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A cage network structure hybrid silsesquioxane flame retardant containing dopo group and its preparation method and application

A technology of silsesquioxane and network structure, which is applied in the field of cage network structure hybrid silsesquioxane flame retardant and its preparation, can solve the problems of difficult uniform dispersion, high cage internal interaction strength, poor process performance, etc. Achieve good process performance, good flame retardant effect, and improve the effect of flame retardancy

Active Publication Date: 2020-06-16
INST OF CHEM CHINESE ACAD OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, POSS with a regular cage structure has high cage interaction strength, which makes its process performance poor when mixed with resin, and it is difficult to disperse uniformly in resin (European Polymer Journal, 2010, 46, 14-23)

Method used

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  • A cage network structure hybrid silsesquioxane flame retardant containing dopo group and its preparation method and application
  • A cage network structure hybrid silsesquioxane flame retardant containing dopo group and its preparation method and application
  • A cage network structure hybrid silsesquioxane flame retardant containing dopo group and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] according to figure 1 The synthetic route shown is the preparation of DOPO group-containing cage network structure hybrid silsesquioxane flame retardant Poly(DOPO-POSS).

[0045] Add 72.846g DOPO-VTMS, 150ml methyl ethyl ketone and 20ml methanol to a three-necked flask equipped with mechanical stirring and reflux condenser, and stir slowly for 1h until completely dissolved. The temperature of the reaction system was controlled at 0-5°C, 0.06g of sodium hydroxide was added, stirring was continued and the temperature was raised to 60°C. Slowly add 15ml of deionized water dropwise. After the dropwise addition, the reaction was continued at 60°C for 32h, and the temperature was lowered to room temperature after the reaction was completed.

[0046] Stand for stratification, wash the organic phase with water for 3 to 5 times, add anhydrous sodium sulfate to remove the moisture in the organic phase, filter the desiccant after 6 hours, and remove the organic solvent by rotary...

Embodiment 2

[0049] In a three-necked flask equipped with mechanical stirring and a reflux condenser, add 18.22g DOPO-VTMS, 1.2319g2-(3,4-epoxycyclohexyl)ethyltrimethoxysilane, 100ml tetrahydrofuran and 5ml methanol, and stir slowly for 1.5 h until completely dissolved. The temperature of the reaction system was controlled at 15-20°C, 0.05g of tetramethylammonium hydroxide was added, stirring was continued and the temperature was raised to 55°C. Slowly add 8ml of deionized water dropwise. After the dropwise addition, continue to react at 55° C. for 60 h, and cool down to room temperature after the reaction is completed.

[0050] Stand for stratification, wash the organic phase with water for 3 to 5 times, add anhydrous magnesium sulfate to remove the moisture in the organic phase, filter the desiccant after 22 hours, and remove the organic solvent by rotary evaporation to obtain a white solid powder, which is the cage containing DOPO group Network structure hybrid silsesquioxane flame re...

Embodiment 3

[0053] Add 18.22g of DOPO-VTMS, 4.034g of 3-aminopropyltrimethoxysilane, 500ml of dichloromethane and 20ml of methanol into a three-necked flask equipped with mechanical stirring and reflux condenser, and stir slowly for 2h until completely dissolved. The temperature of the reaction system was controlled at -5 to 0°C, 0.04g of sodium bicarbonate was added, stirring was continued and the temperature was raised to 50°C. Slowly add 9ml of deionized water dropwise. After the dropwise addition, continue to react at 50°C for 70h, and cool down to room temperature after the reaction is completed.

[0054] Stand for stratification, wash the organic phase with water for 3 to 5 times, add anhydrous magnesium sulfate to remove the moisture in the organic phase, filter the desiccant after 24 hours, and remove the organic solvent by rotary evaporation to obtain a white solid powder, which is the cage containing DOPO group Network structure hybrid silsesquioxane flame retardant Poly(DOPO / N...

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Abstract

The invention discloses a polyhedral oligomeric silsesquioxane-mixed flame retardant containing DOPO (9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide) groups and a preparation method and application thereof, and belongs to the technical field of preparation and application of flame retardants. A formula of the polyhedral oligomeric silsesquioxane-mixed flame retardant containing the DOPO groupsis shown in the attached figure, wherein R group is R1 group, or the combination of R1 and any or two of R2, R3 and R4, and the R2 or R3 or R4 does not simultaneously exist. The polyhedral oligomericsilsesquioxane-mixed flame retardant containing the DOPO groups has the advantages that the halogen-free and poisonless effects are realized, the flame-retarding effect is good, the compatibility with a polymer matrix is good, the preparation method is simple, and the polyhedral oligomeric silsesquioxane-mixed flame retardant is suitable for amplified production.

Description

technical field [0001] The invention belongs to the technical field of flame retardant preparation and application, and in particular relates to a DOPO group-containing cage net structure hybrid silsesquioxane flame retardant, a preparation method and application thereof. Background technique [0002] With the development of high technology, polymer materials have been widely used in electronic appliances, transportation, aerospace, home building materials and other fields. However, most polymer materials are flammable and combustible materials. When burning, the heat release rate is high, the flame spreads quickly, and dense smoke and poisonous gas are produced, which poses a huge threat to life safety. Therefore, the flame retardant research of polymer materials has become an urgent problem to be solved in safe production and life. [0003] Flame retardants can be divided into inorganic flame retardants, halogen flame retardants, phosphorus flame retardants, silicon flame...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/30C08L63/00C08L83/08
CPCC08G77/30C08L63/00C08L2201/02C08L83/08
Inventor 刘兴华赵晓娟黄伟杨欣于然张瑛
Owner INST OF CHEM CHINESE ACAD OF SCI