Preparation method of sulfydryl graphene copolymerized mercapto-alkenyl polymer flame-retardant system

A technology of mercapto compounds and graphene, which is applied in the field of compound synthesis, can solve the problems of weak vinyl reactivity, poor migration resistance, and agglomeration, and achieve excellent heat and oxygen insulation capabilities, improved mechanical properties, and high flame retardant efficiency Effect

Active Publication Date: 2020-12-25
NINGBO UNIVERSITY OF TECHNOLOGY
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

However, this modified carbon nanotube flame retardant is a one-dimensional nano-carbon material, which has a large volume, which leads to poor dispersion of the above-mentioned materials in the matrix and serious agglomeration phenomenon, which reduces the flame retardancy of the flame retardant. The combustion efficiency and the mechanical properties of the mercapto-alkene matrix; under light curing conditions, the reactivity of the vinyl group is weak, and the grafting rate is low, resulting in poor migration resistance of the above-mentioned reactive flame retardants in the matrix

Method used

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  • Preparation method of sulfydryl graphene copolymerized mercapto-alkenyl polymer flame-retardant system
  • Preparation method of sulfydryl graphene copolymerized mercapto-alkenyl polymer flame-retardant system
  • Preparation method of sulfydryl graphene copolymerized mercapto-alkenyl polymer flame-retardant system

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Embodiment 1

[0029] The preparation method of mercaptographene copolymerized mercapto-ene polymer flame retardant system in the present embodiment comprises the following steps:

[0030] (1) Synthesis of mercapto graphene

[0031] Dissolve 100 mg of hydroxygraphene in 50 mL of tetrahydrofuran, ultrasonicate for 1 hour, and then add 200 mg of γ-mercaptopropyltrimethoxysilane, 50 mg of N,N'-dicyclohexylcarbodiimide and 1 mL of ammonia water in sequence under nitrogen protection. React at 65°C for 12 hours; after the reaction, wash with methanol and vacuum dry to obtain a mercapto graphene flame retardant, such as figure 1 As shown; graphene is a new material with a single-layer sheet structure composed of carbon atoms, and the surface is very smooth; it can be seen from the AFM image that the surface of graphene grafted with mercapto compounds has a layer structure surface The different colors of light and dark indicate that the surface of graphene becomes rough due to the functionalization...

Embodiment 2

[0035] The preparation method of mercaptographene copolymerized mercapto-ene polymer flame retardant system in the present embodiment comprises the following steps:

[0036] (1) Synthesis of mercapto graphene

[0037] Dissolve 100 mg of hydroxygraphene in 50 mL of ethanol, sonicate for 1 hour, then add 100 mg of 2-mercaptoethyltriethoxysilane, 50 mg of N,N'-dicyclohexylcarbodiimide and 1 mL of Ammonia, react at 65°C for 12 hours. After the reaction is finished, wash with methanol and dry in a vacuum to obtain the mercaptographene flame retardant;

[0038] (2) Preparation of mercapto-ene polymer flame retardant system

[0039] In a four-necked flask equipped with a stirrer and a condenser, add 100g deionized water, 0.1g NP-4, 0.05g AES-A, and stir at a high speed for 30 minutes; then add 10g EDDT, 12g TMPTA, 0.04g step (1 ) the prepared mercapto graphene flame retardant was dispersed in 100g deionized water, slowly and continuously added to the above-mentioned four-necked fl...

Embodiment 3

[0041] The preparation method of mercaptographene copolymerized mercapto-ene polymer flame retardant system in the present embodiment comprises the following steps:

[0042] (1) Synthesis of mercapto graphene

[0043] Dissolve 100 mg of hydroxygraphene in 50 mL of tetrahydrofuran, sonicate for 1 hour, and then add 200 mg of γ-mercaptopropyltrimethoxysilane, 50 mg of N,N'-dicyclohexylcarbodiimide and 1 mL of tetramethyl ammonium hydroxide, and reacted at 65°C for 12 hours. After the reaction is finished, wash with methanol and dry in a vacuum to obtain the mercaptographene flame retardant;

[0044] (2) Preparation of mercapto-ene polymer flame retardant system

[0045]In a four-necked flask equipped with a stirrer and a condenser tube, add 100g deionized water, 0.1g NP-4, 0.05g AES-A, and stir at a high speed for 30 minutes; then add 10g EDDT, 10g PTTTA, 0.2g step (1 ) the prepared mercapto graphene flame retardant was dispersed in 100g deionized water, slowly and continuous...

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Abstract

The invention relates to a preparation method of a sulfydryl graphene copolymerized mercapto-alkenyl polymer flame-retardant system, which has the advantages of stable structure and migration resistance by virtue of a stable preparation process of starvation-state semi-continuous emulsion polymerization and extremely strong reaction activity of sulfydryl in a modified graphene structure. No precipitation phenomenon occurs after long-term use; moreover, the graphene is a two-dimensional nano carbon material and has good compatibility and dispersity with a matrix, other properties of the matrixare not lost under the existing addition concentration, and the mechanical properties are also improved to a certain extent; according to the prepared flame-retardant system, the mercapto-alkenyl polymer serves as a matrix, mercapto-graphene serves as a flame retardant, the mercapto-alkenyl polymer and the mercapto-grapheneare combined through chemical bonds to form a reaction type flame-retardantsystem, and the graphene flame retardant has excellent heat and oxygen insulation capacity in the combustion process, is extremely high in flame-retardant efficiency and has a very good flame-retardant effect under the condition that the adding amount is 0.2-1 wt%.

Description

technical field [0001] The invention relates to the technical field of compound synthesis, in particular to a preparation method of a mercapto graphene copolymerized mercapto-ene polymer flame retardant system. Background technique [0002] Compared with traditional acrylate polymerization, mercapto-ene polymerization has the advantages of no oxygen inhibition, small shrinkage rate, small shrinkage stress, etc., and has broad applications in high-performance adhesives, electronic optical materials, biomedical materials, etc. prospect. However, in some application fields with high flame retardancy requirements, such as electrical equipment substrates or outer coatings, the flame retardancy of mercapto-ene polymers still has defects, and the limiting oxygen index (LOI) is less than 20. In order to ensure people's safety and reduce fire hazards, flame retardants need to be added to mercapto-ene polymers during processing. [0003] At present, there are mainly two methods for ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G75/045C08K9/06C08K3/04
CPCC08G75/045C08K9/06C08K3/042
Inventor 吴方怡王江波包晓慧黄启泽陈诗琪
Owner NINGBO UNIVERSITY OF TECHNOLOGY
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