Flame-retardant polyol containing phosphorus linked pendant groups and preparation method of polyol

A technology of flame-retardant polyols and phosphorus-containing side groups, which is applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., and can solve problems such as easy hydrolysis, material physical and chemical performance degradation, and fracture , to achieve the effect of easy adjustment of performance, easy control of process, and simple and easy control of process

Inactive Publication Date: 2015-11-25
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Although the above several patents have solved the problem of containing halogens, and the disclosed reactive phosphorus-containing flame retardant blocks into the polyurethane structure have improved the flame-retardant performance of polyurethane materials to a certain extent, but because the flame-retardant phosphorus elements are located in In the main chain structure of polyols, phosphate ester flame retardants have the disadvantage of being easily hydrolyzed (M.Sato, J. Appl. Polym. Sci. ,2000,5:1134;S.Lu, Prog. Polym. Sci. ,2002,8:1661), the main chain of polyurethane is broken during the hydrolysis process, which leads to the decline of the physical and chemical properties of the material

Method used

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  • Flame-retardant polyol containing phosphorus linked pendant groups and preparation method of polyol
  • Flame-retardant polyol containing phosphorus linked pendant groups and preparation method of polyol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] (1) Add 200ml of dichloromethane and 104.2g (1.0mol) of neopentyl glycol to a 500ml four-neck flask equipped with a mechanical stirrer, a constant pressure dropping funnel, a thermometer, and a nitrogen condensing reflux tube, stir and dissolve, Add 184.0 g (1.2 mol) of phosphorus oxychloride dropwise through a constant pressure dropping funnel for 2 hours. After the dropwise addition is completed, heat in an oil bath, slowly raise the temperature to 45°C and reflux for 6 hours to obtain a white solid, cool, filter, wash with deionized water, and vacuum-dry at 70°C to obtain a white powder intermediate neopentyl glycol phosphorus oxychloride ;

[0036] (2) Add 50ml of acetonitrile and 55.3g (0.6mol) of glycerol into a 500ml four-neck flask equipped with a mechanical stirrer, a constant pressure dropping funnel, a thermometer, and a condensing reflux tube, stir, dissolve, and add triethylamine 60.7g (0.6mol), 92.2g (0.5mol) intermediate neopentyl glycol phosphorus oxych...

Embodiment 2

[0038] (1) Add 150ml of chloroform and 104.2g (1.0mol) of neopentyl glycol to a 500ml four-neck flask equipped with a mechanical stirrer, a constant pressure dropping funnel, a thermometer, and a nitrogen condensing reflux tube, stir, dissolve, and pass through a constant Add 153.3g (1.0mol) phosphorus oxychloride dropwise to the pressure dropping funnel for 1 hour. After the dropwise addition is completed, heat in an oil bath, slowly raise the temperature to 65°C and reflux for 4 hours to obtain a white solid, cool, filter, wash with deionized water, and vacuum-dry at 80°C to obtain a white powder intermediate neopentyl glycol phosphorus oxychloride ;

[0039] (2) Add 50ml of N,N - dimethylformamide and 67.1g (0.5mol) 1,2,6 - Hexatriol, stir and dissolve, add 59.3g (0.75mol) of pyridine, add 100ml dropwise through the constant pressure dropping funnel N,N - 92.2 g (0.5 mol) of intermediate neopentyl glycol phosphorus oxychloride dissolved in dimethylformamide, added drop...

Embodiment 3

[0041] (1) Add 200ml of chloroform and 104.2g (1.0mol) of neopentyl glycol into a 500ml four-neck flask equipped with a mechanical stirrer, constant pressure dropping funnel, thermometer, and nitrogen condensing reflux tube, stir, dissolve, and Add 168.7g (1.1mol) phosphorus oxychloride dropwise to the pressure dropping funnel, and the dropping time is 1.5h. After the dropwise addition is completed, heat in an oil bath, slowly raise the temperature to 60°C and reflux for 5 hours to obtain a white solid, cool, filter, wash with deionized water, and vacuum-dry at 75°C to obtain a white powdery intermediate neopentyl glycol phosphorus oxychloride ;

[0042] (2) Add 80ml of N,N -Dimethylacetamide and 66.1g (0.55mol) of trimethylolethane, stir and dissolve, add 48.3g (0.66mol) of pyridine, add 100ml dropwise through a constant pressure dropping funnel N,N - 92.2 g (0.5 mol) of intermediate neopentyl glycol phosphorus oxychloride dissolved in dimethylacetamide, added dropwise fo...

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Abstract

The invention discloses a flame-retardant polyol containing phosphorus linked pendant groups and a preparation method of the polyol. The method specifically comprises steps as follows: 1) a solvent and neopentyl glycol are arranged in a reaction kettle, phosphorus oxychloride is dropwise added, and an intermediate, namely, neopentyl glycol phosphorus oxychloride, is prepared; 2) a solvent and micro-molecular trihydric alcohol or tetrahydric alcohol are arranged in the reaction kettle, an acid-binding agent is added, the intermediate dissolved in the solvent is dropwise added, a reflux reaction is performed, and the flame-retardant polyol containing the phosphorus linked pendant groups is obtained through cooling, filtration and washing. The flame-retardant polyol containing the phosphorus linked pendant groups contains no halogen and is environment-friendly and non-toxic, raw materials are cheap and easy to obtain, the technology is simple and controllable, two or three contained activated terminal hydroxyl groups can react with isocyanate, an intrinsically flame-retardant polyurethane material containing the phosphorus linked pendant groups can be prepared, so that defects that additional flame retardants are poor in compatibility in water-based polyurethane systems, migrate and separate out easily and the like are overcome, and the problem of reduction of physical and chemical properties of the material due to breakage of the polyurethane main chain structure due to the fact that phosphate ester bonds of traditional polyols containing phosphorus linked main chains are not resistant to hydrolysis is also solved.

Description

technical field [0001] The invention belongs to the technical field of flame retardant synthesis, and in particular relates to a side-group phosphorus-containing flame-retardant polyol and a preparation method thereof. Background technique [0002] Water-based polyurethane (WPU), as a multi-functional environmental protection material, has been widely used in leather finishing, synthetic leather manufacturing, fabric coating, building materials, adhesives, printing, ink and paper making and other industries. However, the limiting oxygen index (LOI) of water-based polyurethane is only 17%-18%, which is a flammable material and produces a lot of smoke and toxic gases such as HCN and CO when burned, which greatly hinders its further application. At present, the improvement of the flame retardant performance of water-based polyurethane is mainly achieved by adding flame retardants externally, but the externally added flame retardants have defects such as large amount of flame re...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6574C08G18/32C08G101/00
Inventor 范浩军章培昆陈意颜俊田赛琦石碧
Owner SICHUAN UNIV
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