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High activityhydroxyl-terminated polyepichlorohydrin polyatomic alcohol and preparation thereof

A technology of hydroxyl-terminated polyepichlorohydrin ether and epichlorohydrin, which is applied in the field of highly active hydroxyl-terminated polyepichlorohydrin ether polyols and its preparation, can solve the problems of reaction time increase and achieve narrow molecular weight distribution, Effect of color change and high reactivity

Inactive Publication Date: 2009-08-05
QINGDAO UNIV OF SCI & TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When this type of catalyst catalyzes the polymerization of epichlorohydrin, the reaction time is as long as more than 20 hours. If the end-capping treatment is performed, the reaction time will be further increased

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Embodiment 1. A kind of preparation method of highly active hydroxyl-terminated polyepichlorohydrin ether polyol. Add 15g 4,4-dihydroxydiphenylpropane, 0.099g double metal cyanide complex catalyst (DMC) in the pressure-resistant reactor, remove volatile components in vacuum, add 90g epichlorohydrin, and then heat To 128°C, react under nitrogen protection and high-speed stirring; after the reaction is activated, gradually add the remaining 92.4g of epichlorohydrin dropwise. After the polymerization of epichlorohydrin was completed, the temperature in the reactor was lowered to 115° C., and 17.6 g of ethylene oxide was added dropwise to react for capping. After the reaction is completed, the residual monomers are removed in vacuum, and the hydroxyl-terminated polyepichlorohydrin ether polyol with an average relative molecular mass of 3264 and an average hydroxyl functionality of 2 is obtained by refining.

Embodiment 2

[0024]Embodiment 2. A kind of preparation method of highly active hydroxyl-terminated polyepichlorohydrin ether polyol. Add 15g of 4,4-dihydroxydiphenylpropane and 0.132g of DMC into a pressure-resistant reactor, remove the volatile components in vacuum, add 90g of epichlorohydrin, then heat to 128°C, under nitrogen protection and high-speed stirring Reaction under the condition; After the reaction is activated, gradually add the remaining 224g epichlorohydrin dropwise. After the polymerization of epichlorohydrin was completed, the temperature in the reactor was lowered to 115° C., and 17.6 g of ethylene oxide was added dropwise to react for capping. After the reaction is completed, the residual monomer is removed in vacuum, and the hydroxyl-terminated polyepichlorohydrin ether polyol with an average relative molecular weight of 5264 and an average hydroxyl functionality of 2 is obtained by refining.

Embodiment 3

[0025] Embodiment 3. A kind of preparation method of highly active hydroxyl-terminated polyepichlorohydrin ether polyol. Add 15g of 4,4-dihydroxydiphenylpropane and 0.099g of DMC into a pressure-resistant reactor, remove the volatile components in vacuum, add 90g of epichlorohydrin, then heat to 128°C, under nitrogen protection and high-speed stirring Reaction under the conditions; After the reaction is activated, gradually add the remaining 92.4g epichlorohydrin dropwise. After the polymerization of epichlorohydrin is completed, the temperature in the reactor is lowered to 115° C., and 23.2 g of propylene oxide is added dropwise to react for capping. After the reaction is completed, the residual monomer is removed in a vacuum, and the hydroxyl-terminated polyepichlorohydrin ether polyol with an average relative molecular weight of 3348 and an average hydroxyl functionality of 2 is obtained by refining.

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PUM

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Abstract

The invention relates to high activity hydroxy terminated polyepichlorohydrin polylol with simple preparation technology and good color, and the preparation method thereof. The high activity hydroxy terminated polyether has the molecular structure including a large quantity of methylene lateral chloro groups and terminated by epoxy ethane or propylene oxide, and the high activity hydroxy terminated polyepichlorohydrin polylol has the average relative molecular mass of 500-9000 and the average hydroxide radical functionality of 2-3. The preparation method comprises the following steps: low molecular mass initiator and dual-metal prussiate complex compound catalyst are added in a pressure-proof reaction kettle, volatile components are removed in a vacuumed mode, part of epoxy chloropropane are added in the low molecular mass initiator and dual-metal prussiate complex compound catalyst, all the reactants are heated to 100-140 DEG to react under the nitrogen protection and the high-speed stirring, and the rest part of epoxy chloropropane is added gradually drop by drop after the activation; after the polymerization reaction is finished, the temperature is reduced to 90-120 DEG C, propylene oxide or epoxy ethane is added drop by drop for end capping, and residual monomer is removed in a vacuumed way after the reaction, thus the hydroxy terminated polyepichlorohydrin polylol is obtained.

Description

technical field [0001] The invention belongs to the technical field of polymer synthetic material polyether polyol, and in particular relates to a highly active hydroxyl-terminated polyepichlorohydrin ether polyol and a preparation method thereof. Background technique [0002] Polyether polyol is one of the main raw materials for the synthesis of polyurethane materials, and has been widely used in the synthesis of polyurethane rigid foam, polyurethane soft foam, polyurethane elastomer, polyurethane microcellular elastomer, polyurethane coating and polyurethane adhesive. Its excellent mechanical properties and convenient operability make it have a broad development space in modern life. At present, most of the polyether polyols that have been industrialized and widely used are anionically polymerized polypropylene oxide ether, polyethylene oxide ether, propylene oxide and ethylene oxide copolyether, and sealed with ethylene oxide. terminal polypropylene oxide ether. This ty...

Claims

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Application Information

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IPC IPC(8): C08G65/28C08G18/50
Inventor 顾尧孙兆任冯新武吴如舟
Owner QINGDAO UNIV OF SCI & TECH
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