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Intumescent polyols as well as preparation method and application thereof

A polyol and expansion technology, which is applied in chemical instruments and methods, compounds of group 5/15 elements of the periodic table, organic chemistry, etc., to achieve high char formation performance, good flame retardancy, and long-term flame retardancy.

Inactive Publication Date: 2015-09-09
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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  • Intumescent polyols as well as preparation method and application thereof
  • Intumescent polyols as well as preparation method and application thereof
  • Intumescent polyols as well as preparation method and application thereof

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 invention relates to the field of flame retardants for rigid polyurethane foams and in particular relates to intumescent polyols as well as a preparation method and application thereof. Compared with the prior art, the invention has the following beneficial effects: (1) the two types of novel intumescent polyols integrate an acid source, a carbon source and a gas source, are very good in thermal stability and higher in carbon forming property, have very high phosphorus and nitrogen contents, and can endow a matrix with good flame retardant property; (2) the two types of novel intumescent polyols contain polyhydroxyl active groups, and can react with a raw material namely isocyanate for preparing polyurethane foams to become a part of macromolecule chains of the polyurethane foams, so that the problem that a common flame retardant causes damages to the mechanical properties of a material due to poor compatibility with the matrix can be solved, and the matrix material can keep the flame retardant property for a long time; and (3) the intumescent polyols provided by the invention are simple in preparation process, mild in reaction condition and 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 Applications(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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