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Preparation method for polyethylene glycol mono alkyl ether unsaturated carboxylic ester

A polyethylene glycol monoalkyl ether, unsaturated technology, applied in the field of preparation of polyethylene glycol monoalkyl ether unsaturated carboxylate, can solve the problem of short one-step process route, long two-step process route, Reduce the one-step reaction temperature and other problems to achieve the effect of simplifying the process

Active Publication Date: 2015-06-17
SHANGHAI DUOLUN CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The present invention aims to solve the technical problem of the long two-step route process existing in the prior art, and provides a new preparation method of polyethylene glycol monoalkyl ether unsaturated carboxylate, which has a one-step process route The advantage of being short, and can reduce the reaction temperature of the existing one-step method at the same time

Method used

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  • Preparation method for polyethylene glycol mono alkyl ether unsaturated carboxylic ester
  • Preparation method for polyethylene glycol mono alkyl ether unsaturated carboxylic ester
  • Preparation method for polyethylene glycol mono alkyl ether unsaturated carboxylic ester

Examples

Experimental program
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Effect test

Embodiment 1

[0022] Put 200g of methyl acrylate and 0.8wt% of the catalyst relative to the total weight of methyl acrylate and ethylene oxide into the dry reactor with stirring, electric heating jacket and internal water-cooled coil, relative to methyl acrylate and A polymerization inhibitor with a total weight of 0.5 wt% of ethylene oxide is added, and the reaction kettle is sealed. The autoclave was purged with nitrogen and then evacuated, and this was repeated three times. Turn on the stirring, heat to 80°C and maintain this temperature, slowly pass in 23.23 moles of ethylene oxide (that is, the molar ratio of methyl acrylate to EO is 1:10), and maintain by controlling the feeding rate of ethylene oxide The reaction pressure was 0.9 MPa, and it took 6 hours to pass the above amount of ethylene oxide (that is, the reaction time was 6 hours). Maturation at the reaction temperature for 1 hour, and then cooling to 60° C. and vacuum treatment under a pressure of -0.07 MPa for 10 minutes, sto...

Embodiment 2

[0024] [Example 2] to [Example 9] and [Comparative Example 1] and [Comparative Example 2]

[0025] In addition to the type of unsaturated carboxylic acid ester shown in formula (I), the composition of the catalyst, the amount of the catalyst, the composition of the polymerization inhibitor, the amount of the polymerization inhibitor, the reaction temperature, the reaction pressure, the number of moles of EO (or the formula ( I) The molar ratio of unsaturated carboxylic acid ester to EO is shown) and the reaction time is changed. Other operating conditions are the same as in Example 1.

[0026] In order to facilitate comparison, the important preparation conditions are listed in Table 1, and the product yield, number average molecular weight Mn, dispersion coefficient PD and iodine value are listed in Table 2.

[0027] It can be seen from the comparison of Comparative Example 1 and Comparative Example 2 with Example 1 that SnCl 2 Or BF 3 The reaction time of single-component catalyst ...

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Abstract

The present invention relates to a preparation method for polyethylene glycol mono alkyl ether unsaturated carboxylic ester, wherein a purpose of the present invention is to mainly solve the technical problem of long process route of the existing two-step method in the prior art. A technical scheme of the preparation method is that: in the presence of a catalyst, a polymerization inhibitor and an unsaturated carboxylic ester represented by a formula (I), ethylene oxide is added, and a reaction is performed at a reaction temperature of 30-185 DEG C under reaction pressure of -0.01 to 1.9 MPa to obtain the polyethylene glycol mono alkyl ether unsaturated carboxylic ester, wherein the catalyst is SnCl2 and BF3, a weight ratio of SnCl2 to BF3 is 1:0.5-20, the polymerization inhibitor is hydroquinone and / or 4-methoxyphenol, R1 is hydrogen atom or methyl, and R2 is C1-C8 alkyl. With the technical scheme, the technical problem is solved well. The preparation method can be applicable for polyethylene glycol mono alkyl ether unsaturated carboxylic ester production.

Description

Technical field [0001] The invention relates to a preparation method of polyethylene glycol monoalkyl ether unsaturated carboxylic acid ester. Background technique [0002] Polyethylene glycol monoalkyl ether unsaturated carboxylic acid ester is a new type of non-ionic surfactant. It has double bond, carbonyl group and ether bond structure. It has surface activity and can be added with active hydrogen. It can be adjusted Adjust the length of the ethoxy chain and adjust the molecular weight to obtain products with different properties. It is widely used in many fields such as water reducing agent, foam leveling agent, organic silicon synergist, textile, etc., with great market capacity and potential. Give the product good lubricating effect, soft effect, good spreadability and stable emulsification. [0003] In the prior art, the synthesis method of polyethylene glycol monoalkyl ether unsaturated carboxylic acid ester mainly adopts a two-step method, namely an esterification metho...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/26C07C67/31C07C69/734
Inventor 杨座国林真意朱学文舒建生张江锋
Owner SHANGHAI DUOLUN CHEM