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Method for preparing reactive type halogen-free flame retardant for coating

A reactive flame retardant technology, applied in fire-resistant coatings, chemical instruments and methods, and compounds of Group 5/15 elements of the periodic table, etc., can solve the problems of reducing coating adhesion and weather resistance, and achieve flame retardant performance Good, simple process, and easy-to-obtain raw materials

Inactive Publication Date: 2015-04-08
王树礼
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since fire retardant coatings need to add a relatively large amount of flame retardants to achieve a more ideal flame retardant effect, and the flame retardants in the prior art have the problem of reducing the adhesion, weather resistance and other properties of the coatings after being added to the coatings.

Method used

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  • Method for preparing reactive type halogen-free flame retardant for coating
  • Method for preparing reactive type halogen-free flame retardant for coating
  • Method for preparing reactive type halogen-free flame retardant for coating

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] (1) In a reactor equipped with a thermometer, dropping funnel, nitrogen inlet pipe, and reflux condenser (the tail end is connected to an anhydrous calcium chloride drying tube and a hydrogen chloride absorption bottle), add 0.1mol neopentyl dichloride Alcohol and 300ml chloroform, stirred and heated to the reflux temperature, then added dropwise 0.1mol phosphorus oxychloride, reacted at the reflux temperature after the dropwise addition until no HCl gas was released at the outlet tube, and then removed the solvent to obtain a white solid 2-oxo- 2-Chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane.

[0022] (2) Add 0.1mol 2-oxo-2-chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane and 3ml of phosphine in the reactor as in step (1) After the acid agent and 300ml dimethyl sulfoxide were stirred and dissolved, 0.1mol hydroxyethyl methacrylate was added, and heated to reflux temperature until almost no HCl gas was released. The dispersion medium was distilled off under reduced pressure...

Embodiment 2

[0024] (1) In the second reactor equipped with a thermometer, a dropping funnel, a nitrogen inlet pipe, and a reflux condenser (the tail section is connected to an anhydrous calcium chloride drying tube and a hydrogen chloride absorption bottle), add 0.15mol neopentyl Glycol and 300ml chloroform, stirred and heated to the reflux temperature, then added dropwise 0.1mol phosphorus oxychloride, reacted at the reflux temperature after the dropwise addition until no HCl gas was released at the outlet tube, and then removed the solvent to obtain a white solid 2-oxo -2-Chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane.

[0025] (2) Add 0.1mol 2-oxo-2-chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane and 3ml of phosphine in the reactor as in step (1) After the acid agent and 300ml dimethyl sulfoxide were stirred and dissolved, 0.1mol hydroxyethyl methacrylate was added, and heated to reflux temperature until almost no HCl gas was released. The dispersion medium was distilled off under reduced ...

Embodiment 3

[0027] (1) In a reactor equipped with a thermometer, dropping funnel, nitrogen inlet pipe, and reflux condenser (the tail end is connected to an anhydrous calcium chloride drying tube and a hydrogen chloride absorption bottle), add 0.1mol neopentyl dichloride Alcohol and 300ml chloroform, stirred and heated to the reflux temperature, then added dropwise 0.1mol phosphorus oxychloride, reacted at the reflux temperature after the dropwise addition until no HCl gas was released at the outlet tube, and then removed the solvent to obtain a white solid 2-oxo- 2-Chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane.

[0028] (2) Add 0.1mol 2-oxo-2-chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane and 3ml of phosphine in the reactor as in step (1) After the acid agent and 300ml dimethyl sulfoxide were stirred and dissolved, 0.15mol hydroxyethyl methacrylate was added, and heated to reflux temperature until almost no HCl gas was released. The dispersion medium was distilled off under reduced pressur...

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Abstract

The invention provides a method for preparing a reactive type halogen-free flame retardant for a coating, and belongs to the field of flame retardant synthesis. The method is characterized by comprising the following steps: firstly, implementing reaction on neopentyl glycol and phosphorus oxychloride so as to prepare 2-oxo-2-chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane; implementing condensation reaction on hydroxyethyl methacrylate and 2-oxo-2-chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane so as to prepare a final product 5,5-dimethyl-2-hydroxyethyl methacrylate-2-oxo-1,3,2-dioxaphosphorinane. The method is simple in process, easy in obtaining of raw materials and high in conversion rate, and the prepared reactive type halogen-free flame retardant is good in flame retardancy, does not affect properties such as the adhesion property and the weather resistance of the coating after being added into the coating, can be widely used for preparing various acrylic acid and acrylic flame-retardant coating emulsions, and can be also applied to flame retardancy of plastic, rubber and textile as a reactive type flame retardant additive.

Description

technical field [0001] The invention relates to the field of flame retardant synthesis, in particular to a preparation method of a reactive halogen-free flame retardant for coatings. Background technique [0002] In today's world, safety awareness is becoming more and more popular, and fire-resistant coatings have attracted people's attention because they can effectively protect wooden structures and steel structures and reduce the frequency of fires. Since the fire retardant coating needs to add a relatively large amount of flame retardant to achieve a relatively ideal flame retardant effect, and the flame retardant in the prior art will reduce the adhesion, weather resistance and other properties of the coating after being added to the coating. Therefore, it is necessary to prepare a new type of flame retardant to solve this problem. Contents of the invention [0003] The purpose of the present invention is to overcome the deficiencies of the prior art and provide a met...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6574C09D5/18
Inventor 王树礼张胜孙军胡献宏
Owner 王树礼
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