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Preparation method for polyethylene glycol mono alkyl ether unsaturated carboxylic ester

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

Active Publication Date: 2013-02-13
SHANGHAI DUOLUN CHEM
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  • Abstract
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  • Claims
  • Application Information

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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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Embodiment 1

[0022] Add 200g of methyl acrylate and the catalyst of 0.8wt% relative to methyl acrylate and drop into ethylene oxide gross weight in the dry reactor with stirring, electric heating jacket and internal water-cooled coil, relative to methyl acrylate and Add 0.5 wt% polymerization inhibitor of ethylene oxide gross weight, and seal the reaction kettle. The autoclave was purged with nitrogen and then evacuated three times. Start stirring, and 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 the temperature by controlling the feed rate of ethylene oxide. The reaction pressure was 0.9 MPa, and it took 6 hours to feed the above-mentioned amount of ethylene oxide (ie, the reaction time was 6 hours). Aging at the reaction temperature for 1 hour, then cooling to 60° C. and vacuum treatment for 10 minutes under a pressure of -0.07 MPa, stopping stirring, and opening the rea...

Embodiment 2

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

[0025] Except the unsaturated carboxylate kind shown in formula (I), the composition of catalyzer, the consumption of catalyzer, the composition of polymerization inhibitor, polymerization inhibitor consumption, temperature of reaction, reaction pressure, pass into EO mole number (or in formula ( 1) Shown unsaturated carboxylic acid ester and EO feed molar ratio meter) and reaction time have change, other operating conditions are all identical with embodiment 1.

[0026] Important preparation conditions are listed in Table 1 for ease of comparison, and the yield of product, number average molecular weight Mn, dispersion coefficient PD and iodine value are listed in Table 2.

[0027] From Comparative Example 1 and Comparative Example 2 compared with Example 1, it can be seen that the use of SnCl 2 or BF 3 The reaction time of the single-component catalyst is significantly longer than t...

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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 carboxylate is a new type of nonionic surfactant, which has double bond, carbonyl and ether bond structure, has surface activity, and can add active hydrogen, which can be adjusted The length of the ethoxy chain is adjusted to adjust the molecular weight to obtain products with different properties. It is widely used in many fields such as water reducer, foam stabilizer, silicone synergist, textile, etc., and has a large market capacity and potential. Give the product good lubricating effect, softening 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 two-step method, namely esterification method or transesterification ...

Claims

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Application Information

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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
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