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A kind of triazine hyperbranched polyurea char-forming agent and preparation method thereof

A technology of hyperbranched polyurea char-forming agent, applied in the field of hyperbranched polyurea char-forming agent and its preparation, can solve the problems of difficult dispersion, harmful water resources, poor matrix compatibility, etc., and achieves good compatibility and char-forming. Good performance and high thermal stability

Active Publication Date: 2017-08-15
TAIYUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the traditional intumescent flame retardant system is a small molecule, such as the compound of melamine-pentaerythritol-polyphosphate amine. The disadvantage is that the ternary system is not easy to mix, the compatibility with the matrix is ​​poor, it is not easy to disperse in the matrix, and it is easy to add Substrate Surface Migration
Although this method can produce hyperbranched polyphosphazene flame-retardant char-forming agent with good flame-retardant effect and processability, hexachlorocyclotriphosphazene is easy to sublimate, and its vapor is irritating to eyes and respiratory tract, and is harmful to water resources.
[0006] The existing publication numbers are: CN101880400A, CN104693442A, CN103333336A and CN103756015 disclose the use of diamino, dihydroxy compound or phosphorus-containing diamine and cyanuric chloride to synthesize a hyperbranched charcoal agent, although the method has a continuous reaction process and the product Good thermal stability, high carbon formation rate, etc., but the reaction raw materials use cyanuric chloride, so it is necessary to add an acid-binding agent to absorb hydrogen chloride during the reaction to ensure the smooth progress of the reaction, and the reactivity of the three chlorine atoms Each of them is different, and the temperature control reaction needs to be carried out in three temperature ranges of 0°C-10°C, 30°C-70°C, and 90°C-150°C, and the synthesis process is cumbersome

Method used

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  • A kind of triazine hyperbranched polyurea char-forming agent and preparation method thereof
  • A kind of triazine hyperbranched polyurea char-forming agent and preparation method thereof
  • A kind of triazine hyperbranched polyurea char-forming agent and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Take 20 parts of toluene diisocyanate and add 50 parts of acetone to dissolve it completely, then pour the solution into a three-necked flask, and at the same time add 30 parts of melamine into the three-necked flask. After fully stirring at a rotating speed of 20 min, 2 parts of triethylamine were added, and then the reaction was continued for 5 hours. Washing with 50 parts of N,N-dimethylformamide solvent for several times and then washing with water, drying the obtained solid at 100° C. for 8 hours to obtain a triazine hyperbranched polyurea char-forming agent.

[0033] In the above-mentioned experimental process, the infrared spectrograms of the prepared triazine hyperbranched polyurea char-forming agent, melamine and isocyanate are as follows: figure 1 As shown, 1512cm -1 It is the vibration absorption peak of -NH-CO-NH-, 1600cm -1 It is the -C=O- vibration absorption peak in -NH-CO-NH-, and at 2278cm -1 The -NCO group vibration peak at 3300cm -1 -3500cm -1 -N...

Embodiment 2

[0035] Take 30 parts of 4,4'-diphenylmethane diisocyanate and add 50 parts of N,N-dimethylformyl to dissolve it completely, then pour the solution into a three-necked flask, and at the same time add 40 parts of melamine In the three-necked flask, under nitrogen atmosphere, after fully stirring at 80° C. at a speed of 150 r / min for 10 minutes, 3 parts of triethanolamine were added, and then the reaction was continued for 6 hours. Washing with water after washing with 70 parts of acetone solvent for several times, drying the obtained solid at 80° C. for 6 hours to obtain a triazine hyperbranched polyurea char-forming agent.

Embodiment 3

[0037] Take 35 parts of 2,4'-diphenylmethane diisocyanate and add 60 parts of N,N-diethylformamide to dissolve it completely, then pour the solution into a three-necked flask, and at the same time add 35 parts of melamine In the three-necked flask, under a nitrogen atmosphere, after fully stirring at 70° C. for 30 minutes at a speed of 120 r / min, 4 parts of triethanolamine were added, and then the reaction was continued for 7 hours. Washing with 60 parts of N,N-dimethylacetamide solvent for several times and then washing with water, drying the obtained solid at 70° C. for 6 hours to obtain a triazine hyperbranched polyurea char-forming agent.

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Abstract

The invention relates to a triazine type hyperbranched polyurea charring agent and a preparing method thereof. In a solvent, -NCO groups of isocyanate and -NH2 in melamine are used for being reacted with each other, and the charring agent with the hyperbranched structure is generated, wherein triazine rings and a plurality of benzene rings are contained in the molecular structure, good charging performance is achieved, good hydrophobicity is shown, the contact angle reaches 90 degrees, and the compatibility with high polymer matrixes can be obviously improved. The charring agent has very good thermal stability and meets the processing requirement of high polymers, and the phenomenon that materials are degraded in the processing process, and consequently the flame retardance of the materials is lowered is avoided; when the charring agent and acid-source ammonium polyphosphate are added into polypropylene at 1:2, the limit oxygen index of a polypropylene composite reaches up to 32%, and a sample strip with the thickness of 1.6 mm can pass the UL-94 perpendicular combustion V-0 grade.

Description

technical field [0001] The invention relates to a hyperbranched polyurea char-forming agent and a preparation method thereof, in particular to a char-forming agent with a hyperbranched structure composed of isocyanate, melamine, a catalyst and a solvent and a preparation method thereof. Background technique [0002] Compared with other materials, polymer materials are widely used in all aspects of our lives because of their unique structure, easy processing and irreplaceable excellent performance. However, the flammability of polymer materials has also become a potential threat to people's lives and property safety. In order to change the flammability of polymer materials, the usual method is to add flame retardants to polymer materials, so as to reduce the ignition point of materials. [0003] With the improvement of people's quality of life and environmental quality, intumescent flame retardants are gradually replacing halogenated flame retardants and inorganic flame Fue...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G18/32C08G18/18
CPCC08G18/18C08G18/1825C08G18/3246
Inventor 晏泓张猛赵晶葛维娟许美贤魏丽乔许并社
Owner TAIYUAN UNIV OF TECH
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