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Phosphorus-nitrogen co-reactive flame retardant used for polyurethane, preparation method therefor and application thereof

A synergistic reaction and flame retardant technology, applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., can solve problems such as harsh and complicated synthesis conditions, and achieve low cost and high yield , Improve the effect of low flame retardant efficiency

Inactive Publication Date: 2015-12-23
QUANGANG PETROCHEM RES INST OF FUJIAN NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to overcome the problems of harsh and complex synthesis conditions in the production of existing structural flame-retardant polyurethane materials, and to provide a phosphorus-nitrogen compound with a simple synthesis process, high yield, and a double hydroxyl group containing DOPO group as the terminal group. Preparation method of synergistic reaction flame retardant

Method used

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  • Phosphorus-nitrogen co-reactive flame retardant used for polyurethane, preparation method therefor and application thereof
  • Phosphorus-nitrogen co-reactive flame retardant used for polyurethane, preparation method therefor and application thereof
  • Phosphorus-nitrogen co-reactive flame retardant used for polyurethane, preparation method therefor and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0044] Add 105g (1.0mol) diethanolamine and 110mL absolute ethanol to a dry three-necked flask, raise the temperature to 28°C, add 92.5g (1.0mol) epichlorohydrin dropwise while stirring, react for 5 hours, and raise the temperature to 50°C, NaOH solution (concentration: 50wt%) was added dropwise at a constant speed, and the reaction was continued for 2 h to obtain a white suspension. Remove NaCl by filtration, remove the solvent by rotary evaporation, and dry to obtain the reaction intermediate glycidyldiethanolamine.

[0045] Add 80.5g (0.5mol) of glycidyldiethanolamine and 200mL of absolute ethanol to a dry three-necked flask, raise the temperature to 120°C, add 108g (0.5mol) of DOPO in batches while stirring, and react for 8 hours. A light yellow transparent liquid was obtained. Add diethyl ether to the liquid, a white precipitate is formed, remove the filtrate by filtration, rinse the precipitate with diethyl ether several times, and dry at 80°C to obtain a white powder, ...

Embodiment 2

[0048] Add 133g (1.0mol) of diisopropanolamine and 150mL of absolute ethanol into a dry three-necked flask, raise the temperature to 25°C, add 92.5g (1.0mol) of epichlorohydrin dropwise while stirring, react for 5 hours, and raise the temperature to At 40°C, NaOH solution (concentration: 50wt%) was added dropwise at a constant speed, and the reaction was continued for 2 hours to obtain a white suspension. Remove NaCl by filtration, remove the solvent by rotary evaporation, and dry to obtain the reaction intermediate glycidyl diisopropanolamine.

[0049] Add 94.5g (0.5mol) glycidyl diisopropanolamine and 200mL absolute ethanol to a dry three-necked flask, raise the temperature to 120°C, add 108g (0.5mol) DOPO in batches while stirring, and react for 8 hours to obtain shallow Yellow transparent liquid. Add diethyl ether to the liquid, a white precipitate is formed, remove the filtrate by filtration, rinse the precipitate with diethyl ether several times, and dry at 80°C to obta...

Embodiment 3

[0052] Add 161g (1.0mol) of dibutanolamine and 200mL of absolute ethanol into a dry three-necked flask, raise the temperature to 30°C, add 92.5g (1.0mol) of epichlorohydrin dropwise while stirring, react for 5 hours, and raise the temperature to 60°C ℃, NaOH solution (concentration 50%) was added dropwise at a constant speed, and the reaction was continued for 2 hours to obtain a white suspension. Remove NaCl by filtration, remove the solvent by rotary evaporation, and dry to obtain the reaction intermediate glycidyl butanolamine.

[0053] Add 108.5g (0.5mol) glycidyl butanolamine and 100mL absolute ethanol to a dry three-necked flask, raise the temperature to 120°C, add 108g (0.5mol) DOPO in batches while stirring, and react for 8 hours to obtain light yellow transparent liquid. Add diethyl ether to the liquid, a white precipitate is formed, remove the filtrate by filtration, wash the precipitate with diethyl ether several times, and dry at 80°C to obtain a white powder, tha...

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Abstract

The present invention discloses a phosphorus-nitrogen co-reactive flame retardant used for polyurethane, a preparation method therefor and an application thereof. The method comprises: adding epoxy chloropropane and alcohol amine compound into an organic solvent; carrying out an ring-opening and ring-closing reactions in a reaction molar ratio; and filtering, and removing the solvent under reduced pressure, thereby obtaining a reaction intermediate glycidol alcohol amine which is viscous liquid at room temperature; and carrying out a reaction between DOPO and an epoxy group to form a reactive flame retardant with end groups as double hydroxyl groups and a DOPO flame retardant group. The flame retardant has a phosphorus-nitrogen co-reactive flame retardant effect, is environmentally-friendly,non-toxic, low in smoke, and can be used as a chain extender to apply to the preparation for a structural flame retardant polyurethane material, so that the preparation process is simple, and the flame-retardant effect is remarkable. The polyurethane material synthesized by using the flame retardant has good mechanical properties, an oxygen index increased to 27-29%, and a flame retardant grade up to UL94 V-0.

Description

technical field [0001] The invention relates to the preparation and application of a phosphorus-nitrogen synergistic reaction flame retardant for polyurethane. Background technique [0002] With the enhancement of people's awareness of fire prevention and the development of social economy, research and development of various low-toxicity and high-efficiency flame retardants has become a major trend. At present, the commonly used flame retardants are mainly three types: organohalogen, organophosphorus and inorganic. Phosphorus flame retardants are the flame retardants with the most application potential in contemporary times. Among them, 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) has a unique chemical structure, thermal stability is better than general phosphate, and has low phosphorus content, The advantages of halogen-free and non-toxic have attracted extensive attention from researchers. Utilizing its active P-H bond to easily react with unsaturated bonds,...

Claims

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Application Information

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IPC IPC(8): C08K5/53C08G18/42C08G18/38C08G18/32C08G18/66C07F9/6571
Inventor 郑雪琳李毅辉翁家宝陈登龙
Owner QUANGANG PETROCHEM RES INST OF FUJIAN NORMAL UNIV
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