Halogen-free and flame-retardant composite polyimide foam material and preparation method thereof

A foam material and polyimide technology, applied in the field of low-density halogen-free composite flame-retardant polyimide foam material and its preparation, can solve the problems of low density, insufficient structure and use performance, etc.

Active Publication Date: 2017-10-24
TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The foam material has the characteristics of low density, uniform cell size distribution, excellent mechanical properties and flame-retardant properties, and well overcomes the problems of insufficient structure and service performance in polyimide products prepared by the prior art.

Method used

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  • Halogen-free and flame-retardant composite polyimide foam material and preparation method thereof
  • Halogen-free and flame-retardant composite polyimide foam material and preparation method thereof
  • Halogen-free and flame-retardant composite polyimide foam material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] (1) Graphite and red phosphorus prepare a halogen-free composite flame retardant with a weight ratio of 1:0.5; the specific preparation process is as follows:

[0057] Put 6.67g of expanded graphite, 3.33g of elemental red phosphorus and 200g of steel balls with a diameter of 6mm into a 100mL steel sealed tank, vacuumize the sealed tank, and carry out ball milling at a ball milling speed of 480rpm for 48 hours. The obtained black powder is It is a halogen-free composite flame retardant;

[0058] (2) Heat 100 parts of BTDA and 100 parts of DMF to 100°C and disperse evenly, add 15 parts of methanol to reflux at 70°C for esterification for 0.5h to obtain a clear solution A;

[0059] (3) Disperse 10 parts of deionized water, 15 parts of foam stabilizer and 5 parts of composite catalyst in the clarified solution A in step (2) at 60°C, and then add 5 parts of halogen-free composite flame retardant to obtain a uniform Suspension B;

[0060] (4) 200 parts of PAPI are quickly ...

Embodiment 2

[0064] (1) Graphite and red phosphorus prepare a halogen-free composite flame retardant with a weight ratio of 1:1; the specific preparation process is as follows:

[0065] Put 5g of expanded graphite, 5g of elemental red phosphorus and 200g of steel balls with a diameter of 6mm into a 100mL steel airtight tank, vacuumize the inside of the airtight tank, and perform ball milling at a ball milling speed of 480rpm for 48 hours to obtain a black powder that is Halogen compound flame retardant;

[0066] (2) Heat 100 parts of BTDA and 100 parts of DMF to 100°C and disperse evenly, add 15 parts of methanol to reflux at 70°C for esterification for 0.5h to obtain a clear solution A;

[0067] (3) Disperse 10 parts of deionized water, 15 parts of foam stabilizer and 5 parts of composite catalyst in the clarified solution A in step (2) at 60°C, and then add 5 parts of halogen-free composite flame retardant to obtain a uniform Suspension B;

[0068] (4) 200 parts of PAPI are quickly add...

Embodiment 3

[0072] (1) Graphite and red phosphorus prepare a halogen-free composite flame retardant with a weight ratio of 1:1.5; the specific preparation process is as follows:

[0073] Put 4g of expanded graphite, 6g of elemental red phosphorus and 200g of steel balls with a diameter of 6mm into a 100mL steel airtight tank, vacuumize the inside of the airtight tank, and perform ball milling at a ball milling speed of 480rpm for 48 hours to obtain a black powder that is Halogen compound flame retardant;

[0074] (2) Heat 100 parts of BTDA and 200 parts of DMF to 90°C and disperse evenly, add 15 parts of methanol to reflux at 70°C for esterification for 0.5h, and obtain a clear solution A;

[0075] (3) Disperse 15 parts of deionized water, 15 parts of foam stabilizer and 5 parts of composite catalyst in the clarified solution A in step (2) at 60°C, and then add 6 parts of halogen-free composite flame retardant to obtain a uniform Suspension B;

[0076](4) 150 parts of PAPI are quickly a...

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Abstract

The invention discloses a halogen-free and flame-retardant composite polyimide foam material and a preparation method thereof. The foam material is prepared from raw materials in parts by weight as follows: 100 parts of aromatic dianhydride, 50-500 parts of a polar solvent, 5-30 parts of fatty alcohol, 5-20 parts of deionized water, 15 parts of a foam stabilizer, 5 parts of a composite catalyst, 4-100 parts of a halogen-free composite flame retardant and 100-500 parts of polyisocyanate. The preparation method comprises the steps as follows: aromatic dianhydride is heated in the polar solvent to react with fatty alcohol; the deionized water, the foam stabilizer, the composite catalyst and the halogen-free composite flame retardant are added, and a suspension is obtained; finally, polyisocyanate is added, foaming and vacuum heating curing are performed, and the flame-retardant polyimide foam material is obtained finally. The prepared foam material has the characteristics of low density, uniform pore size distribution, excellent mechanical property, heat resistance and flame-retardant and smoke-suppression performance and the like, and the requirement for the polyimide foam material used in aerospace, navigation and other high-end fields can be met.

Description

technical field [0001] The invention relates to the technical field of polymer materials, in particular to a low-density halogen-free composite flame-retardant polyimide foam material and a preparation method thereof. Background technique [0002] Polyimide is by far the polymer material with the highest heat resistance level in the industrial field. It can also withstand extremely low temperatures and has excellent mechanical properties. Polyimide has excellent foaming performance, adjustable density, radiation resistance, flame resistance, low smoke performance, and no harmful gas release. Polyimide foam materials are increasingly used in key materials such as heat insulation, shock absorption and noise reduction, and insulation in high-tech fields such as aerospace, ocean transportation, national defense, and microelectronics. [0003] The polyimide foam prepared by the powder foaming method has excellent comprehensive properties, but the preparation process is complicat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/10C08K7/24C08K3/02
CPCC08G73/1035C08K3/02C08K7/24C08K2003/026C08G2110/005
Inventor 耿建新许林利黄勇
Owner TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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