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Technique for synthesizing boron-containing thermoplastic phenol formaldehyde resin by solvothermal process

A phenolic resin and solvothermal technology, applied in the field of synthesizing phenolic resin, can solve the problems of increasing the viscosity of the system, being difficult to form, restricting the production and application of boron-containing phenolic resin, and achieving the effects of good thermal stability and good heat resistance.

Active Publication Date: 2015-02-25
XI AN JIAOTONG UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The main problems in the synthesis process are: 1. the borate structure, especially the aryl borate structure, is difficult to form when there is water or alcohol, resulting in low boron content in the resin, and the synthesis process of the resin is complicated; 2. in the resin During the synthesis process, the formation of borate ester structure will significantly increase the viscosity of the system, and even lead to resin gel
These deficiencies seriously limit the production and application of boron-containing phenolic resins, especially when synthesizing boron-containing thermoplastic phenolic resins (CN201310476899.X), the above-mentioned deficiencies are more obvious

Method used

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  • Technique for synthesizing boron-containing thermoplastic phenol formaldehyde resin by solvothermal process

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Effect test

Embodiment 1

[0034] 100g of random thermoplastic phenolic resin, 10g of 4-hydroxymethylbenzeneboronic acid and 1g of oxalic acid are added into a solvothermal reactor with a volume of 500mL, and then 100g of solvent is added to the solvent reactor, and after stirring, a milky white suspension is obtained; The thermal reaction kettle was sealed, and the reaction product was obtained after being kept at 140° C. for 3 hours. Naturally cool the solvothermal reactor to reduce pressure, and then open the reactor after cooling to room temperature to obtain a viscous and transparent liquid, which is light yellow in color; dry the above-mentioned light yellow viscous liquid at 70°C and -0.08MPa for 4 hours Finally, a white block is obtained, and a boron-containing thermoplastic phenolic resin is obtained after grinding; wherein, the solvent is formed by mixing absolute ethanol and deionized water with a mass ratio of 1:0.11.

[0035] The content of free phenol in the synthesized boron-containing th...

Embodiment 2

[0037] Add 100g of high-ortho thermoplastic phenolic resin, 20g of 2-hydroxymethylphenylboronic acid monoester and 2g of oxalic acid into a solvothermal reaction kettle with a volume of 500mL, then add 100g of solvent to the solvent reaction kettle, and obtain a milky white suspension after stirring liquid; seal the solvothermal reaction kettle, and keep the temperature at 160°C for 2 hours to obtain the reaction product. Naturally cool the solvothermal reactor to reduce pressure, and then open the reactor after cooling to room temperature to obtain a viscous and transparent liquid, which is light yellow in color; dry the above-mentioned light yellow viscous liquid at 80°C and -0.08MPa for 1 hour Finally, a white block is obtained, and a boron-containing thermoplastic phenolic resin is obtained after grinding; wherein, the solvent is composed of absolute ethanol and deionized water with a mass ratio of 1:0.25.

[0038] The content of free phenol in the synthesized boron-contai...

Embodiment 3

[0040] Add 100g of bisphenol A type thermoplastic phenolic resin, 5g of 5-hydroxymethylpyridine-3-boronic acid and 0.5g of oxalic acid into a solvothermal reactor with a volume of 500mL, then add 60g of solvent to the solvent reactor, and after stirring A milky white suspension was obtained; the solvothermal reaction kettle was sealed and kept at 120° C. for 6 hours to obtain a reaction product. Naturally cool the solvothermal reactor to reduce pressure, and then open the reactor after cooling to room temperature to obtain a viscous and transparent liquid, which is light yellow; dry the above-mentioned light yellow viscous liquid at 60°C and -0.08MPa for 6 hours Finally, a white block is obtained, and a boron-containing thermoplastic phenolic resin is obtained after grinding; wherein, the solvent is anhydrous ethanol and deionized water with a mass ratio of 1:0.7.

[0041] The content of free bisphenol A in the synthesized boron-containing thermoplastic phenolic resin is 0.27%...

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Abstract

The invention relates to a technique for synthesizing a boron-containing thermoplastic phenol formaldehyde resin by a solvothermal process, which comprises the following steps: adding a thermoplastic phenol formaldehyde resin, a boron-containing compound, oxalic acid and a solvent into a solvothermal reaction kettle, sealing, heating to 120-160 DEG C, keeping the temperature for 0.5-6 hours, cooling to room temperature, and removing the solvent contained in the product, thereby obtaining the boron-containing thermoplastic phenol formaldehyde resin, wherein the boron-containing compound uses an aromatic ring structure as the parent nucleus and hydroxymethyl and boron-containing structure as the substituent group of the aromatic ring structure, and the solvent is water or an alcohol solvent or a mixture of an alcohol solvent and water in a mass ratio of 1:(0.05-0.7). The method has the advantages of high raw material conversion rate and simple technical process; and the obtained product has the advantages of uniform molecular weight distribution and favorable heat resistance. Since the conversion rate of various raw materials is higher, the residual micromolecules do not need to be removed by water washing, thereby effectively reducing the sewage discharge.

Description

technical field [0001] The invention relates to a process for synthesizing phenolic resin, in particular to a process for synthesizing boron-containing thermoplastic phenolic resin through a solvothermal method. technical background [0002] Phenolic resin is one of the earliest artificially synthesized resins. It is widely used in construction, manufacturing and aerospace industries due to its easy-to-obtain raw materials, convenient synthesis, good mechanical properties, heat resistance and outstanding high-temperature ablation resistance. and other fields. Compared with thermosetting phenolic resins, thermoplastic phenolic resins have the advantages of low free phenol content, long storage period, low curing temperature and fast curing. However, the existing thermoplastic phenolic resins still have deficiencies in the process of use, and the main deficiencies are reflected in the ablation resistance, especially the thermal decomposition temperature and char formation rat...

Claims

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Application Information

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IPC IPC(8): C08G8/28
Inventor 井新利王勇王淑娟辜朝辉
Owner XI AN JIAOTONG UNIV
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