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Refining method of bisphenol A epoxy resin

A refining method and epoxy resin technology, applied in the field of epoxy resin purification, can solve the problems of shortening the service life, difficult to remove co-catalysts, affecting the insulation performance of insulating parts, long-term stability of aging performance, etc., to achieve insulation performance and aging performance. Excellent, reduce the content of hydrolyzable chlorine, and ensure the effect of long-term safe operation

Active Publication Date: 2020-11-20
HEFEI UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The purity of epoxy resin mainly affects its operating life and reliability under actual operating conditions. In the presence of oxygen, moisture, etc., the hydrolyzable chloride ions in epoxy resin will precipitate, and the insulating parts will be accelerated under the action of moisture. Corrosion of the insert affects the performance of the insulation and shortens its service life
[0003]Because the conversion rate of chemical reaction is difficult to reach 100%, it is difficult to remove all organic chlorine in the reaction process of preparing bisphenol A epoxy resin
At present, the problem of the hydrolyzable chlorine content of bisphenol A type epoxy resin is mainly based on the crude epoxy resin with high hydrolyzable chlorine content as raw material, which is refined by vacuum distillation, solvent extraction, crystallization separation, etc., but these The method has strict requirements on the materials of the equipment, and complex molecular distillation devices or separation equipment need to be installed, which is costly and unsuitable for large-scale industrial applications.
Therefore, bisphenol A type epoxy resin mainly adopts sodium hydroxide to carry out refining reaction in toluene solution at present, but bisphenol A type epoxy resin exists in the organic phase, sodium hydroxide exists in the water phase, and the refining reaction only exists in the water phase. The interface between phase and organic phase is actually very small, and it is difficult to reduce the content of hydrolyzable chlorine in bisphenol A epoxy resin to a large extent, which will affect the insulation performance, aging performance and long-term performance of insulating parts. stability
The Chinese patent with the publication number CN 102816295A discloses a refining process of bisphenol A liquid epoxy resin, which is to put crude epoxy resin, NaOH solution, and solvent into the reactor, and add a cocatalyst to increase the amount of NaOH The degree of reaction with the hydrolyzable chlorine on the crude resin reduces the content of hydrolyzable chlorine in the bisphenol A liquid epoxy resin, but the cocatalyst added in the refining process is difficult to remove in the washing stage after the refining reaction, resulting in epoxy resin A small amount of catalyst remains in the resin, which affects the thermal, mechanical and electrical properties of epoxy resin

Method used

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  • Refining method of bisphenol A epoxy resin

Examples

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preparation example Construction

[0028] The conventional process for the preparation of bisphenol A epoxy resin is to use bisphenol A and epichlorohydrin etherification reaction, and then undergo a ring-closing reaction to obtain the crude epoxy resin, and then refine the crude epoxy resin by a second ring-closing reaction. Finally, after purification, bisphenol A epoxy resin is obtained. Generally, when refining, since there is an organic phase in the crude epoxy resin, and there is an aqueous phase in sodium hydroxide, the refining reaction is only carried out at the interface between the aqueous phase and the organic phase. , the refining reaction is very limited, making hydrolyzable chlorine removal limited. Based on the original technology, the present invention adopts spraying and atomizing lye combined with multi-source and multi-frequency ultrasonic vibration, so as to remove the hydrolyzable chlorine in the epoxy resin to the greatest extent. It can be understood that the etherification reaction of b...

Embodiment 1

[0038] A refining method for bisphenol A type epoxy resin, comprising the following steps:

[0039] Add 224 g of crude epoxy resin, 260 mL of toluene and 50 mL of deionized water to figure 1 In the shown reactor 10;

[0040] 10.95g of NaOH solution with a mass fraction of 48.5% was added to the jet atomizer;

[0041]Turn on the jet atomizer (temperature range of high temperature tank: room temperature to 150°C, power supply: AC220V 50Hz) and turn on the reactor 10 to stir at the same time, spray and atomize the NaOH solution while stirring, and the stirring speed is 100rpm;

[0042] After the atomization of the NaOH solution is completed, adjust the temperature of the material in the reactor 10 to 75° C., and simultaneously set the stirring speed to 200 rpm;

[0043] Turn on the ultrasonic vibrating rod 102 (vibration frequencies are set to 27kHz, 35kHz, 25kHz and 40kHz in turn), perform multi-source multi-frequency ultrasonic vibration while stirring, and stop after 2 hours...

Embodiment 2

[0045] A kind of refining method of bisphenol A type epoxy resin, comprises the following steps:

[0046] Add 224 g of crude epoxy resin, 230 mL of toluene, and 38 mL of deionized water to figure 1 In the shown reactor 10;

[0047] Add 8.15g of NaOH solution with a mass fraction of 48.5% to the jet atomizer;

[0048] Turn on the jet atomizer (same as in Example 1) and simultaneously turn on the reactor 10 for stirring, and spray and atomize NaOH while stirring, and the stirring speed is 100rpm;

[0049] After the atomization of the NaOH solution is completed, adjust the temperature of the material in the reactor 10 to 85°C, and at the same time, set the stirring speed to 200rpm;

[0050] Turn on the ultrasonic vibrating rod 102 (same as in Example 1), perform multi-source multi-frequency ultrasonic vibration while stirring, and stop after reacting for 2 hours.

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Abstract

The invention discloses a refining method of bisphenol A epoxy resin, which comprises the following steps: adding crude epoxy resin, an organic solvent and deionized water into a reaction container, stirring at a rotating speed of 100-200 rpm, spraying atomized alkali liquor into the reaction system while stirring, wherein the temperature in the reaction container is adjusted to 75-95 DEG C and the stirring rotating speed is changed to 200-400 rpm, stirring and carrying out multi-source multi-frequency ultrasonic vibration reaction for at least 2 hours, and then stopping the reaction. Throughthe refining method, the content of hydrolysable chlorine in bisphenol A epoxy resin can be greatly reduced, so that the performance of the epoxy resin insulating composite material is improved.

Description

technical field [0001] The invention belongs to the technical field of epoxy resin purification, in particular to a method for refining bisphenol A epoxy resin. Background technique [0002] Epoxy resin is widely used in the power industry because of its good mechanical strength and excellent electrical insulation. It is an important insulating material for power electronic packaging devices, GIS and other equipment. The purity of epoxy resin mainly affects its operating life and reliability under actual operating conditions. In the presence of oxygen, moisture, etc., the hydrolyzable chloride ions in epoxy resin will precipitate, and the insulating parts will be accelerated under the action of moisture. Corrosion of the insert affects the performance of the insulation and shortens its service life. [0003] Since the conversion rate of the chemical reaction is difficult to reach 100%, it is difficult to remove all organic chlorine in the reaction process for preparing bisp...

Claims

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Application Information

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IPC IPC(8): C08G59/02C08G59/06
CPCC08G59/025C08G59/063
Inventor 赵玉顺闫程杨克荣白金辉豆宏利蔡进豪
Owner HEFEI UNIV OF TECH
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