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Preparation method, product and application of semi-solid thermosetting phenolic resin

A phenolic resin and thermosetting technology, which is applied in the field of preparation of semi-solid thermosetting phenolic resin, achieves the effects of small product life and performance damage, easy transportation, easy process deployment and processing and molding

Active Publication Date: 2021-12-07
浙江自立高分子化工材料有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Based on this, it is necessary to address the technical problem of adding phenolic resin and hexamethylenetetramine to the preparation of existing phenolic molding compounds, and provide a method for preparing a semi-solid thermosetting phenolic resin. The semi-solid thermosetting phenolic resin prepared by the preparation method Resin does not need to add curing agent when preparing phenolic molding compound

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] (1) in the reactor that agitator, thermometer, vacuum gauge, condensation and reflux device, temperature raising and cooling device are housed, add 540 grams of phenol, 5.78g paraformaldehyde and 35.36g ammonia solution successively, wherein paraformaldehyde not only Participate in the reaction and act as a curing agent to a certain extent. Adding a small amount of paraformaldehyde is beneficial to reduce the curing temperature, improve curing efficiency, and reduce curing time. Adding too much is not conducive to the control of the reaction and increases the cost. Heat and stir to mix the raw materials evenly. When the temperature rises to 65°C, add the first batch of 30g resorcinol, and slowly raise the temperature. When the temperature rises to 73-78°C, start to add 594g of 37wt% formaldehyde solution dropwise, and carry out the second batch. One-stage reaction, the reaction in this stage is mainly the addition reaction of small molecules, the constant temperature rea...

Embodiment 2

[0043] (1) Add 540 grams of phenol, 5.78 g of paraformaldehyde and 35.36 g of ammonia solution successively in the reactor equipped with stirrer, thermometer, vacuum gauge, condensation and reflux device, heating and cooling device, heat and stir, slowly Raise the temperature, add the first batch of 30g resorcinol when the temperature rises to 65°C, slowly raise the temperature, wait for the temperature to rise to 73-78°C, start to add 594g 37wt% formaldehyde solution dropwise to carry out the first-stage reaction, this stage reacts with small molecule The addition reaction is the main one, and the constant temperature reaction time is 1.0-1.5 hours. After cooling down to 65°C, add the second batch of 30g resorcinol and 5.78g paraformaldehyde, raise the temperature to 75-78°C, and continue the constant temperature reaction for 0.5-1.0 Hour.

[0044](2) After the formaldehyde solution is added dropwise, the temperature is raised to 90°C for the second-stage reaction. In this st...

Embodiment 3

[0046] (1) Add 540 grams of phenol, 5.78 g of paraformaldehyde and 46.67 g of ammonia solution successively in the reactor equipped with stirrer, thermometer, vacuum gauge, condensation and reflux device, heating and cooling device, heat and stir, slowly Raise the temperature, add the first batch of 30g resorcinol when the temperature rises to 65°C, slowly raise the temperature, wait for the temperature to rise to 73-78°C, start to add 594g 37wt% formaldehyde solution dropwise to carry out the first-stage reaction, this stage reacts with small molecule The addition reaction is the main one, and the constant temperature reaction time is 1.0-1.5 hours. After cooling down to 65°C, add the second batch of 30g resorcinol and 5.78g paraformaldehyde, raise the temperature to 75-78°C, and continue the constant temperature reaction for 0.5-1.0 Hour.

[0047] (2) After the formaldehyde solution is added dropwise, the temperature is raised to 90°C for the second-stage reaction. In this s...

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Abstract

This application relates to a preparation method, product and application of a semi-solid thermosetting phenolic resin. The preparation method includes: 1) adding phenol, paraformaldehyde and an alkali catalyst into a reaction kettle, heating and stirring to raise the temperature to 60-70°C, adding For the first batch of resorcinol, heat up to 70-80°C and start adding aldehyde aqueous solution dropwise, and carry out the first-stage constant temperature reaction; 2) Cool down to 60-70°C, add the second batch of resorcinol and paraformaldehyde , the temperature is raised to 75-80° C., and the constant temperature reaction is continued; 3) After step 1) the aldehyde aqueous solution is added dropwise, the temperature is raised to 80-105° C. for the second-stage constant temperature reaction. The preparation method regulates the reaction trend of phenols and aldehydes through segmental temperature control, and the obtained thermosetting phenolic resin can be cured without excessive temperature, has short curing time, fast curing speed, and certain fluidity, and can be used as a precision electrical appliance. Adhesives for phenolic molding compounds required by special industries such as instruments and meters.

Description

technical field [0001] This application relates to the field of phenolic resin synthesis, in particular to a preparation method, product and application of a semi-solid thermosetting phenolic resin. Background technique [0002] The traditional phenolic molding compound manufacturing process adopts a two-step method, most of which need to add a curing agent. The two-step process uses thermoplastic phenolic resin as a binder, plus inorganic or organic fillers, curing agents, curing accelerators, lubricants, colorants and plasticizers to form phenolic molding compounds. [0003] However, since the thermoplastic phenolic resin contains no or very little methylol, it will only melt and not solidify when heated. Therefore, the curing of phenolic molding compound generally requires the addition of hexamethylenetetramine, namely urotropine, as a curing agent. When heated, hexamethylenetetramine will decompose and release a small amount of ammonia gas, most of which will volatiliz...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G8/24C08G8/10C08G8/22C08L61/06
CPCC08G8/10C08G8/22C08G8/24C08L61/06
Inventor 苏志强王金婷王富成王继满李波樊华锋
Owner 浙江自立高分子化工材料有限公司