. for 5.0 hours until no HCl was detected to obtain polytetramethylene ether terminated with p-nitrobenzoyl chloride at both ends.

[0107] The two ends prepared in the above steps of 100 grams are 10% palladium-carbon catalysts (by Shaanxi Kaida Chemical Co., Ltd.) The company's production) was added into the high pressure reaction kettle and mixed and then fed with hydrogen to a pressure of 3.0MPa, heated to 30°C and reacted for 4.0 hours to obtain a mixture of low-activity amino-termina...

Embodiment 2

[0111] Into a four-necked flask equipped with a stirrer, thermometer, nitrogen inlet and reflux device was added 100 g of polytetramethylene ether glycol (PTMG1000 produced by Mitsubishi Chemical Corporation, Japan) with a hydroxyl functionality of 2 and a molecular weight of 650. , 1 g of triethylamine (produced by Shanghai Aladdin Biochemical Technology Co., Ltd.) and 65.1 g of p-nitrophenyl chloroformate (produced by Xinyi Yongcheng Chemical Co., Ltd.) The reaction was carried out at 90° C. for 4.0 hours until no HCl was detected to obtain polytetramethylene ether end-capped with p-nitrophenyl chloroformate at both ends.

[0112] The two ends prepared in the above steps of 100 grams are 5% palladium-carbon catalysts (by Shaanxi Kaida Chemical Co., Ltd.) Company production) was added to the high pressure reaction kettle and mixed, and then introduced hydrogen to a pressure of 1.0 MPa, heated to 60 ° C and reacted for 8.0 hours to obtain a mixture of low-activity amino-termin...

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Abstract

The invention provides steric hindrance type amino-terminated polyether, a preparation method of the steric hindrance type amino-terminated polyether and a preparation method of slow reaction type polyurea. Specifically, the steric hindrance type amino-terminated polyether has a structure represented by the following general formula (1), in which X is a divalent residue obtained by removing two hydroxyl groups from polyether polyol; and Y is a direct bond or O. The steric hindrance type amino-terminated polyether disclosed by the invention is low in cost, wide in molecular weight range and high in amino conversion rate; a polyurea product obtained by reacting the steric hindrance type amine-terminated polyether with polyisocyanate has relatively long curing time, has excellent physical properties such as tensile strength, elongation at break and tear strength after being cured, and also has excellent weather resistance and aging resistance.

Description

technical field [0001] The invention relates to the field of polyurea coatings, in particular to a sterically hindered low-activity amino-terminated polyether, a preparation method of a sterically hindered low-activity amino-terminated polyether, and a preparation method of a slow-reaction polyurea . Background technique [0002] As the key raw material for the synthesis of polyurea, amino-terminated polyethers (ie, polyethers with both ends capped by amino groups, referred to as ATPE) can be divided into primary amine-type high-activity amino-terminated polyethers and sterically hindered low-activity amino-terminated polyethers according to their activities. polyether. The primary amine type high-activity amino-terminated polyether is a straight-chain primary amine, which has a fast reaction with isocyanate, cures in a few seconds, and concentrates the heat release, resulting in a decrease in the adhesion of the sprayed polyurea product to the substrate. Primary amine typ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/333C08G18/50
CPCC08G65/33389C08G18/5027
Inventor 翟现明张弼伟要如磊桑颖慧赵沛
Owner 山西省建筑科学研究院集团有限公司