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Preparation method and application for reaction-type halogen-containing flame-retardant polyether polyol

A flame retardant polyether and polyol technology is applied in the preparation of polyether polyol and the preparation of reactive halogen-containing flame retardant polyether polyol, which can solve the problems of high price, low functionality, high viscosity, etc. The effect of moderate viscosity, good compatibility and excellent mechanical properties

Active Publication Date: 2014-01-08
JIANGSU YOKE TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of this invention is to prepare a new type of reactive halogen-containing flame-retardant polyether polyol, which has solved the common problems of high price, high viscosity and low functionality of current flame-retardant polyether

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] 1. Weigh 261g of dibromoneopentyl glycol and add it to a 1L four-necked flask with mechanical stirring, thermometer, dropping funnel and condenser tube, and simultaneously weigh 460g of epichlorohydrin and add it to the dropping funnel (dibromoneopentyl glycol) The molar ratio of pentylene glycol to epichlorohydrin is 1:4.97), heat the solid material to 120°C until it is completely melted, add 1.1g of oleum, and start adding epichlorohydrin dropwise at 120°C, drop After completion, the insulation was continued for 4 hours to obtain difunctional polyepichlorohydrin with a reaction yield of 99%.

[0028] 2. Cool the product obtained in the first step reaction to 40°C, add 160g of 50wt% sodium hydroxide aqueous solution (the molar ratio of sodium hydroxide to polyepichlorohydrin is 2:1), stir at 50°C for 3 hours, and let it stand Set liquid separation, after separating the dark brown liquid in the lower layer, carry out vacuum distillation at 90 ℃ to remove a small amount ...

Embodiment 2

[0033] 1. Weigh 505g of tetrabromodipentaerythritol and add it to a 1L four-neck flask with a mechanical stirrer, a thermometer, a dropping funnel and a condenser tube, and simultaneously weigh 388g of epichlorohydrin and add it to the dropping funnel (tetrabromodipentaerythritol and The molar ratio of epichlorohydrin is 1:4.2), heat the solid material to 110°C until it is completely melted, add 5g of fuming sulfuric acid, keep 110°C and start adding epichlorohydrin dropwise, and continue to keep warm for 5 Hour, obtain the polyepichlorohydrin of bifunctionality, reaction yield 99%.

[0034] 2. Cool the product obtained in the first step to 40°C, add 80g of 50wt% sodium hydroxide ethanol solution (the molar ratio of sodium hydroxide to polyepichlorohydrin is 1:1), and stir at 60°C for 4 hours Stand for liquid separation, separate the dark brown liquid in the lower layer, carry out vacuum distillation at 90°C to remove a small amount of water, and finally filter to remove resid...

Embodiment 3

[0039]1. Weigh 543g of tetrabromobisphenol A and 162g of epichlorohydrin, and add them to a 2L four-neck flask with mechanical stirring, thermometer, dropping funnel and condenser tube, and weigh 578g of epichlorohydrin to add the dripping solution Funnel (the molar ratio of tetrabromobisphenol A to epichlorohydrin is 1:8), heat the solid material to 120°C until it is completely melted, add 4.3g perchloric acid, keep 120°C and start dripping epoxy chlorine Propane, continue to keep warm for 8 hours after the dropwise addition is completed, to obtain difunctional polyepichlorohydrin, and the reaction yield is 99%.

[0040] 2. Cool the product obtained in the first step reaction to 50°C, add 336g of 50wt% potassium hydroxide aqueous solution (the molar ratio of potassium hydroxide to polyepichlorohydrin is 3:1), stir at 50°C for 3 hours and then statically Set liquid separation, after separating the dark brown liquid in the lower layer, carry out vacuum distillation at 90°C to r...

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PUM

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Abstract

A preparation method for a reaction-type halogen-containing flame-retardant polyether polyol belongs to the field of organic synthesis. The preparation method comprises: initiating a ring-opening polymerization reaction of chloropropylene oxide by a bromine-containing dihydric alcohol / phenol initiator under the effect of a catalyst, to prepare a bifunctionalpolyepichlorohydrin; reacting bifunctionalpolyepichlorohydrin with a strong alkali solution to remove partial chlorine atoms and further to obtain an epoxy-terminated compound; under the effect of an acidic catalyst, in the presence of water and an organic solvent, performing a hydrolysis reaction on the epoxy-terminated compound to obtain a multi-functional halogen-containing flame-retardant polyether polyol solution; performing reduced pressure distillation on the polyether polyol solution to obtain the product halogen-containing flame-retardant polyether polyol. The method has the advantages of cheap and easily available raw materials, a simple and controllable reaction and a yield of 95% or more; the prepared reaction-type halogen-containing flame-retardant polyether polyol is moderate in viscosity, and good in compatibility with foaming agents or other auxiliary agents; a combined material by using the polyether polyol is uniform, transparent, excellent in fluidity and good in stability.

Description

technical field [0001] The present invention relates to a preparation method of polyether polyol which can be used for flame retardancy of polyurethane rigid foam material, more specifically relates to a preparation method and application of reactive halogen-containing flame retardant polyether polyol, which belongs to the field of organic synthesis . technical background [0002] At present, improving the flame retardant performance of polyurethane foam is mainly achieved by adding flame retardants to the foaming formula, and mainstream flame retardants can be divided into two categories: additive flame retardants and reactive flame retardants. Among them, additive flame retardants are mainly compounds containing flame retardant elements such as chlorine, bromine, and phosphorus that do not have active reactive groups; while reactive flame retardants are the main raw materials of polyurethane materials, polyether polyols Or reactive additives prepared by introducing chlori...

Claims

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Application Information

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IPC IPC(8): C08G65/328C08G65/32C08G65/28C07C41/26C07C43/11C07C43/23C08G18/50C08G18/32
Inventor 沈琦曹恒周浩青范金和陈俊
Owner JIANGSU YOKE TECH
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