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Preparation method and application of low-ployphosphate ester polyhydric alcohol

A technology of oligomeric phosphate ester and polyol, which is applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc. The problems such as increase and large activity can achieve the effect of simple process, easy industrial production and mild reaction.

Inactive Publication Date: 2015-12-23
UNIV OF JINAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The patent application number is CN201010227072.1, which discloses a preparation method of oligomeric phosphate polyols, which is to dilute phosphorus oxychloride with a solvent, add monohydric alcohol, and reflux until no hydrogen chloride gas escapes to obtain dichlorophosphoric acid Mono-alkane ester reaction solution; continue to add acid-binding agent triethylamine, catalyst and glycol until no hydrogen chloride gas escapes to obtain a mixture of oligophosphate alcohols; filter the mixture, and heat and distill the filtrate to obtain oligophosphate polyols; although this method produces a reactive additive flame retardant, it also uses phosphorus oxychloride as a reactant, which not only has high activity and requires high operating technology, but also produces a large amount of hydrogen chloride gas. The increase in the post-treatment process will inevitably bring Substantial increase in manpower, equipment and other costs

Method used

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Embodiment 1 A kind of preparation method of oligomeric phosphate ester polyol

[0039] 1) Add 15g of phosphorus pentoxide to the reaction kettle, start stirring, add 3.0g of water in 5min, heat to 50-80℃ for 40-60min; add 70g of propylene oxide in 5-10min, and then Add 0.45g of catalyst and heat to 130°C for 3h to prepare phosphate-based polyol;

[0040] 2) Cool to 50-80°C, add 20g of phosphorus pentoxide, and react for 20min to dissolve completely;

[0041] 3) Add 100g of ethylene oxide, add 1.3g of catalyst tetraethylammonium bromide, raise the temperature to 115-125°C, react for 3h, cool, and discharge to prepare oligomeric phosphate polyol; Phosphate polyol is a light yellow transparent liquid with an acid value of 18mgKOH / g and a viscosity of 7053mPa.s.

Embodiment 2

[0042] Embodiment 2 A kind of preparation method of oligomeric phosphate ester polyol

[0043] 1) Add 15g of phosphorus pentoxide to the reaction kettle, start stirring, add 4.0g of water in 5-10min, heat to 50-80℃ for 50min; add 90g of epichlorohydrin in 7min, then add 0.35 g catalyst, heated to 135 ° C for 3 hours to prepare phosphate-based polyols;

[0044] 2) Cool to 50-80°C, add 25g of phosphorus pentoxide, and react for 40min to dissolve completely;

[0045] 3) Add 120 g parts by mass of propylene oxide, add 1.0 g of catalyst benzyltriethylammonium chloride, raise the temperature to 120°C, react for 3 hours, cool, and discharge to prepare oligomeric phosphate polyol; Polyphosphate polyol is a light yellow transparent liquid with an acid value of 16.4mgKOH / g and a viscosity of 7840mPa.s.

Embodiment 3

[0046] Embodiment 3 A kind of preparation method of oligomeric phosphate ester polyol

[0047] 1) Add 15g of phosphorus pentoxide to the reaction kettle, start stirring, add 4.0g of water in 5-10min, heat to 50-80℃ for 60min; add 110g of epichlorohydrin in 6min, then add 0.25 g catalyst, heated to 140 ° C for 3 hours to prepare phosphate-based polyols;

[0048] 2) Cool to 50-80°C, add 20-30 parts by mass of phosphorus pentoxide, and react for 20-60 minutes to completely dissolve;

[0049] 3) Add 140g of epichlorohydrin, add 0.8g of catalyst benzyltrimethylammonium chloride, raise the temperature to 125°C, react for 3h, cool, and discharge to obtain oligomeric phosphate polyol; the oligomeric Phosphate polyol is a light yellow transparent liquid with an acid value of 10.8mgKOH / g and a viscosity of 8206mPa.s.

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Abstract

The invention discloses a preparation method and application of low-ployphosphate ester polyhydric alcohol, which belong to the technical field of high polymer materials, reactive flame retardants, energy conservation and protection, environmentally friendly new processes and building insulation materials. The low-ployphosphate ester polyhydric alcohol is prepared through catalytic reaction by adopting phosphorus pentoxide, water and alkylene oxide as raw materials. According to the preparation method, the raw materials are low in cost and easy to get, the reaction is mild, the process is simple and easy to operate, and the preparation method is easy for industrial production; the target product is used for preparing flame retardant polyurethane foam materials.

Description

technical field [0001] The present invention relates to a preparation method and application of oligomeric phosphate polyols, in particular to a method for preparing oligomeric phosphate polyols used to prepare flame-retardant polyurethane foams, belonging to polymer materials and reactive flame retardants , Energy conservation and protection, environmentally friendly new technology and building insulation materials technology fields. Background technique [0002] Due to its excellent performance, polyurethane polymer materials have been widely used in many fields, such as construction, transportation, furniture, electrical appliances and other industries. The oxygen index of ordinary polyurethane materials is only 17%, which is a flammable material, which is easy to cause fire, which brings great hidden dangers to people's lives and property safety. Adding flame retardants to raw materials is to improve the flame retardancy of polyurethane foam plastics. The most performan...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G79/04C07F9/11C08G18/64C08G18/32
Inventor 匡轩王刚王志玲
Owner UNIV OF JINAN
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