Preparation method of reactive halogen-free nitrogen-phosphorus flame retardant

A nitrogen-phosphorus flame retardant and reactive technology, applied in the field of flame retardant materials, can solve the problems of shrinkage and closed cells of polyurethane foam products, high product acid value, unfavorable polyurethane foaming reaction, etc. Avoid the effect of intermediate decomposition

Inactive Publication Date: 2020-04-14
南京晨化新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the acid value of the product prepared according to this method is relatively large, which may easily lead to shrinkage and closed cells of polyurethane foam products.
In addition, use NaOH solution to adjust the pH of the paraformaldehyde depolymerization process, which has two unfavorable factors, one is the introduction of water into the system, and the other is the introduction of sodium ions, which are catalysts for polyurethane foaming, which is very harmful to the subsequent polyurethane foaming reaction. unfavorable

Method used

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  • Preparation method of reactive halogen-free nitrogen-phosphorus flame retardant
  • Preparation method of reactive halogen-free nitrogen-phosphorus flame retardant
  • Preparation method of reactive halogen-free nitrogen-phosphorus flame retardant

Examples

Experimental program
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Effect test

Embodiment 1

[0042] (1) Calculate by molar mass, take by weighing paraformaldehyde: alcohol amine=1:1, be converted into mass parts as, 30 parts of paraformaldehyde and 105 parts of diethanolamine, the paraformaldehyde that is ground into powder will join in Stir in a flask containing diethanolamine, control the temperature at 40°C, and continue the reaction for 1 hour after the paraformaldehyde is completely dissolved to obtain the intermediate 3-(2-hydroxyethyl)-1,3-oxazolane solution.

[0043] (2) The intermediate 3-(2-hydroxyethyl)-1,3-oxazolane solution obtained in step (1) was decompressed with an oil pump at 80°C (gauge pressure -0.097Mpa) After dehydration for 1 h, the intermediate 3-(2-hydroxyethyl)-1,3-oxazolane was obtained.

[0044] (3) Control the temperature of the intermediate 3-(2-hydroxyethyl)-1,3-oxazolane obtained in step (2) at 60°C, and add 110 parts of dimethyl phosphite dropwise while stirring , After the dropwise addition was completed, it was reacted for 2 hours ...

Embodiment 2

[0047] (1) Calculate by molar mass, take by weighing paraformaldehyde:alcohol amine=2:1, convert into mass parts as, 60 parts of paraformaldehyde and 105 parts of diethanolamine, the paraformaldehyde that will be ground into powdery joins Stir in a diethanolamine flask, control the temperature at 45°C, and continue the reaction for 1.5 hours after the paraformaldehyde is completely dissolved to obtain the intermediate 3-(2-hydroxyethyl)-1,3-oxazolane solution .

[0048] (2) The 3-(2-hydroxyethyl)-1,3-oxazolane intermediate solution obtained in step (1) was decompressed with an oil pump at 70°C (gauge pressure-0.097Mpa) After dehydration for 1 h, the intermediate 3-(2-hydroxyethyl)-1,3-oxazolane was obtained.

[0049] (3) Control the temperature of the intermediate 3-(2-hydroxyethyl)-1,3-oxazolane obtained in step (2) at 60°C, and add 138 parts of diethyl phosphite dropwise while stirring , After the dropwise addition was completed, the mixture was reacted for 2 hours to obta...

Embodiment 3

[0052] (1) Calculate by molar mass, take by weighing paraformaldehyde:alcohol amine=2:3, be converted into mass parts as, 30 parts of paraformaldehyde and 157.5 parts of diethanolamine, the paraformaldehyde that will be ground into powder is added to Stir in a diethanolamine flask, control the temperature at 50°C, and continue the reaction for 2 hours after the paraformaldehyde is completely dissolved to obtain the intermediate 3-(2-hydroxyethyl)-1,3-oxazolane solution.

[0053] (2) The intermediate 3-(2-hydroxyethyl)-1,3-oxazolane solution obtained in step (1) was decompressed with an oil pump at 90°C (gauge pressure -0.098Mpa) After dehydration for 1 h, the intermediate 3-(2-hydroxyethyl)-1,3-oxazolane was obtained.

[0054] (3) Control the temperature of the intermediate 3-(2-hydroxyethyl)-1,3-oxazolane obtained in step (2) at 70°C, and add 166 parts of diisopropyl phosphite dropwise while stirring The ester was reacted for 4 hours after the dropwise addition to obtain 292...

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Abstract

The invention provides a reactive halogen-free nitrogen-phosphorus flame retardant and a preparation method thereof. The preparation method comprises the following steps: (1) adding grinded paraformaldehyde powder into molten alcohol amine, stirring at 40-50 DEG C, and reacting for 1-2 hours to obtain an intermediate solution; (2) heating the intermediate obtained in the step (1) to 70-90 DEG C, and dehydrating under reduced pressure by a vacuum pump to obtain an intermediate; (3) heating the intermediate obtained in the step (2) to 50-70 DEG C again, adding phosphite in a dropwise manner while stirring, and reacting for 2-4 hours after dropwise adding to obtain a yellow transparent liquid; and (4) adding Ca(OH)2 into the yellow transparent liquid obtained in the step (3), stirring for 2-4hours at normal temperature, and filtering to obtain a final product. According to the process, adverse effects of water on inhibition of intermediate generation and hydrolysis of phosphonate are eliminated, the acid value of the obtained product is low, the process flow is optimized, and the yield and the purity of the product are improved.

Description

technical field [0001] The invention belongs to the field of flame retardant materials, and in particular relates to a preparation method of a reactive halogen-free nitrogen and phosphorus flame retardant. Background technique [0002] Polyurethane is an important industrial synthetic polymer material, which is used in all aspects of life, but its flammability can also bring serious hazards, and flame retardants can reduce its fire risk, so the research on flame retardant materials has been researchers' attention. At present, the most commonly used flame retardants in the world are halogen-containing flame retardants, which are added in a small amount and have high flame retardant efficiency, but because they emit a large amount of toxic and corrosive gases when burned, they cause environmental pollution and endanger human health. The scope is increasingly limited. Therefore, the flame-retardant materials with high flame-retardant efficiency, good safety performance, low t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G18/32C07F9/06
CPCC07F9/06C08G18/3889
Inventor 汲方奎董晓红毕继辉房连顺贾正仁吕志锋陈燕
Owner 南京晨化新材料科技有限公司
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