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Expanded polyol and its preparation method and application

A polyol, expansion type technology, applied in chemical instruments and methods, compounds of group 5/15 elements of the periodic table, organic chemistry, etc., to achieve the effects of mild reaction conditions, good thermal stability, and good flame retardancy

Inactive Publication Date: 2017-06-16
ZHONGBEI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But even in the improved process, the preparation of the flame retardant requires relatively complicated steps such as dehydration, Lewis acid catalyst, etc.

Method used

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  • Expanded polyol and its preparation method and application
  • Expanded polyol and its preparation method and application
  • Expanded polyol and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] The preparation method of the expanded polyol DOP-DEA:

[0030] (1) In a 250mL reaction vessel equipped with a stirring and cooling device, add 18.40g of 2,2-dimethyl-1,3-propanediol-phosphonyl chloride (0.1mol) and 50mL of tetrahydrofuran, start stirring to dissolve evenly; Diethanolamine (0.1 mol, 10.51 g), triethylamine (0.3 mol, 30.36 g) and 100 mL of tetrahydrofuran solution were slowly added dropwise while stirring at -10°C, and a white precipitate gradually formed in the system.

[0031] (2) After the dropwise addition of the solution, the system was reacted at 0-10°C for 10 hours, then heated to 20°C for 12 hours, the white precipitate triethylamine hydrochloride was filtered, concentrated under reduced pressure, purified and dried to obtain light Yellow transparent oily liquid product with a yield of 98.5%.

Embodiment 2

[0033] The preparation method of the expanded polyol DOP-DEA:

[0034] (1) In a 250mL reaction vessel equipped with a stirring and cooling device, add 18.40g of 2,2-dimethyl-1,3-propanediol-phosphonyl chloride (0.1mol) and 50mL of tetrahydrofuran, and start stirring to dissolve evenly. Diethanolamine (0.1 mol, 10.51 g), pyridine (0.2 mol, 15.82 g) and 100 mL of tetrahydrofuran solution were slowly added dropwise while stirring at 0-10°C, and a white precipitate gradually formed in the system.

[0035] (2) After the solution is added dropwise, let the system react at 0-10°C for 8 hours, then raise the temperature to 20°C and react for 8 hours, filter the white precipitate pyridine hydrochloride, concentrate under reduced pressure, purify and dry to obtain light yellow transparent Oily liquid product, yield 90.6%.

Embodiment 3

[0037] The preparation method of the expanded polyol DOP-DEA:

[0038](1) In a 250mL reaction vessel equipped with a stirring and cooling device, add 18.40g of 2,2-dimethyl-1,3-propanediol-phosphonyl chloride (0.1mol) and 50mL of dichloromethane, and start stirring to dissolve evenly. Diethanolamine (0.1 mol, 10.51 g), triethylenediamine (0.1 mol, 11.20 g) and 100 mL of dichloromethane solution were slowly added dropwise while stirring at 0-10°C, and a white precipitate gradually formed in the system.

[0039] (2) After the solution was added dropwise, the system was reacted at 0-10°C for 10 hours, then heated to 20°C for 12 hours, the white precipitate was filtered, concentrated under reduced pressure, purified and dried to obtain a light yellow transparent oily liquid product, The yield was 93.8%.

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Abstract

The present invention relates to the field of flame retardants for rigid polyurethane foams, in particular to an intumescent polyol and its preparation method and application. Compared with the prior art, it has the following beneficial effects: (1) two novel intumescent Type polyol, which integrates acid source, carbon source and gas source, has good thermal stability and higher char-forming performance, and has high phosphorus and nitrogen content, which can endow the matrix with good flame retardant performance; (2) Two kinds of expansion type polyols described in the present invention contain polyhydric active group, can react with the raw material isocyanate of polyurethane foam, become a part in the macromolecular chain of polyurethane foam, not only can solve general flame retardant because of The problem of poor matrix compatibility and damage to the mechanical properties of the material, and the long-term maintenance of flame retardancy of the matrix material; (3) the expansion polyol of the present invention has a simple preparation process and mild reaction conditions, and is suitable for industrial production.

Description

technical field [0001] The invention relates to the field of flame retardants for rigid polyurethane foams, in particular to an expansion polyol and its preparation method and application. Background technique [0002] Rigid polyurethane foam, due to its excellent thermal insulation performance, good mechanical properties and simple molding process, is more and more widely used; but at the same time, its fatal disadvantage of flammability limits its application range. At present, strict flame retardant grade requirements are put forward for the use of polyurethane foam materials both at home and abroad. [0003] Intumescent flame retardants are currently a research hotspot in the field of flame retardants, and they are widely used in polyolefin substrates. In recent years, people have also begun to pay attention to the research on the flame retardant effect of intumescent flame retardants on polyurethane foam. Intumescent flame retardants are flame retardants containing ac...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/6574C08G18/66C08G18/32
Inventor 赵斌刘亚青李飞熊宽宽王晓峰柳学义
Owner ZHONGBEI UNIV
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