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Phosphorus-containing vegetable oil-based flame-retardant polyol and its preparation method and application

A flame-retardant polyol, vegetable oil-based technology, which is applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc. problem, to achieve good synergistic flame retardant effect, improved storage stability, and high flame retardancy.

Active Publication Date: 2018-06-26
INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Researchers have conducted a lot of research on the structure and performance of DOPO for a long time, but due to the high production cost of DOPO, the wide application of DOPO flame retardants in production engineering is limited.

Method used

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  • Phosphorus-containing vegetable oil-based flame-retardant polyol and its preparation method and application
  • Phosphorus-containing vegetable oil-based flame-retardant polyol and its preparation method and application
  • Phosphorus-containing vegetable oil-based flame-retardant polyol and its preparation method and application

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Effect test

preparation example Construction

[0044] See Attached Table 1 and Attached Table 2 for the preparation formula and performance test results of vegetable oil-based flame-retardant rigid polyurethane foam. The combination of polyol and isocyanate is used as the main raw material. When foaming, the molar ratio of NCO / OH is 1.5-2.5. The specific operation is as follows: Mix the combined polyol and additives evenly under the condition of rapid stirring, then stir with 130 parts of isocyanate at the speed of 2000-3000r / min for 10-20s, pour into the mold, and mature for 48h .

[0045] The selection of isocyanate: toluene diisocyanate, xylene diisocyanate, polymethyl polyphenyl polyisocyanate (PAPI), preferably PAPI, the trade name is PM-200 of Yantai Wanhua Polyurethane Co., Ltd.

Embodiment 1

[0047] Proportionally, weigh 4.0g phosphotungstic acid, dissolve in 15mL distilled water, add 31mL 30wt.% H 2 o 2 Stir at room temperature to make it dissolve completely and mix evenly; add 1.30 g of dodecylpyridinium chloride chloroform solution dropwise into the above solution using a dropping funnel, and continue stirring for 30 min at the same time, after the reaction ends , filtered, and vacuum-dried at 60°C to obtain a quaternary ammonium phosphotungstic acid phase transfer catalyst.

[0048] Tung oil methyl ester and hydrogen peroxide are epoxidized to obtain epoxidized tung oil methyl ester (mol ratio n C＝C :n H2O2 =1:2), the epoxidation reaction condition is 50°C, and the reaction time is 4h; after the reaction is completed, it is cooled to -15°C, and the hydrogen peroxide, water and catalyst in the system are separated by centrifugation; 60 parts by mass of epoxy Put tung oil methyl ester and 0.06 parts by mass of triphenylphosphine in a four-necked flask, and aft...

Embodiment 2

[0050] Proportionally, weigh 4.0g phosphotungstic acid, dissolve in 15mL distilled water, add 35mL 30wt.% H 2 o 2 Stir at room temperature to make it dissolve completely and mix evenly; add 1.30 g of dodecylpyridinium chloride chloroform solution dropwise into the above solution using a dropping funnel, and continue stirring for 30 min at the same time, after the reaction ends , filtered, and vacuum-dried at 60°C to obtain a quaternary ammonium phosphotungstic acid phase transfer catalyst.

[0051] Tung oil methyl ester and hydrogen peroxide are epoxidized to obtain epoxidized tung oil methyl ester (mol ratio n C＝C :n H2O2 =1:2), the epoxidation reaction condition is 50°C, and the reaction time is 4h; after the reaction is completed, it is cooled to -15°C, and the hydrogen peroxide, water and catalyst in the system are separated by centrifugation; 60 parts by mass of epoxy Put tung oil methyl ester and 0.05 parts by mass of triphenylphosphine in a four-necked flask, and aft...

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Abstract

The invention relates to phosphorus-containing vegetable oil based flame-retardant polyol and a preparation method and application thereof. The preparation method of the phosphorus-containing vegetable oil based flame-retardant polyol comprises the following steps: carrying out epoxide reaction on tung oil methyl ester with hydrogen peroxide and methanoic acid under the catalyzing effect of a home-made phase transfer catalyst at first to prepare multi-functionality-degree epoxidized tung oil methyl ester; reacting the obtained epoxidized tung oil methyl ester with reactive-hydrogen-containing DOPO (DOPO belongs to phosphorus-containing phenanthrene ring and heterogeneous ring compound, and the full name of DOPO is 9,10-diamine-9-oxygen heterocyclic-10- phosphaphenanthrene-10-oxide) to obtain the phosphorus-containing vegetable oil based flame-retardant polyol. The obtained polyol is a flame retardant, the synthesized structural flame-retardant vegetable oil based polyol is used in hard polyurethane flame-retardant foam, mechanical strength and flame retardance of the foam are improved, and a preparation process is simple, convenient to operate and easy to obtain. The phosphorus-containing vegetable oil based flame-retardant polyol is compounded with tris( 2-chloropropyl) phosphate, phosphorus-nitrogen synergistic flame retardant effect is good, the use amount of a flame retardant can be reduced, the flame retardant effect is much better than the flame retardant effect of the tris( 2-chloropropyl) phosphate which is used independent, and the oxygen index (LOI) can reach 29%.

Description

technical field [0001] The invention belongs to the technical field of structural flame-retardant vegetable oil-based polyols, and mainly relates to phosphorus-containing vegetable oil-based flame-retardant polyols and a preparation method and application thereof. Background technique [0002] Polyurethane foam insulation material is currently the best insulation material in the world. Rigid polyurethane foam has excellent properties such as light weight, low thermal conductivity, good heat resistance, easy bonding with other substrates, and no droplet. However, the polyurethane material without flame retardant treatment is combustible. When burning, it will not only produce a lot of smoke but also release toxic gas, which not only brings difficulties to fire fighting, but also poses a threat to people's health and life safety. Therefore, the requirements for heat resistance, flame retardancy and non-toxicity of rigid polyurethane foam are getting higher and higher. Variou...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/6571C08G18/38C08G18/48C08G18/66C08G101/00
CPCC07F9/657163C08G18/3878C08G18/48C08G18/6696C08G2101/00
Inventor 周永红郑敏睿张猛薄采颖
Owner INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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