Silicon/boron-modified phenolic resin and preparation method thereof

A technology of phenolic resin and silicon modification, which is applied in the field of silicon-boron modified phenolic resin and its preparation, can solve the problems of high cost, complicated preparation process, and no control of the dispersion state of modified components, so as to achieve controllable process and step-by-step Simple, scalable effects

Active Publication Date: 2016-09-28
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method adds a silane coupling agent to modify the silica, which increases the compatibility, but the preparation process is complicated and the cost is high
[0007] As far as the above-mentioned technology and other current publicly reported data are concerned, the dispersion state of the modified component in the resin is not controlled.
For silicon-boron modified resins, the microscopic phase state of the modified components is closely related to the high-temperature performance of the resin. The key technical problem is how to obtain good high-temperature oxidation resistance by controlling the dispersion state of the modified components in the resin. still not well resolved

Method used

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  • Silicon/boron-modified phenolic resin and preparation method thereof
  • Silicon/boron-modified phenolic resin and preparation method thereof
  • Silicon/boron-modified phenolic resin and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0063] Preparation of silicon-boron modified phenolic resin with methyltrimethoxysilane (MTMS) and silicon-modified phenolic resin with phenolic resin hydroxyl molar ratio of 1 blended with 5 wt% boric acid. Marked as 100MSN5BA.

[0064] (1) Add 103.0g novolac (polymerization degree 3-6) and 136g MTMS (1mol) into a 500mL three-neck flask, stir at 80°C to dissolve the novolak in MTMS to form a uniform mixed solution, then Add 1.03g of catalyst glacial acetic acid, stir and heat up to 90°C, react for 18h, then heat up to 130°C, distill under reduced pressure for 20min, remove by-product methanol and residual MTMS, and obtain silicon-modified phenolic resin.

[0065] (2) silicon-modified phenolic resin is dissolved in dehydrated alcohol and is made into the solution that solid contains is 60%, adds the boric acid of silicon-modified phenolic resin quality 5% and the hexamethylenetetramine (HMTA) of 10%, 30 °C, mix and stir evenly, and dry the obtained homogeneous solution in a v...

Embodiment 2

[0067] Preparation of silicon-boron modified phenolic resin with methyltrimethoxysilane and phenolic resin hydroxyl molar ratio of 1 silicon-modified phenolic resin blended with 7wt% boric acid. Marked as 100MSN7BA.

[0068] (1) Add 103.0g novolac (polymerization degree 3-6) and 136.0g MTMS (1mol) into a 500mL three-necked flask, stir at 80°C to dissolve the novolak in MTMS to form a uniform mixed solution, Then add 0.515g of catalyst glacial acetic acid, stir and raise the temperature to 110°C, react for 20h, then raise the temperature to 120°C, distill under reduced pressure for 25min, remove the by-product methanol and residual MTMS, and obtain the synthesized silicon-modified phenolic resin.

[0069] (2) Silicon-modified phenolic formaldehyde is dissolved in tetrahydrofuran (THF), and solid content is 65%, and boric acid and 10% HMTA of silicon-modified phenolic resin quality 7% are added, mix and stir at 40 ℃, the gained homogeneous solution is in vacuum Dry in a drying ...

Embodiment 3

[0071] Preparation of silicon boron modified phenolic resin with phenyltrimethoxysilane (PTMS) and silicon modified phenolic resin with phenolic resin hydroxyl molar ratio of 0.5 blended with 5wt% boric acid. Marked as 50PSN5BA.

[0072] (1) Add 103.0g novolac (polymerization degree 3-6) and 99.1g PTMS (0.5mol) into a 500mL three-neck flask, stir at 80°C to dissolve the novolak in PTMS to form a uniform mixed solution , then add 1.03g of catalyst triethylamine, stir and heat up to 100°C, react for 24h, and then distill under reduced pressure at 150°C for 45min to remove by-product methanol and residual PTMS to obtain a synthesized silicon-modified phenolic resin.

[0073] (2) The silicon-modified phenolic resin is dissolved in acetone with a solid content of 75%. Add 5% boric acid and 10% HMTA by the quality of the silicon-modified phenolic resin. Mix and stir evenly at 40°C. The resulting homogeneous solution is placed in a vacuum oven Dry at 50°C for 4 hours to obtain silic...

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Abstract

The invention discloses a silicon / boron-modified phenolic resin and a preparation method thereof. The preparation method comprises the following steps: (1) preparation of silicon-modified phenolic resin: adding linear phenol formaldehyde into a silane monomer, stirring to form a solution, adding a catalyst, heating to carry out esterification reaction, and carrying out reduced pressure distillation to obtain the silicon-modified phenolic resin; and (2) preparation of silicon / boron-modified phenolic resin: dissolving the silicon-modified phenolic resin in a solvent to obtain a resin solution, adding boric acid and hexamethylenetetramine, blending, and carrying out vacuum drying to obtain the silicon / boron-modified phenolic resin. The modified phenolic resin is in an island-like phase separation structure, and has obviously higher thermal oxidation stability. Besides, the preparation method has the advantages of simple steps, low cost and controllable process, and is suitable for popularization.

Description

technical field [0001] The invention belongs to the field of modified polymers, and in particular relates to a silicon-boron modified phenolic resin and a preparation method thereof. Background technique [0002] Phenolic resins are widely used as thermal insulation materials, refractory materials, adhesives, etc. Adhesives, flame retardant materials, etc., and also the most commonly used resin matrix for ablation and heat-resistant composite materials in the defense and aerospace industries. However, a large number of phenolic hydroxyl groups and methylene groups in the phenolic resin structure are easily oxidized and decomposed at high temperatures, which affects the heat resistance and oxidation resistance of the phenolic resin. In addition, the phenolic resin has low elongation and high brittleness. Therefore, pure phenolic resin can no longer meet the requirements of various fields, and more and more phenolic resins are modified. Improving the thermo-oxidative stabili...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L61/14C08K3/38C08G8/28
CPCC08G8/28C08K3/38C08K2003/387C08L2201/08C08L61/14
Inventor 赵彤李珊李昊
Owner INST OF CHEM CHINESE ACAD OF SCI
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