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Preparation method and application of flame-retardant polyether polyol

A flame-retardant polyether and polyol technology, applied in polyurea/polyurethane adhesives, adhesive types, adhesives, etc., can solve problems such as unsatisfactory flame-retardant properties, and achieve good flame-retardant effects, excellent Flame retardancy, the effect of reducing the viscosity of the system

Active Publication Date: 2022-01-28
江苏钟山新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to its excellent performance, polyurethane materials are widely used in clothing, shoes and hats, building exterior walls, pipes, aerospace, furniture, automobiles, medical care and other fields, but the flame retardancy of existing polyurethane materials is not satisfactory

Method used

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  • Preparation method and application of flame-retardant polyether polyol
  • Preparation method and application of flame-retardant polyether polyol
  • Preparation method and application of flame-retardant polyether polyol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Prepare allyl methylphosphoramidate dimethyl ester by Atherton-Todd reaction as follows: put 1 mol dimethyl phosphite, 1.1 mol carbon tetrachloride and 6 mol anhydrous tetrahydrofuran into the reaction kettle under nitrogen atmosphere at 5°C After starting the stirring, add dropwise a mixture of 1.05mol N-allylmethylamine, 1.1mol triethylamine and 3mol anhydrous tetrahydrofuran, and drop it over 2 hours; React for 10 hours; finally filter and distill under reduced pressure to obtain allyl methylphosphoramidate dimethyl.

[0033] Prepare 1-methylphosphoramidate-2,3-epoxypropane by in-situ epoxidation as follows: put 0.9 mol of allylmethylphosphoramidate into the reaction kettle at 40 °C, Add 0.8mol formic acid, raise the temperature to 50°C, add dropwise 0.9mol hydrogen peroxide (provided in the form of an aqueous hydrogen peroxide solution with a concentration of 30% by mass) at 50°C. The reaction was continued for 6 hours under stirring; finally, after washing with wa...

Embodiment 2

[0036] According to the method in Example 1, 1-dimethylphosphoramidate-2,3-epoxypropylene was prepared.

[0037] Prepare flame-retardant polyether polyol B by coordination polymerization as follows: 100g of polyether polyol N-306 (glycerol polyoxypropylene ether, molecular weight 600, purchased from Jiangsu Zhongshan Chemical Co., Ltd. ) and 100ppm DMC catalyst, start stirring, nitrogen replacement 3 times, vacuumize to -0.1MPa, and heat up to 150°C while vacuuming; , close the vacuum valve and stop heating, pass into the mixture of 30g propylene oxide and 1-methylphosphoramidate-2,3-propylene oxide (propylene oxide and 1-methylphosphoramidate-2,3 -The mass ratio of propylene oxide is 5:3), after pressure drop, temperature rise, continue to pass into the mixture of 370g propylene oxide and 1-methylaminophosphoric acid dimethyl ester-2,3-propylene oxide (ring The mass ratio of oxypropane to 1-methylphosphoramidate-2,3-propylene oxide is 5:3), during the continuous feeding proc...

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Abstract

The invention provides a preparation method and application of flame-retardant polyether polyol, and belongs to the field of organic synthesis. The preparation method comprises the following steps: adding a mixture of phosphite ester, carbon tetrachloride and anhydrous tetrahydrofuran in a nitrogen atmosphere at 0-5 DEG C, dropwise adding a mixture of N-allylmethylamine, triethylamine and anhydrous tetrahydrofuran, and conducting reacting at 15-30 DEG C for 6-12 hours to obtain allylmethylamino phosphate; adding allylmethylamino phosphate at 35-45 DEG C, adding formic acid, dropwise adding hydrogen peroxide at 45-55 DEG C, and continuously conducting reacting at 45-55 DEG C for 4-6 hours; and carrying out coordination polymerization reaction on low-molecular polyol, 1-methylamino phosphate-2,3-epoxypropane and epoxypropane at the temperature of 145-155 DEG C, so as to obtain the flame-retardant polyether polyol. The flame-retardant polyether polyol disclosed by the invention can be used for preparing a polyurethane adhesive and polyurethane foam with good flame retardance.

Description

technical field [0001] The invention belongs to the field of organic synthesis, and in particular relates to a preparation method and application of a flame-retardant polyether polyol. Background technique [0002] Polyurethane materials have the characteristics of strong wear resistance, excellent shock absorption performance, and excellent machining performance, and through the selection of main raw materials and optimized design of formula, polyurethane products with various properties can be prepared. Due to its excellent performance, polyurethane materials are widely used in clothing, shoes and hats, building exterior walls, pipes, aerospace, furniture, automobiles, medical care and other fields, but the flame retardancy of existing polyurethane materials is not satisfactory. Contents of the invention [0003] The object of the present invention is to provide a preparation method of flame-retardant polyether polyol, and the obtained flame-retardant polyether polyol ca...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/28C08G18/50C09J175/08C08G101/00
CPCC08G65/2639C08G65/2663C08G65/2696C08G18/509C09J175/08C08G2101/00
Inventor 陆逸峰宗红亮刘荣张丽君李月文吴亚清俞绿绿
Owner 江苏钟山新材料有限公司