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A kind of unsaturated polyether monomer and its preparation method and application

A polyether monomer, unsaturated technology, applied in the field of polyether, can solve the problem of low polymerization activity of polyether monomer, achieve the effect of improving dispersion performance, simple preparation method, and environmental friendliness

Active Publication Date: 2018-06-05
联泓新材料科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to overcome the defects of low polymerization activity of polyether monomers in the prior art, and provide an unsaturated polyether monomer and its preparation method and application

Method used

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  • A kind of unsaturated polyether monomer and its preparation method and application
  • A kind of unsaturated polyether monomer and its preparation method and application
  • A kind of unsaturated polyether monomer and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] 240 parts of unsaturated polyoxyalkyl ether (methallyl polyoxyethylene ether with a molecular weight of 2400) was vacuum dehydrated at 85° C. for about 1 hour until the water content was as low as 0.3%. Then place it in a three-necked flask equipped with a nitrogen protection device, a thermometer and a stirrer, perform nitrogen replacement, turn on the heating, stir and heat up to 70°C, then slowly add 13.32 parts of m-toluene isocyanate to the flask at a uniform speed, and control the reaction temperature to 70°C. ℃, the dropping time is 20 minutes, after the dropwise addition is completed, keep warm for 2 hours, vacuumize and degas, and discharge the material to obtain the new unsaturated end-capped polyether product.

[0030] NMR nuclear magnetic resonance proton spectrum measures novel unsaturated capped polyether structural formula as shown in formula (3), 1 See attached for HNMR spectrum figure 1 .

[0031]

[0032] According to the hydroxyl value method, th...

Embodiment 2

[0034] 300 parts of unsaturated polyoxyalkyl ether (methallyl polyoxyethylene ether with a molecular weight of 3000) was vacuum dehydrated at 85° C. for about 1 hour until the water content was lower than 0.3%. Then place it in a three-necked flask equipped with a nitrogen protection device, a thermometer and a stirrer, perform nitrogen replacement, turn on the heating, stir and heat up to 70°C, then slowly add 19.97 parts of butyl isocyanate to the flask at a uniform speed, and control the reaction temperature to 70°C. ℃, the dropping time is 40 minutes, after the dropping is completed, keep warm for 2 hours, after vacuuming and degassing, the material is discharged, and the new unsaturated end-capped polyether product is obtained. The structural formula of the novel unsaturated end-capped polyether determined by hydrogen NMR spectroscopy is shown in formula (4).

[0035]

[0036] The end-capping rate calculated by the hydroxyl value method was 91.2%.

Embodiment 3

[0038] 400 parts of unsaturated polyoxyalkyl ether (3-methyl-3-butenyl polyoxypropylene polyoxyethylene ether with a molecular weight of 4000, block, EO / PO mass ratio = 7:1) were vacuum dehydrated at 85°C For about 1 hour, dehydrate until the moisture content is as low as 0.3%. Then place it in a three-necked flask equipped with a nitrogen protection device, a thermometer and a stirrer, perform nitrogen replacement, turn on the heating, stir and raise the temperature to 80°C, then slowly add 39.95 parts of p-toluene isocyanate to the flask at a uniform speed, and control the reaction temperature to 80°C. ℃, the dropping time is 10 minutes, after the dropping is completed, the temperature is kept for 2 hours, and after vacuuming and degassing, the material is discharged to obtain the novel unsaturated end-capped polyether product. The structural formula of the novel unsaturated capped polyether determined by hydrogen nuclear magnetic resonance spectrum is shown in formula (5). ...

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Abstract

The invention relates to a polyether, in particular to an unsaturated polyether monomer. A structural formula (I) of the unsaturated polyether monomer is as shown in the specification, wherein R1s are identical or different and refer to hydrogen atoms or alkyl groups with 1-20 carbon atoms; R2 refers to an alkyl group with 1-20 carbon atoms; R3 refers to a carbonyl group or an alkyl group with 1-10 carbon atoms; X', Y' and Z' refers to H or a structure as shown in the specification and cannot be H at the same time, R4O refers to an oxyalkylene group with 2-18 carbon atoms; p refers to an average addition mole number of the oxyalkylene group and is an integer or a fraction in a range of 1-300; R5 refers to an alkyl group, an alkenyl group, a phenyl group, a substituted phenyl group or an alpha-substituted benzyl group. The unsaturated terminated polyether monomer is high in polymerization activity and stability and can be used for preparation of comb-like branched polymers and polycarboxylate superplasticizer to improve dispersibility of the polycarboxylate superplasticizer.

Description

technical field [0001] The invention relates to a polyether, in particular to a novel urethane-capped unsaturated capped polyether and a preparation method thereof. Background technique [0002] In recent years, the research and production of concrete admixtures have tended to develop in the direction of high performance and pollution-free. Concrete water reducer is the most widely used and most widely used concrete admixture. The polycarboxylate high-efficiency water reducer with comb-shaped molecular structure is suitable for the preparation of high-strength and ultra-high-strength concrete because of its high water-reducing rate, good slump retention performance, low dosage, no pollution, less retarding time, and low cost. , high fluidity and self-compacting concrete has become a hot spot in the research and development of concrete admixtures at home and abroad. Polycarboxylate superplasticizer is a high-performance superplasticizer and a cement dispersant used in cemen...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/333C08F283/06C08F220/06C08F228/02C04B24/16C04B103/30
CPCC04B24/165C04B2103/30C08F283/065C08G65/33351C08G65/33358C08F220/06C08F228/02
Inventor 朱军成牛峰郭晓锋李方
Owner 联泓新材料科技股份有限公司