Unlock instant, AI-driven research and patent intelligence for your innovation.

A kind of process of synthesizing boron-containing thermoplastic phenolic resin by solvothermal method

A technology of phenolic resin and solvothermal method, which is applied in the field of synthetic phenolic resin, can solve the problems of increasing the viscosity of the system, difficulty in forming, complex resin synthesis process, etc., and achieve the effect of good heat resistance and good thermal stability

Active Publication Date: 2017-06-27
XI AN JIAOTONG UNIV +1
View PDF3 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The main problems in the synthesis process are: 1. the borate structure, especially the aryl borate structure, is difficult to form in the presence of water or alcohol, resulting in low boron content in the resin, and the resin synthesis process 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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • A kind of process of synthesizing boron-containing thermoplastic phenolic resin by solvothermal method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] 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.

[0036] The content of free phenol in the synthesized boron-containing th...

Embodiment 2

[0038] 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.

[0039] The content of free phenol in the synthesized boron-contai...

Embodiment 3

[0041] 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.

[0042] The content of free bisphenol A in the synthesized boron-containing thermoplastic phenolic resin is 0.27%...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
softening pointaaaaaaaaaa
softening pointaaaaaaaaaa
softening pointaaaaaaaaaa
Login to View More

Abstract

A process for synthesizing boron-containing thermoplastic phenolic resin by solvothermal method, adding thermoplastic phenolic resin, boron-containing compound, oxalic acid and solvent into a solvothermal reaction kettle, sealing it and heating it to 120-160°C, keeping it warm for 0.5-6 hours and then cooling down To room temperature, the solvent contained in the obtained product is removed to obtain a boron-containing thermoplastic phenolic resin; wherein, the boron-containing compound uses an aromatic ring structure as the core, and a methylol group and a boron-containing structure as the substituent of the aromatic ring structure The compound; the solvent is water, alcoholic solvent or alcoholic solvent and water with a mass ratio of 1: (0.05-0.7). The method for synthesizing the boron-containing thermoplastic phenolic resin by the solvothermal method of the present invention has the advantages of high raw material conversion rate and simple process flow, and the obtained product has uniform molecular weight distribution and good heat resistance. Due to the high conversion rate of various raw materials, it does not need to be washed with water to remove residual small molecules, which can effectively reduce 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. [0002] technical background [0003] 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 forma...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): C08G8/28
Inventor 井新利王勇王淑娟辜朝辉
Owner XI AN JIAOTONG UNIV