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High-temperature-resistant high-crosslinking thermosetting resin system and preparation method thereof

A high-crosslinking, thermosetting technology, applied in the field of thermosetting resins, can solve the problems of high curing temperature and poor processability of benzoxazine resins

Active Publication Date: 2020-07-17
镇江利德尔复合材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the curing temperature of benzoxazine resins is generally high, resulting in poor processability

Method used

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  • High-temperature-resistant high-crosslinking thermosetting resin system and preparation method thereof
  • High-temperature-resistant high-crosslinking thermosetting resin system and preparation method thereof
  • High-temperature-resistant high-crosslinking thermosetting resin system and preparation method thereof

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preparation example Construction

[0044] In a second aspect, the present invention provides a method for preparing a high-temperature resistant and highly cross-linked thermosetting resin system. Specifically, the method for preparing the high-temperature-resistant and highly cross-linked thermosetting resin system may include the following steps:

[0045] Mix resveratrol, allylamine and paraformaldehyde in a molar ratio of 1:3:6 and add to the organic solvent, heat up to 110-125°C and react for 4-8 hours;

[0046] The organic solvent is one or a mixture of toluene, xylene and dioxane;

[0047] Alkali washing the reaction solution, rotary evaporation, and drying to obtain the propenyl-containing trifunctional benzoxazine monomer;

[0048] The propenyl-containing trifunctional benzoxazine monomer and the dithiol compound are physically blended at room temperature in a molar ratio of 2:1 to 2:4. After uniform mixing, the temperature rises to cure, copolymerize and crosslink to obtain High temperature resistant ...

Embodiment 2

[0061] The reactant 4,4'-thiodiphenylthiol in the second step in the embodiment 1 is replaced by 1,5-dimercaptonaphthalene, the amount of the reactant is changed accordingly, and other operating steps are the same as in the embodiment 1 in the steps.

[0062] In the second step reaction, the amount of reactants was changed to: 4.71 g (0.01 mol) of propenyl-containing trifunctional benzoxazine monomer, and 2.88 g (0.015 mol) of 1,5-dimercaptonaphthalene. The specific chemical structure of the obtained highly cross-linked thermosetting resin product is:

[0063]

[0064] The temperature of the highly crosslinked thermosetting resin product obtained in this example is 365°C when the thermosetting weight loss is 5%, and the carbon residue rate is 72% when the inert gas atmosphere is 800°C, and the heat release energy of the flame retardant test result is 36Jg -1 K -1 , UL94 rating is V0.

Embodiment 3

[0066] The reactant 4,4'-thiodiphenylthiol in the second step in Example 1 is replaced by 2,5-dimercaptothiadiazole, the amount of the reactant is changed accordingly, and other operating steps are implemented in the same way Steps in Example 1.

[0067] In the second step reaction, the amount of the reactant was changed to: 4.71 g (0.01 mol) of the propenyl-containing trifunctional benzoxazine monomer, and 2.25 g (0.015 mol) of 2,5-dimercaptothiadiazole. The specific chemical structure of the obtained highly cross-linked thermosetting resin product is:

[0068]

[0069] The temperature of the highly cross-linked thermosetting resin product obtained in this example is 394°C when the thermosetting weight loss is 5%, and the carbon residue rate is 77% when the inert gas atmosphere is 800°C, and the heat release energy of the flame retardant test result is 27Jg -1 K -1 , UL94 rating is V0.

[0070] After a large amount of data investigation, it was found that the thiol-ene ...

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Abstract

The invention discloses a high-temperature-resistant high-crosslinking thermosetting resin system and a preparation method thereof. The preparation method comprises the following steps: mixing resveratrol, allylamine and paraformaldehyde, adding the mixture into an organic solvent, heating to 110-125 DEG C, continuing to react for 4-8 hours, carrying out alkali washing, rotary evaporation and drying on the reaction solution after the reaction is completed, thereby obtaining the allyl-containing trifunctional benzoxazine monomer, physically blending the allyl-containing trifunctional benzoxazine monomer and a dithiol compound according to a molar ratio at room temperature, and after uniformly mixing, heating, curing, copolymerizing and crosslinking to obtain the high-temperature-resistant high-crosslinking thermosetting resin. The curing temperature of benzoxazine is reduced by introducing dithiol, so that the processability of the resin is improved, propenyl in benzoxazine and mercaptan are subjected to further crosslinking under the mercaptan-alkene reaction, the crosslinking density of the thermosetting resin material is improved, the cured novel crosslinking material has more excellent thermodynamics and mechanical properties, and the flame retardant property is further improved.

Description

technical field [0001] The invention relates to the technical field of thermosetting resins, in particular to a high-temperature-resistant high-crosslinking thermosetting resin system and a preparation method thereof. Background technique [0002] Benzoxazine is a new type of thermosetting resin with six-membered heterocyclic rings composed of O and N atoms developed based on traditional phenolic resins. Benzoxazine resin can undergo ring-opening self-polymerization or copolymerization with epoxy resins under the condition of heating without a catalyst to form a three-dimensional network cross-linked structure. No small molecules are generated during its curing process, and the volume shrinkage rate is close to zero. It overcomes the disadvantages of poor dimensional stability of traditional phenolic resins, and has high glass transition temperature and thermal stability, as well as excellent flame retardancy and mechanical properties. In actual industrial production, acco...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G75/045C08G75/0227
CPCC08G75/045C08G75/0227
Inventor 谢富平张侃
Owner 镇江利德尔复合材料有限公司
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