Phosphorus-containing polyol, preparation method thereof and flame-retardant polyurethane containing same

A polyol and diol technology, applied in the field of flame retardant polyurethane, can solve the problems of destroying the ratio of soft-hard segments and reducing the elasticity of polyurethane resin, achieving the effects of low volatility and greatly reducing mechanical properties.

Active Publication Date: 2013-05-15
山东海思蓝高分子材料有限公司
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] Since the current phosphorus-containing polyols are mainly small molecular hydroxyphosphonates, there are almost no large-molecular-weight phosphorus-containing polyols, which will destroy the soft-hard segment ratio of the obtained polyurethane when preparing polyurethane resins, thereby reducing the obtained The elasticity of the polyurethane resin

Method used

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  • Phosphorus-containing polyol, preparation method thereof and flame-retardant polyurethane containing same

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[0036]In one embodiment of the present invention, a method for preparing the above-mentioned phosphorus-containing polyol is also provided, which uses phosphonate ester and diol as raw materials, and obtains polyphosphine terminated with hydroxyl groups through transesterification condensation polymerization. esters. Among them, the raw materials for the preparation of phosphorus-containing polyols include: phosphonate esters with the structure in formula (2) and one or more diols with the structure in formula (3),

[0037]

[0038] HO-R 2 -OH (3)

[0039] In formula (2), R is methyl, ethyl, nitrile or phenyl; R 1 is methyl, ethyl or phenyl, in formula (3) R 2 is an alkyl or aryl group;

[0040] The preparation method of phosphorus-containing polyol comprises the following: S1, the phosphonate of mx mol is mixed with one or more dibasic alcohols whose total molar amount is (m+1)x~(1.03m+1)x mol, A mixed solution A is obtained, wherein m is an integer from 1 to 20, and ...

Embodiment 1

[0055] Preparation of Phosphorus-Containing Polyols

[0056] Preparation raw materials: 124g (1mol) of dimethyl methylphosphonate (boiling point: 181°C), 70g (1.13mol) of ethylene glycol (boiling point: 197.3°C), 0.4g (0.2wt of the total reactants) of dibutyltin dilaurate %) The theoretical hydroxyl value of the pre-prepared phosphorus-containing polyol is 87.5mgKOH / g. (At this time, in mx mol of dimethyl methylphosphonate and m+1)x~(1.03m+1)x mol of ethylene glycol, x=0.1, m=10, and ethylene glycol is in excess, The excess rate is 3% times the molar mass of dimethyl methylphosphonate)

[0057] Preparation method: Add dimethyl methylphosphonate, ethylene glycol, and dibutyltin dilaurate to a four-necked flask equipped with a stirrer, a thermometer, a nitrogen inlet, and a condenser, and stir evenly to form a mixed solution A, and pour it into a four-necked flask Nitrogen was introduced, and the mixed solution A was slowly heated to 180°C under the protection of nitrogen, and...

Embodiment 2

[0060] Preparation of phosphorus-containing polyols:

[0061] Raw materials: 166g (1mol) of diethyl ethylphosphonate (boiling point: 198°C), 94.5g (1.05mol) butanediol (boiling point: 228°C), 118g (boiling point: 253°C-260°C) hexanediol ( 1mol), 0.36g of cobalt acetate (0.1wt% of the total amount of reactants), and the theoretical hydroxyl value of the pre-prepared phosphorus-containing polyol is 30.5mgKOH / g after conversion. (At this time, in mx mol of diethyl ethyl phosphonate and (m+1)x~(1.03m+1)xmol of diol, x=1, m=1, and appropriate increase in diol The amount of butanediol, the ratio is 5% times the molar mass of diethyl ethyl phosphonate)

[0062] Preparation method: Add diethyl ethyl phosphonate, butanediol, hexanediol, and cobalt acetate to a four-necked flask equipped with a stirrer, a thermometer, a nitrogen inlet, and a condenser, and stir evenly to form a mixed solution A. Nitrogen gas was passed into the flask, and the mixed solution A was slowly heated to 140°...

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Abstract

The invention discloses a phosphorus-containing polyol, a preparation method thereof and flame-retardant polyurethane containing the same, wherein the phosphorus-containing polyol has the structural formula as shown in formula (1), in the formula (1), R is methyl, ethyl or phenyl; R2 is alkyl or aryl; and n is an integer from 1 to 20, and when n is more than 1, R2 in all the groups can be same or different. The phosphorus-containing polyol is the macromolecular phosphorus-containing polyol with a linear structure, the molecular weight of the phosphorus-containing polyol is similar to that of a polyether polyol or a polyester polyol used in the preparation process of polyurethane resin, and the phosphorus-containing polyol contains a reactive functional group and can be used as the polyol for preparing the polyurethane resin; and furthermore, the volatility of the phosphorus-containing polyol is lower, when the phosphorus-containing polyol is used, the soft-hard section ratio in the polyurethane resin during preparation can not be damaged, the flame retardance is further ensured, and the mechanical properties of the prepared polyurethane resin are simultaneously improved.

Description

technical field [0001] The invention relates to the field of flame-retardant polymers, in particular to a phosphorus-containing polyol, a preparation method thereof and a flame-retardant polyurethane containing the same. Background technique [0002] In order to achieve the purpose of flame retardancy, a flame retardant is usually added. According to the reactivity, the flame retardant can be divided into two types: additive type and reactive type. Additive flame retardants are commonly used, but there are disadvantages such as large amount of addition, great influence on the mechanical properties of polymers, and easy precipitation; reactive flame retardants can react with certain functional groups of polymers to improve compatibility with polymers , especially, when the flame retardant molecule is used as a reactive monomer to completely react with the polymer monomer to form a homogeneous polymer, the polymer becomes a structural flame retardant material, which is an idea...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G79/04C07F9/40C08G18/32C08G18/64
Inventor 卢丽燕
Owner 山东海思蓝高分子材料有限公司
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