Preparation method and application of phosphorus-halide-cooperation inflaming retarding polyether polyol

A technology of flame retardant polyether and phosphorus halogen synergy

Active Publication Date: 2012-08-15
WANHUA CHEM NINGBO RONGWEI POLYURETHANE
View PDF5 Cites 4 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] In the preparation method disclosed in this patent, the post-treatment process is complicated, and the yield of the product is low, only 68.5%, which is not conducive to industrial production
At the same time, in the preparation process, the aqueous solution of sodium hydroxide is added dropwise to the aqueous solution of bisphenol compounds and chlorinated glycerin, because sodium hydroxide can not only react with bisphenol A compounds to generate sodium phenate, sodium phenate can be combined with 1-chloroglycerin The reaction generates the target product; and sodium hydroxide can also react with 1-chloroglycerol to generate glycerol or glycidol, which consumes the reaction raw materials, will directly affect the preparation of the target product, reduce the yield of the product, and increase the difficulty of product purification and waste water. processing fee

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Preparation method and application of phosphorus-halide-cooperation inflaming retarding polyether polyol
  • Preparation method and application of phosphorus-halide-cooperation inflaming retarding polyether polyol
  • Preparation method and application of phosphorus-halide-cooperation inflaming retarding polyether polyol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] 1. Weigh 92.5g of epichlorohydrin into a 500mL three-necked flask with a magnetic stirrer, a constant pressure dropping funnel and a thermometer, weigh 0.23g of concentrated sulfuric acid and dissolve it in 144g of water and transfer it to a constant pressure dropping funnel , the inner air of the flask was replaced with nitrogen three times at room temperature, then the temperature was raised to 80° C., and the water containing sulfuric acid was started to be added dropwise.

[0055] 2. Cool down the reaction solution obtained in step 1 to 55-65°C, first use a water pump to remove the water in the system by vacuum distillation under the condition that the vacuum degree is not less than 0.095Mpa, and gradually raise the temperature to 100°C to ensure that the system The water in it is completely removed. Then use an oil pump to further distill under reduced pressure, and heat up to 160 ° C. The collected fraction is the target product 3-chloro-1,2-propanediol (intermedi...

Embodiment 2

[0059] 1. Weigh 92.5g of epichlorohydrin and add it to a 500mL three-neck flask with a magnetic stirrer, constant pressure dropping funnel and thermometer, add 0.9g of ion resin, weigh 180g of water in the constant pressure dropping funnel, and Replace the internal air with nitrogen three times at room temperature, then raise the temperature to 60°C, start to add sulfuric acid water dropwise, and continue to insulate and reflux for 5 hours after the dropwise addition is completed;

[0060] 2. Cool down the reaction solution obtained in step 1 to 55-65°C, first use a water pump to remove the water in the system by vacuum distillation under the condition that the vacuum degree is not less than 0.095Mpa, and gradually raise the temperature to 100°C to ensure that the system The water in it is completely removed. Then use an oil pump to further distill under reduced pressure, and heat up to 160°C. The collected fraction is the target product 3-chloro-1,2-propanediol (intermediate ...

Embodiment 3

[0064] 1. Weigh 92.5g of epichlorohydrin into a 500mL three-neck flask with a magnetic stirrer, constant pressure dropping funnel and thermometer, add 1.8g of aluminum trichloride, weigh 90g of water in the constant pressure dropping funnel , the internal air of the flask was replaced with nitrogen three times at room temperature, then the temperature was raised to 100°C, and water containing sulfuric acid was started to be added dropwise.

[0065] 2. Cool down the reaction solution obtained in step 1 to 55-65°C, first use a water pump to remove the water in the system by vacuum distillation under the condition that the vacuum degree is not less than 0.095Mpa, and gradually raise the temperature to 100°C to ensure that the system The water in it is completely removed. Then use an oil pump to further distill under reduced pressure, and heat up to 160°C. The collected fraction is the target product 3-chloro-1,2-propanediol (intermediate CPG), which is a colorless viscous liquid ...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

PropertyMeasurementUnit
oxygen indexaaaaaaaaaa
Login to view more

Abstract

The invention provides a preparation method and an application of phosphorus-halide-cooperation inflaming retarding polyether polyol. The preparation method of the polyol mainly comprises the following steps of: performing hydrolysis on epoxy chloropropane to generate 3-chloro-1,2-propanediol; reacting a halide aromatic diphenol compound with alkalis hydroxide with phosphorus flame retardant serving as a dissolvent, and then reacting the halide aromatic diphenol compound with the 3-chloro-1,2-propanediol under the action of a catalyst; and performing reduced pressure distillation and filtration on a reaction liquid to obtain a light yellow liquid, wherein the contained halide component is halide aromatic diphenol diglycerol ether, the contained phosphorus component is the phosphorus flame retardant, and the total recovery of products is more than 90%. A polyurethane material prepared with the novel phosphorus-halide-cooperation inflaming retarding polyether polyol being inflaming retarding polyol has excellent thermal stability and flame retardance and good mechanical properties.

Description

technical field [0001] The invention relates to a preparation method of a polyether polyol which can be used for flame retardancy of polyurethane materials, and more specifically relates to a preparation method and application of a phosphorus-halogen synergistic flame-retardant polyether polyol, which belongs to the field of organic synthesis. Background technique [0002] With the continuous deepening of the country's promotion of energy conservation and environmental protection and the implementation of building energy conservation regulations, there will be a broad market for building energy conservation and thermal insulation materials in the future. At present, the main building energy-saving insulation materials on the market include extruded polystyrene (XPS), foam board (EPS), sprayed polystyrene (SPS), polyurethane foam (PUR) and other insulation materials. Due to the excellent heat insulation and sound insulation performance of polyurethane foam itself, as well as ...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
Patent Type & Authority Applications(China)
IPC IPC(8): C08G18/32C08K5/521C08K5/523C08K5/5333C08L75/04C07C43/225C07C41/16C07C31/42C07C29/10
Inventor 鞠昌迅陈海波郭克银刘运海隋宝华李晶华卫琦
Owner WANHUA CHEM NINGBO RONGWEI POLYURETHANE
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap