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Preparation method and application of brominated flame-retardant polyether glycol

A flame retardant polyether and polyol technology, applied in the field of organic synthesis, can solve the problems of high price, high viscosity and low functionality of flame retardant polyether, and achieve the effects of good compatibility, moderate viscosity and good stability

Inactive Publication Date: 2015-12-02
JIANGYIN POLYTECHNIC COLLEGE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The technical problem to be solved by the present invention is to provide a preparation method of brominated flame-retardant polyether polyols in view of the above-mentioned prior art, so as to solve the common problems of high price, high viscosity and low functionality of current flame-retardant polyethers. question

Method used

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  • Preparation method and application of brominated flame-retardant polyether glycol

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] 1. Weigh 104g of neopentyl glycol and add it to a 1L four-necked flask equipped with a mechanical stirrer, thermometer, dropping funnel and condenser. At the same time, weigh 462g of epichlorohydrin and add it to the dropping funnel to heat the solid material to 120 O C After it is completely melted, add 0.09g of fuming sulfuric acid to keep 110 O C started to add epichlorohydrin dropwise, and continued to keep warm for 4 hours after the dropwise addition to obtain difunctional polyepichlorohydrin, with a reaction yield of 99%.

[0035] 2. Cool the product obtained in the first step to -20°C O C, and then keep the stream temperature at -20 O Under the condition of C, 320 g of liquid bromine was added dropwise, and the dropwise addition time was 7 hours. After the dropwise addition, the unreacted liquid bromine was distilled off under reduced pressure at room temperature, and the reaction yield was 98%.

[0036] 3. Heat the product obtained in the second step reaction...

Embodiment 2

[0040] 1. Weigh 90g of 1,4-butanediol and add it into a 1L four-necked flask equipped with a mechanical stirrer, thermometer, dropping funnel and condenser tube. At the same time, weigh 555g of epichlorohydrin and add it to the dropping funnel. Heat the material to 120 O C After it is completely melted, add 0.1g of fuming sulfuric acid, keep 120 O C began to drop epichlorohydrin, and after the dropwise addition was completed, the temperature was continued for 6 hours to obtain difunctional polyepichlorohydrin, and the reaction yield was 99%.

[0041] 2. Cool the product obtained in the first step to 0 O C, and then keep the stream temperature at 0 O Under the condition of C, 480 g of liquid bromine was added dropwise for 9 hours. After the dropwise addition, unreacted liquid bromine was distilled off under reduced pressure at room temperature, and the reaction yield was 98%.

[0042] 3. Heat the product obtained in the second step reaction to 60 O C, add 50wt% sodium hydro...

Embodiment 3

[0046] 1. Weigh 228g of bisphenol A and 162g of epichlorohydrin, and add them into a 2L four-necked flask equipped with a mechanical stirrer, a thermometer, a dropping funnel and a condenser tube, and simultaneously weigh 763g of epichlorohydrin into the dropping funnel. Solid material heated to 60 O C After it is completely melted, add 1.1g perchloric acid, keep 60 O C began to drop epichlorohydrin, and after the dropwise addition was completed, the temperature was continued for 10 hours to obtain difunctional polyepichlorohydrin, and the reaction yield was 99%.

[0047] 2. Cool the product obtained in the first step reaction to 20 O C, then keep the stream temperature at 20 O Under the condition of C, 160 g of liquid bromine was added dropwise for 3 hours. After the dropwise addition, unreacted liquid bromine was distilled off under reduced pressure at room temperature, and the reaction yield was 98%.

[0048] 3. Cool the product obtained in the second step reaction to 0 ...

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Abstract

The invention discloses a preparation method and application of brominated flame-retardant polyether glycol. The method mainly comprises the following steps: ring-opening polymerization reaction of dibasic alcohol / phenolic compound and epoxy chloropropane, bromination reaction, cyclization dechlorination reaction, and ring-opening hydrolysis reaction. The brominated flame-retardant polyether glycol can be used for preparing a polyurethane rigid foam material with the flame-retardant grade of B1 when being combined with an additive phosphorus flame retardant, and endows the polyurethane rigid foam material with excellent mechanical properties on the premise of enhancing the flame retardancy of the polyurethane rigid foam.

Description

technical field [0001] The invention relates to a preparation method of a brominated polyether polyol which can be used for flame retardancy of rigid polyurethane foam materials, and more particularly relates to a preparation method and application of a brominated flame-retardant polyether polyol. It belongs to the field of organic synthesis. Background technique [0002] Rigid polyurethane foam has excellent thermal insulation properties, light weight, good dimensional stability, and easy molding. It is usually used as thermal insulation materials in building insulation, refrigeration, transportation, and chemical industries. However, its flammability is the biggest problem limiting the application range of rigid polyurethane foam. At present, the main way to solve this problem is to add flame retardants in the material preparation process. Flame retardants suitable for rigid polyurethane foam can be divided into two categories: additive type and reactive type. Among the...

Claims

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Application Information

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IPC IPC(8): C08G65/28C08G18/48C08G101/00
Inventor 徐娜陆敏
Owner JIANGYIN POLYTECHNIC COLLEGE
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