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Preparation method of calixarene [4] modified thermosetting phenolic resin

A technology of phenolic resin and calixarene, which is applied in the field of thermosetting modification of phenolic resin and phenolic resin with chain structure, which can solve the problems of poor heat resistance and ablation resistance, limited application range of phenolic resin, low carbon residue rate of resin, etc. problems, to achieve high heat resistance, high production efficiency, high product yield and high purity

Inactive Publication Date: 2008-09-03
SICHUAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The traditional chain structure phenolic resin has relatively good reactivity and physical properties, but the disadvantage is that the stability is relatively poor, especially at high temperature, because the carbon contained in it is decomposed and the residual carbon rate of the resin is low, so its The heat resistance and ablation resistance are poor, and the device products made of traditional phenolic resin can only be used in a relatively low temperature environment, which greatly limits the application range of traditional phenolic resin

Method used

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  • Preparation method of calixarene [4] modified thermosetting phenolic resin
  • Preparation method of calixarene [4] modified thermosetting phenolic resin
  • Preparation method of calixarene [4] modified thermosetting phenolic resin

Examples

Experimental program
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Effect test

Embodiment 1

[0042]In a 500ml three-neck flask equipped with a stirrer, a thermometer, and a condenser, add 0.25 mole of resorcinol, 50ml of absolute ethanol and 50ml of concentrated hydrochloric acid with 150ml of distilled water added dropwise, and stir in a constant temperature water bath (about 20°C) , slowly dropwise add 0.25 molar concentration of 40% formaldehyde solution. After the dropwise addition of the formaldehyde solution is completed, heat up to about 80°C, and a pale yellow precipitate precipitates out. After reacting at this temperature for 6 hours, cool to room temperature, filter with suction, and wash the filter cake with a mixture of ethanol and distilled water. After the filter cake is dried, a light yellow powder can be obtained, and after methanol recrystallization, a white light yellow needle-like resorcinol-based calixarene [4] crystal can be obtained with a yield of 57.5%.

Embodiment 2

[0044] Pour 0.06 moles of p-tert-butylphenol, 0.72 moles of 37% formaldehyde solution and 0.005 moles of sodium hydroxide dissolved in a small amount of water into a 250ml three-necked flask, install a water separator and a thermometer, stir magnetically, and use electric heating The jacket is heated, and the temperature is rapidly raised to about 110°C, and the reaction is carried out at this temperature for about 2 hours. During the reaction, it was observed that water was separated, and the white transparent liquid gradually thickened into an orange-yellow viscous liquid. When the reactant was so viscous that it could not be stirred, the heating was stopped, and a yellow lump was obtained. After crushing the yellow solid, add an appropriate amount of dilute hydrochloric acid solution, stir for 1 hour, filter and wash with water until neutral. After drying the yellow powder at about 120°C for 30 minutes, transfer it into a 500mL three-necked flask equipped with a water separ...

Embodiment 3

[0046] Add 0.03 moles of aniline dissolved in 30 mL of ethanol and 0.006 moles of resorcinol-based calixarene[4] dissolved in 33 mL of ethanol into a 250 mL three-neck flask equipped with a condenser, agitator, and thermometer, stir and heat to 50 °C, Add 0.06 mol of formaldehyde solution with a concentration of 30% dropwise. After the dropwise addition, continue to heat to the reflux temperature of about 78°C. A white reddish precipitate is formed. After about 4 hours of reflux reaction, the temperature is lowered, and the white reddish precipitate can be obtained by suction filtration. Resorcinol-based calixarene [4] crystals containing an oxazine ring. After drying, it was recrystallized with methanol and chloroform, and the yield was 78%.

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Abstract

The present invention discloses one kind of calicene modified thermosetting phenolic resin and its preparation process. The calicene modified thermosetting phenolic resin is prepared with phenolic resin and resorcinol base calicene, p-tert-butyl calicene or resorcinol base calicene containing oxazine cycle. Introducing calicene into thermosetting phenolic resin can raise the high temperature carbon residue greatly and result in high heat resistance. The calicene modified thermosetting phenolic resin has carbon residue at 700 deg.c over 60 wt% and is suitable for preparing ablation resisting composite material.

Description

technical field [0001] The invention relates to the technical field of phenolic resins, more specifically, to the technical field of thermosetting modification of chain-structure phenolic resins. Background technique [0002] The traditional phenolic resin in the prior art has a chain structure and a relatively large molecular size. The traditional chain structure phenolic resin has relatively good reactivity and physical properties, but the disadvantage is that the stability is relatively poor, especially at high temperature, because the carbon contained in it is decomposed and the residual carbon rate of the resin is low, so its The heat resistance and ablation resistance are poor, and the device products made of traditional phenolic resin can only be used in a relatively low temperature environment, which greatly limits the application range of traditional phenolic resin. Contents of the invention [0003] For the deficiency that the phenolic resin of prior art exists,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G8/30C08G8/22
Inventor 雷毅沈红杨洋张敏
Owner SICHUAN UNIV
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