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One-step preparation method of polyoxyethylene ether acrylate

A polyoxyethylene ether and acrylate technology, which is applied in the preparation of carboxylate, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of difficult product purification, many by-products, complicated processes, etc., and achieves low cost, The effect of short production cycle and simple process

Inactive Publication Date: 2013-06-05
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The above method fails to solve the technical problems of many by-products, difficult product refining, low yield, complex process and high cost

Method used

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  • One-step preparation method of polyoxyethylene ether acrylate

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Clean the autoclave, add 100g of methyl methacrylate, 2.7g of catalyst, 0.9g of cocatalyst and 1.6g of polymerization inhibitor, cover the lid of the kettle, tighten the screws, install the thermocouple thermometer, and check the air tightness of the whole system. The autoclave was purged 3 times with nitrogen. Start slow stirring at 50r / min, fill the autoclave with nitrogen gas to a gauge pressure of 0.1MPa, and then vacuumize, repeating this three times. Turn on medium-speed stirring, and turn on heating. When heated to 20°C, introduce ethylene oxide at a rate of 2.5g / min, control the total reaction pressure of 0.2-0.4MPa, and the temperature in the kettle is 25°C. When 880g of ethylene oxide is added, keep the pressure constant for 1.0h, cool down to 30°C and pump for 10min to discharge.

[0024] The light yellow clear liquid was obtained by filtration, the yield of methyl methacrylate polyoxyethylene ether was 93.1%, the average molecular weight was 940, and the av...

Embodiment 2

[0026] Clean the autoclave, add methyl methacrylate 100g, catalyst 3.8g, cocatalyst 1.3g and polymerization inhibitor 2.3g, cover the kettle lid, tighten the screws, install the thermocouple thermometer, and check the air tightness of the whole system. The autoclave was purged 3 times with nitrogen. Start slow stirring at 50r / min, fill the autoclave with nitrogen gas to a gauge pressure of 0.1MPa, and then vacuumize, repeating this three times. Turn on medium-speed stirring and turn on heating. When heated to 60°C, introduce ethylene oxide at a rate of 1.5g / min, control the total reaction pressure to 0.1-0.4MPa, and the temperature in the kettle to be 65°C. When the feeding of 660g of ethylene oxide is completed, keep the pressure constant for 1.0h, cool down to 30°C and pump for 10min to discharge.

[0027] The light yellow clear liquid was obtained by filtration, and the yield of polyoxyethylene methyl methacrylate was 90.4%, the average molecular weight was 760, and the av...

Embodiment 3

[0029] Clean the autoclave, add 86g of methyl acrylate, 2.6g of catalyst, 0.9g of cocatalyst and 1.6g of polymerization inhibitor, cover the lid of the kettle, tighten the screws, install the thermocouple thermometer, and check the airtightness of the whole system. The autoclave was purged 3 times with nitrogen. Start slow stirring at 150r / min, fill the autoclave with nitrogen gas to a gauge pressure of 0.3MPa, and then vacuumize, repeating this three times. Turn on medium-speed stirring and turn on heating. When heated to 90°C, introduce ethylene oxide at a rate of 2.5g / min, control the total reaction pressure to 0.5-0.7MPa, and the temperature in the kettle to be 95°C. When 440g of ethylene oxide is added, keep the pressure constant for 1.0h, cool down to 30°C and pump for 10min to discharge.

[0030] The light yellow clear liquid was obtained by filtration, and the yield of methyl acrylate polyoxyethylene ether was 92.7%, the average molecular weight was 526, and the avera...

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Abstract

The invention discloses a one-step preparation method of polyoxyethylene ether acrylate. The one-step preparation method comprises the following steps of 1, preparing acrylate and ethylene oxide as raw materials into polyoxyethylene ether acrylate having a polymerization degree of 1 to 25 according to a mole ratio of ethylene oxide to acrylate of (1: 1) to (25: 1), 2, utilizing a B-series main catalyst and a metal salt cocatalyst, 3, protecting allyl double bonds by a polymerization inhibitor in reaction and storage, and 4, carrying out ethoxylation of acrylate at a certain temperature under pressure in a high pressure autoclave to obtain the polyoxyethylene ether acrylate finished product. The one-step preparation method has the advantages of simple processes, less side reaction, high product yield, low cost, narrow polyether product molecular weight distribution and good applicability.

Description

【Technical field】 [0001] The invention relates to the technical field of fine chemicals, in particular to a production method of acrylate polyoxyethylene ether. 【Background technique】 [0002] Acrylate polyoxyethylene ether is a new type of nonionic surfactant, which has a structure of double bond, ester bond and polyether bond. It has good surface activity and can be added with active hydrogen or with unsaturated compounds. Copolymerization endows the product with good lubricating effect, soft effect, good spreadability and stable emulsification. By changing the length of its ethoxy chain, it can be widely used in construction water reducer, polyurethane soft or hard homogeneous Foaming agent, agricultural silicone synergist, low-foaming detergent, lubricating oil, textile and many other fields, the market capacity and potential are very large. [0003] At present, the production of acrylate polyoxyethylene ether adopts an indirect method, that is, polyethylene glycol mono...

Claims

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Application Information

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IPC IPC(8): C08G65/26C07C69/54C07C67/293
Inventor 杨座国钟敏舒建生林真意
Owner EAST CHINA UNIV OF SCI & TECH
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