A kind of high thermal conductivity polyimide thermosetting resin containing aromatic ester structure and preparation method thereof

A high thermal conductivity, thermosetting technology, applied in the field of thermosetting resins, can solve the problems of decreased comprehensive performance, poor compatibility and good flame retardancy of materials, and achieve the effect of excellent mechanical

Active Publication Date: 2021-11-23
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the compatibility between additive flame retardants and epoxy resins is generally poor, and the introduction of chemical weak bonds will also reduce the overall performance of materials.
[0004] Existing thermosetting resins are still difficult to meet the requirements of high thermal conductivity, high heat-resistant temperature, good flame retardancy, and easy recycling.

Method used

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  • A kind of high thermal conductivity polyimide thermosetting resin containing aromatic ester structure and preparation method thereof
  • A kind of high thermal conductivity polyimide thermosetting resin containing aromatic ester structure and preparation method thereof
  • A kind of high thermal conductivity polyimide thermosetting resin containing aromatic ester structure and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Add 45mmol of 2,2-bis[4-(4-aminophenoxy)phenyl]propane to 120ml of N-methylpyrrolidone solvent, and dropwise add 22.5 mmol 4-formylphenyl 4-formylbenzoate, keep stirring for 1h, then add 15mmol tris[(4-formylphenoxy)-methyl]ethane dissolved in 100ml N-methylpyrrolidone, continue After reacting for 1 hour, the reaction pre-polymerization solution was coated on a horizontal glass plate, and dried at 120°C for 12 hours to obtain a sheet-like material. Laminate multiple sheets of sheet material into a mold for hot pressing under the conditions of 230°C and 3MPa to obtain polyimide resin target products of different thicknesses ( figure 1 ). The tensile strength, Young's modulus and elongation at break of the resin are 92Mpa, 3.5Gpa and 7.9% respectively, and the bending strength and modulus reach 106MPa and 3.2Gpa respectively. The glass transition temperature is 232°C, the 5wt% thermal decomposition temperature is 435°C, and the thermal conductivity is 0.43W / (m·K). The...

Embodiment 2

[0041]Add 45mmol p-phenylenediamine to 120ml N,N-dimethylacetamide solvent, add dropwise 22.5mmol 4-formylbenzoic acid 4 dissolved in 100ml N,N-dimethylacetamide at 60°C -Formylphenyl ester, keep stirring for 1h, then add 15mmol tris[(4-formylphenoxy)-methyl]propane dissolved in 100ml N,N-dimethylacetamide, continue the reaction for 1h, and then The reaction solution was poured into water, filtered, and dried to obtain an orange-yellow solid. The obtained solid is put into a mold and carried out hot pressing, the condition is 250 ℃, 4MPa, obtains polyimide resin target product ( image 3 ). The tensile strength, Young's modulus and elongation at break of the resin are 96Mpa, 3.8Gpa and 4.6% respectively, and the bending strength and modulus reach 103MPa and 3.3Gpa respectively. The glass transition temperature is 243°C, the 5wt% thermal decomposition temperature is 435°C, and the thermal conductivity is 0.46W / (m·K). The flame retardant level reaches UL94 V-0 (1.6mm) level. ...

Embodiment 3

[0044] Add 45 mmol of 4-aminophenyl 4-aminobenzoate to 120 ml of dimethyl sulfoxide solvent, and add 30 mmol of tris[(4-formylphenoxy) dissolved in 100 ml of dimethyl sulfoxide at 60°C -Methyl]ethane, react for 1 hour, then apply the reaction pre-polymerization solution on a horizontal glass plate, and dry it at 120°C for 12 hours to obtain a sheet-like material. A plurality of sheets of sheet materials are stacked and put into a mold for hot pressing under the conditions of 240°C and 3MPa to obtain the target product of polyimide resin ( Figure 4 ). The tensile strength, Young's modulus and elongation at break of the resin are 104Mpa, 4.0Gpa and 3.2% respectively, and the bending strength and modulus reach 112MPa and 3.7Gpa respectively. The glass transition temperature is 246°C, the 5wt% thermal decomposition temperature is 440°C, and the thermal conductivity is 0.37W / (m·K). The flame retardant level reaches UL94 V-0 (1.6mm) level. The prepared resin was placed in 50ml o...

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Abstract

The invention discloses a high thermal conductivity polyimide thermosetting resin containing an aromatic ester structure and a preparation method thereof. The preparation method comprises the steps of: 1) dissolving a difunctional aromatic amine and a difunctional aromatic aldehyde in an organic solvent; Stir and react at 20-100°C for 0.05-3 hours, then add a cross-linking agent and continue the reaction for 0.05-5 hours to obtain prepolymer precipitation or prepolymer solution; After the solution is dried, it is put into a mold, and hot-pressed at 150-250°C and 1-20 MPa to obtain a thermosetting resin, whose structural characteristics are as shown in formula Ⅰ, where R 1 , R 2 , R 3 It is an aromatic structure containing a benzene ring. The thermosetting resin of the present invention is a polyimide containing an aromatic ester structure, has excellent thermal conductivity, machinery, heat resistance and flame retardancy, and has a simple preparation process and an adjustable structure. The prepared resin can be recycled and reused, and has broad application potential. Application prospect.

Description

technical field [0001] The invention relates to the field of thermosetting resins, in particular to a high thermal conductivity polyimide thermosetting resin containing an aromatic ester structure and a preparation method thereof. Background technique [0002] Thermosetting resins and their composite materials have been widely used in high-tech fields such as aerospace, transportation, and electronic packaging. With the development of products, the demand for light weight and miniaturization of scientific and technological products is increasing day by day. It has become a trend for polymer components to replace metal components, which requires more effective solutions to heat dissipation, flammability, thermal stability and other issues. Compared with thermoplastic resins, traditional thermosetting resins are insoluble and insoluble once cured and formed, and cannot be remolded or recycled, making their composite materials difficult to recycle. [0003] In addition, ordina...

Claims

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Application Information

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Patent Type & AuthorityPatents(China)
IPC IPC(8): C08G12/08C08L61/22
CPCC08G12/08C08L61/22
Inventor袁彦超陆信航赵建青刘述梅
OwnerSOUTH CHINA UNIV OF TECH