Method for preparing alkyl polyoxyethylene ether acrylate or alkyl polyoxyethylene ether methacrylic ester

A technology of alkyl polyoxyethylene ether methacrylate and alkyl polyoxyethylene ether acrylate, which is applied in the field of preparation of polymerizable surfactants, can solve the problems of troublesome preparation of solid superacid and high cost of use, and achieve equipment Less corrosive, better quality, better yield and better quality

Inactive Publication Date: 2012-08-01
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The solid superacid used in this patent is easy to separate from the product, which improves the quality of the product and can be reused. However, the preparation of the solid superacid is troublesome and the cost of use is relatively high.

Method used

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  • Method for preparing alkyl polyoxyethylene ether acrylate or alkyl polyoxyethylene ether methacrylic ester
  • Method for preparing alkyl polyoxyethylene ether acrylate or alkyl polyoxyethylene ether methacrylic ester
  • Method for preparing alkyl polyoxyethylene ether acrylate or alkyl polyoxyethylene ether methacrylic ester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Preparation of resin solid acid: Add 500 g of water and 5 g of gelatin into a 1 L three-necked flask, start stirring, and raise the temperature to 50° C. to dissolve the gelatin. Then add 100g styrene, 18g divinylbenzene (80wt%), 1.2gBPO and 85g liquid paraffin, heat up to 80°C for 3 hours, then heat up to 95°C for 1 hour, cool to room temperature, filter, wash with water, and dry Then get the white ball. Next, the porogen is extracted with petroleum ether, and cross-linked styrene-divinylbenzene resin white pellets with a diameter of 0.20-1.40 mm are screened out.

[0035] Take 100 g of the cross-linked styrene-divinylbenzene resin white pellets prepared above and put them in a 1L three-necked flask, swell with 100 g of dichloroethane for 2 hours, add 300 g of concentrated sulfuric acid while stirring, and heat up to 90 ° C for 4.5 hours under reflux , then heat up to 110°C to distill ethylene dichloride, then add dropwise 400g of oleum 30% and then insulate at 115°C ...

Embodiment 2

[0043] In a 500ml four-necked flask equipped with a stirrer, a thermometer and a water separator, add 150g of stearyl polyoxyethylene ether and 120g of cyclohexane, heat to dissolve, start stirring, keep the temperature at 80°C, and make the mixture azeotropic. Divide water until the distillate is clear.

[0044] Cool down to 45°C, then add 40g of acrylic acid, 0.2g of polymerization inhibitor hydroquinone, and 50g of resin solid acid catalyst (preparation method is the same as in Example 1) into the four-necked flask, heat, keep the internal temperature at 80°C, and use The reaction process was tested by thin-layer chromatography, and the developer was chloroform:isopropanol=3:1 (volume ratio). When no alkyl polyoxyethylene point was observed on the TLC spot plate, the reaction was terminated.

[0045] After the reaction is completed, cool to room temperature, filter under reduced pressure, and collect and reprocess the resin solid acid for future use. The filtrate was added...

Embodiment 3

[0047] Preparation of resin solid acid: Add 500 g of water and 5 g of gelatin into a 1 L three-necked flask, start stirring, and raise the temperature to 50° C. to dissolve the gelatin. Then add 120g styrene, 14g divinylbenzene (80wt%), 1.4gBPO and 95g liquid paraffin, heat up to 80°C for 3 hours, then heat up to 95°C for 1 hour, cool to room temperature, filter, wash with water, and dry Then get the white ball. Next, the porogen is extracted with petroleum ether, and cross-linked styrene-divinylbenzene resin white pellets with a diameter of 0.20-1.40 mm are screened out.

[0048] The above-mentioned cross-linked styrene-divinylbenzene resin white beads obtained are sulfonated according to the method of example 1, and the performance of the resin acid catalyst obtained at last is: the total exchange capacity of mass is 5.35mmol / g [H + ], with an average pore size of 46nm and an average particle size of 0.8mm, brown spherical polymer particles with sulfonic acid groups.

[00...

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Abstract

The invention discloses a method for preparing alkyl polyoxyethylene ether acrylate or alkyl polyoxyethylene ether methacrylic ester. The method includes dehydrating alkyl polyoxyethylene ether by the aid of entrainer at first, adding inhibitor, resin solid acid catalyst and crylic acid or methacrylic ester, heating while controlling reaction temperature to range from 70 DEG C to 120 DEG C, stirring, realizing reaction and removing water generated in the esterification reaction by the aid of azeotropy; and carrying out filtering, and decompressing and distilling filtrate to obtain a target product. During reaction, resin solid acid is used as the catalyst insoluble in a reaction system, is easy to be removed by means of separating solid from liquid after the reaction is completed, and can be reused, accordingly, cost is lowered, and the quality of the product is improved. In addition, the ecologically environment-friendly alkyl polyoxyethylene ether is selectively used as a raw material, and prepared alkyl polyoxyethylene ether acrylic acid (methacrylic acid) ester non-ionic polymerizable surfactant has a fine application prospect.

Description

technical field [0001] The invention relates to a preparation method of alkyl polyoxyethylene ether acrylate or alkyl polyoxyethylene ether methacrylate, and belongs to the technical field of preparation of polymerizable surfactants. Background technique [0002] Alkyl polyoxyethylene ether acrylates or alkyl polyoxyethylene ether methacrylates are a class of nonionic polymerizable surfactants. Alkyl polyoxyethylene ether type nonionic surfactant is prepared by polymerizing fatty alcohol (lipophilic group) and ethylene oxide (hydrophilic group) with active hydrogen, and can be adjusted by adjusting lipophilic group (fatty alcohol base) and hydrophilic groups (polyoxyethylene groups) to adjust their own hydrophilic-lipophilic balance. Because alkyl polyoxyethylene ether has good emulsification, decontamination, water solubility, salt resistance, acid and alkali resistance and antistatic properties, it can be used as solubilizer, dispersant, antistatic agent and emulsifier, a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/324C07C69/54C07C69/533C07C67/08B01F17/44B01F17/52C09K23/44C09K23/52
Inventor 任碧野蓸贤武冯润强高明
Owner SOUTH CHINA UNIV OF TECH
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