O-phthalo nitrile modified high ortho phenolic resin and its preparing method

A technology of phthalonitrile and phenolic resin, applied in the field of phenolic resin, to achieve the effect of improving heat resistance and toughness, improving heat resistance and ablation resistance, and easily obtaining raw materials

Inactive Publication Date: 2007-04-11
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, because traditional phenolic resins are difficult to meet higher requirements, the modification of phenolic resins and the synthesis of new-structured phenolic resins have become a hot spot in the research of ablation-resistant materials.

Method used

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  • O-phthalo nitrile modified high ortho phenolic resin and its preparing method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Add 1.12 moles of phenol, 0.78 moles of phenolic solution (phenolic formaldehyde weight concentration 37%) and 0.02 moles of zinc acetate in a 250ml three-necked flask designed with a stirring device, a reflux condensing device and a thermometer, and reflux at about 102°C for about 4 hour, after the reaction finished, the product obtained was cooled down, then filtered, washed and dried to obtain 98.3g yellow powder high ortho phenolic resin with a yield of about 85%.

Embodiment 2

[0034] Add 1.12 moles of phenol, 0.78 moles of phenolic solution (phenolic formaldehyde weight concentration 37%) and 0.03 moles of zinc acetate into a 250ml three-necked flask designed with a stirring device, a reflux condensing device and a thermometer, and reflux at about 100°C for about 2 hour, after the reaction finished, the product obtained was cooled down, then filtered, washed and dried to obtain 96.3g yellow powder high ortho phenolic resin with a yield of about 84%.

[0035] Preparation of phthalonitrile diazonium salt solution.

[0036] Example 1

[0037] Dissolve 0.02 mole of 4-aminophthalonitrile in 20ml of sulfuric acid solution with a concentration of 70%, stir well and cool to about 5°C, and dissolve 10ml of the solution containing 0.04 mole of sodium nitrite at about 5°C within 1 hour Add dropwise to the above solution to prepare phthalonitrile diazonium salt solution.

[0038] Example 2

[0039] Dissolve 0.01 mole of 4-aminophthalonitrile in 20ml of 70% a...

Embodiment 5

[0046]Add 0.03 mole of high ortho phenolic formaldehyde into 150ml of NaOH solution with a concentration of 1mol / L and add it to a reaction kettle equipped with a stirring device and a thermometer, so that the high ortho phenolic formaldehyde is dissolved in NaOH solution, and then 0.007 mole of 4-aminophthalamide The diazonium salt solution of phthalonitrile prepared by nitrile synthesis was added dropwise to the phenolic NaOH solution while stirring within 1 hour, and the temperature was kept at about 13°C. During the dropping process, use alkaline solution to adjust the pH of the system to 8. After the dropping, use sulfuric acid solution to adjust the pH to 5 to obtain a red precipitate. After suction filtration, hot water washing and drying, the phthalonitrile-modified The high ortho-position phenolic resin, the yield is 83.7%.

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Abstract

The present invention discloses one kind of o-phthalonitrile modified high ortho phenolic resin and preparation process of high ortho phenolic resin and o-phthalonitrile diazo salt. O-phthalonitrile is introduced into synthesized high ortho phenolic resin structure to raise the carbon residue rate of the phenolic resin. O-phthalonitrile can further react with high ortho phenolic resin to improve the heat resistance and toughness and make high ortho phenolic resin suitable for use in preparing high performance ablation resisting material.

Description

technical field [0001] The invention relates to phenolic resin technology, more specifically, relates to the technology of modifying thermosetting phenolic resin by adding other compounds, and belongs to the field of thermosetting resin synthesis. Background technique [0002] Phenolic resin is one of the main varieties of thermosetting resins, which was the first to be industrialized, and has now developed into an important class of industrial resins in the world, mainly used in electronics, electrical, laminates, molding compounds, adhesives and insulating materials, etc. field. Since the 1960s, phenolic resin has been used as an instantaneous high temperature resistant and ablation material for space vehicles, missiles, rockets, and supersonic aircraft. With the rapid development of the aerospace industry, ablative materials are required to have higher heat resistance and better ablation resistance than before. However, the traditional phenol...

Claims

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Application Information

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IPC IPC(8): C08G8/28C08G8/10C08K5/22
Inventor 雷毅王海静杨洋张敏
Owner SICHUAN UNIV
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