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Compound with a plurality of active groups and preparation method of compound

A technology of active groups and compounds, which is applied in the field of compounds containing multiple active groups and their preparation, can solve problems such as easy combustion, and achieve the effects of good carbon-forming performance, simple equipment and high thermal stability.

Inactive Publication Date: 2014-08-13
ZHONGBEI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to solve the problem that the commonly used reactive flame retardants have relatively few reactive groups and the amount of flame retardants is relatively large, the present invention provides a Compound with multiple active groups and preparation method thereof

Method used

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  • Compound with a plurality of active groups and preparation method of compound
  • Compound with a plurality of active groups and preparation method of compound
  • Compound with a plurality of active groups and preparation method of compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] The preparation method of the compound (FR-1) containing multiple active groups,

[0038] The steps are:

[0039] first step,

[0040] (1) Weigh 5.52g (0.03mol) of cyanuric chloride and dissolve it in 50mL of toluene, stir until completely dissolved, slowly raise the temperature to 60°C, keep stirring while keeping warm, so that the reactants are evenly dispersed;

[0041] (2) Under nitrogen protection atmosphere, add 5.48g (0.033mol) triethyl phosphite solution dissolved in 50mL acetone, react for 4h, keep stirring during the reaction;

[0042] (3) After the reaction is over, stop the heat preservation, gradually cool to room temperature, filter, and rotary evaporate to obtain intermediate M;

[0043] second step,

[0044] (4) Dissolve 5.72g (0.02mol) of intermediate M in 50mL of tetrahydrofuran, stir until completely dissolved, slowly raise the temperature to 60°C, keep stirring while keeping warm, so that the reactants are evenly dispersed;

[0045] (5) Weigh 1.0...

Embodiment 2

[0049] The preparation method of the compound (FR-1) containing multiple active groups,

[0050] The steps are:

[0051] first step,

[0052] (1) Weigh 9.30g (0.05mol) of cyanuric chloride and dissolve it in 80mL of acetone, stir until completely dissolved, slowly raise the temperature to 60°C, keep stirring while keeping warm, so that the reactants are evenly dispersed;

[0053] (2) Under nitrogen protection atmosphere, add 6.20g (0.05mol) trimethyl phosphite solution dissolved in 80mL toluene and acetone mixed solvent (1:2 volume ratio), react for 6h, keep stirring during the reaction ;

[0054] (3) After the reaction is over, stop the heat preservation, gradually cool to room temperature, filter, and rotary evaporate to obtain intermediate M;

[0055] second step,

[0056] (4) Dissolve 9.76g (0.04mol) of intermediate M in 80mL of 1,4-dioxane, stir until completely dissolved, slowly raise the temperature to 55°C, keep stirring while keeping warm, so that the reactants ar...

Embodiment 3

[0060] The preparation method of the compound (FR-2) containing multiple active groups,

[0061] The steps are:

[0062] first step,

[0063] (1) Weigh 7.44g (0.04mol) of cyanuric chloride and dissolve it in 70mL of 1,4-dioxane, stir until completely dissolved, slowly raise the temperature to 60°C, keep stirring while keeping warm, so that the reactants are evenly dispersed;

[0064] (2) Under nitrogen protection atmosphere, add 7.30g (0.044mol) triethyl phosphite solution dissolved in 50mL 1,4-dioxane, react for 5h, keep stirring during the reaction;

[0065] (3) After the reaction is over, stop the heat preservation, gradually cool to room temperature, filter, and rotary evaporate to obtain intermediate M;

[0066] second step,

[0067] (4) Dissolve 8.58g (0.03mol) of intermediate M in 70mL of tetrahydrofuran, stir until completely dissolved, slowly raise the temperature to 40°C, keep stirring while keeping warm, so that the reactants are evenly dispersed;

[0068] (5) W...

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Abstract

The invention relates to a reaction type phosphorus-nitrogen flame retardant and in particular to a compound with a plurality of active groups and a preparation method of the compound. The preparation method comprises the following steps: (1) weighing cyanuric chloride, dissolving cyanuric chloride into a first solvent, stirring till being completely dissolved, slowly heating to be 60 DEG C, preserving heat while continuously stirring to uniformly disperse reactant; and (2) in the presence of nitrogen, adding a phosphite ester solution which is dissolved in the first solvent, reacting for 4-6 hours, and keeping stirring in the reaction process. Compared with the prior art, the compound with the plurality of active groups has the beneficial effects that the compound is prepared from raw materials, namely, cyanuric chloride, phosphite ester compounds (trimethyl phosphate or triethyl phosphate) and polyhydric alcohol compounds (neopentyl glycol, glycerol or pentaerythritol) with quaternary carbon (or secondary carbon) atoms, through Michaelis-Arbuzov electrophilic addition reaction and nucleophilic substitution reaction.

Description

technical field [0001] The invention relates to a reactive phosphorus-nitrogen flame retardant, in particular to a compound containing multiple active groups and a preparation method thereof. Background technique [0002] With the development of material science, synthetic polymer materials are widely used in various fields and have a great impact on people's production and life. However, most organic materials are flammable. According to incomplete statistics, there were as many as 110,000 fires in my country in 2012. In the face of such a high risk of fire, it is urgent to study the flame retardant technology of materials. [0003] Reactive flame retardants are a class of flame retardants containing special active functional groups, which introduce flame retardant groups into polymer materials by chemical bonding, and can be evenly distributed in the polymer molecular chain in the form of molecules, so , high flame retardant efficiency, only a small amount can effective...

Claims

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Application Information

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IPC IPC(8): C07F9/6521C08K5/5353
Inventor 赵培华刘亚青李欣航赵贵哲
Owner ZHONGBEI UNIV
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