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Thermoplastic phenolic resin with low bisphenol compound content as well as preparation method and application thereof

A technology of phenolic compounds and phenolic resins, applied in the field of new materials, can solve the problems of reducing the softening point and viscosity of phenolic resins, affecting the manufacturability of phenolic resins, and increasing the crosslinking density of resins, so as to achieve improved performance, excellent thermal stability, High value-added effect

Pending Publication Date: 2020-02-14
XI AN JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In fact, there will always be a considerable amount of bisphenol compounds in industrially synthesized NR, which can even reach more than 10%. These bisphenol compounds will seriously affect the processing and application of NR, mainly in the following ways: ①As a small molecular compound Acting as a plasticizer, it reduces the softening point and viscosity of phenolic resin, thereby affecting the manufacturability of phenolic resin and limiting the application range of NR; ②In order to make the bisphenol compounds in NR can participate in the reaction, more More curing agents, such as hexamethylenetetramine, but this will lead to an increase in the crosslinking density of the resin, making the toughness of the resin worse, etc.
[0005] In summary, although the thermal stability of the phenolic resin obtained through the existing synthesis or modification methods has been improved to a certain extent, the root cause of its low thermal stability, namely the influence of bisphenol compounds, has been ignored. Need a kind of new thermoplastic phenolic resin with low bisphenol compound content and preparation method thereof

Method used

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  • Thermoplastic phenolic resin with low bisphenol compound content as well as preparation method and application thereof
  • Thermoplastic phenolic resin with low bisphenol compound content as well as preparation method and application thereof
  • Thermoplastic phenolic resin with low bisphenol compound content as well as preparation method and application thereof

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preparation example Construction

[0034] The preparation method of the novolak resin with low bisphenol compound content in the embodiment of the present invention specifically includes the following steps:

[0035] The first step is the synthesis of phenolic resin:

[0036] Add phenolic compounds, aldehydes, water and acidic catalysts to the reaction kettle to obtain a mixture; specifically, it can be, in terms of mole parts, 5 to 160 parts of phenolic compounds and 0.01 to 20 parts of acidic catalysts, and phenol The molar ratio of the aldehyde compound to the aldehyde compound is 1: (0.85 to 1.3), and then it is dissolved in 200 to 1000 mL of water.

[0037] Stir and heat the mixture and reflux for 0.5-4h. After the mixture is cooled, let it stand for 0.5~2h, siphon out the upper layer of water, change the condensation to vacuum distillation, heat, and raise the temperature of the reactor to 110~130℃ under the pressure of 6~14kPa until it reaches the preset requirement Or maintain the preset reaction time to obt...

Embodiment 1

[0054] The comparative example is a phenolic resin containing a larger amount of bisphenol compounds.

[0055] According to the mass ratio of phenolic resin: extractant=1:2, add 50g of purchased phenolic resin and 100g of xylene into a four-necked flask equipped with a stirring blade and a condenser, and stir at 160℃ for 1h under a nitrogen atmosphere. , Pour out the supernatant while it is hot, complete the process of extracting bisphenol compounds once, repeat the above extraction process 5 times, and dry the solvent to obtain the novolak resin with low content of bisphenol compounds, the yield is 90%, grinding Later characterize.

[0056] See figure 1 , Using liquid chromatography to quantify the content of bisphenol in phenolic resin, liquid chromatography test conditions are: chromatographic column: C18 (2.1×50mm, 3mm); column temperature: 30℃; mobile phase: methanol: water = 38:62 Volume ratio; Flow rate: 0.4mL / min; UV detection wavelength: 270nm. The liquid chromatographic...

Embodiment 2

[0061] Add 130 g of phenol (1.38 mol), 13 mL of water, 92.4 g of 37% formaldehyde solution (1.14 mol) and 1 g of oxalic acid dihydrate into a 1000 mL reaction kettle, stir and heat the mixture, and reflux for 30 min. Add 1g of oxalic acid hydrate, continue to reflux for 1h, add 400mL of water, wait for the mixture to cool, let it stand for 30min, siphon out the upper layer of water, and change the condensation to vacuum distillation, heating, and under the pressure of 10kPa, make the kettle temperature rise At 120°C, until the requirement is reached, a novolak resin containing a larger amount of bisphenol compounds can be obtained with a yield of 103%.

[0062] According to the mass ratio of novolak resin: extractant=1:2, add 50g of synthetic phenolic resin and 100g of xylene into a four-necked flask equipped with a stirring blade and condenser, and stir at reflux temperature under an inert atmosphere For 1 h, the supernatant was poured out while it was hot to complete an extract...

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Abstract

The invention discloses thermoplastic phenolic resin with a low bisphenol compound content as well as a preparation method and application thereof. The preparation method comprises the following steps: mixing thermoplastic phenolic resin with an extractant to obtain a mixture A; in an inert atmosphere, stirring the mixture A for a preset period of time at a reflux temperature of the extractant , and pouring out the supernatant at a temperature higher than the preset temperature to obtain extracted thermoplastic phenolic resin; repeating extraction for a plurality of times; and carrying out reduced pressure distillation to remove the extractant to obtain the thermoplastic phenolic resin with a low bisphenol compound content. The preparation method disclosed by the invention is used for preparing the thermoplastic phenolic resin with an extremely low bisphenol compound content, the thermoplastic phenolic resin obtained by the preparation method has good manufacturability and excellent thermal stability, and good thermal stability and mechanical properties can be achieved by crosslinking the resin with a small amount of the curing agent.

Description

Technical field [0001] The invention belongs to the technical field of new materials, and particularly relates to a thermoplastic phenolic resin with low bisphenol compound content, and a preparation method and application thereof. Background technique [0002] Phenolic Resin (PR) is the earliest polymer material synthesized by humans. Compared with other polymer materials, PR has low raw material and production costs, excellent electrical properties, good heat resistance and chemical resistance, and product size stability Good sex and other characteristics. These characteristics make PR widely used in various fields, especially in the aerospace field. Because of its excellent ablation resistance and high-quality retention rate, PR and its composite materials are used in the application of transient high temperature and ablation structural materials. It has an important position and is the earliest and is still widely used as a matrix resin for ablation resistant composite mater...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G8/10C08G8/24C08L61/10C08L61/12
CPCC08G8/10C08G8/24C08L61/06C08L61/12
Inventor 井新利张萍王淑娟张晓婷
Owner XI AN JIAOTONG UNIV
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