Method for preparing bisphenol-A liquid epoxy resin

A technology of liquid epoxy resin and bisphenol, which is applied in the field of polymer preparation, can solve the problems of no monitoring method given, no in-depth discussion of etherification reaction conditions, resin epoxy value, etc.

Active Publication Date: 2009-12-30
CHINA PETROCHEMICAL CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The U.S. Patent No. 4582892 points out that with bisphenol A and epichlorohydrin (the molar ratio is 1: 9.85) in the presence of phase transfer catalyst to synthesize epoxy resin, the phase transfer catalyst is benzyltrimethylammonium chloride , the etherification reaction temperature is 55°C, the etherification reaction is stopped when the conversion rate of bispheno...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Add bisphenol A and epichlorohydrin into a four-necked flask at a monomer molar ratio of 1:8, stir under nitrogen protection to completely dissolve bisphenol A in epichlorohydrin, and add tetramethyl bromide after heating up to 70°C ammonium chloride (mass fraction is 5‰ of bisphenol A), and etherification reaction at constant temperature for 150 minutes under the protection of nitrogen. After the etherification reaction is completed, remove the nitrogen filling device, carry out decompression and vacuum pumping, keep the vacuum degree of the system at 0.095, stabilize the system temperature at 60-62°C, add NaOH aqueous solution (50% by mass fraction of NaOH, and the Ratio is 2.1: 1), and the dropwise addition time is 3 hours. After adding alkali, continue to maintain the reaction until the temperature of the system drops below 40° C. to stop the reaction.

[0017] In the post-treatment, first use a rotary evaporator to remove unreacted epichlorohydrin, the solid conten...

Embodiment 2

[0019] Add bisphenol A and epichlorohydrin into a four-necked flask according to the monomer molar ratio of 1:12, stir under nitrogen protection to completely dissolve bisphenol A in epichlorohydrin, and add tetramethyl bromide after heating up to 70°C Ammonium chloride (mass fraction is 7‰ of bisphenol A), and etherification reaction at constant temperature for 180 minutes under the protection of nitrogen. After the etherification reaction is completed, remove the nitrogen filling device, carry out decompression and vacuum pumping, so that the vacuum degree of the system is maintained at about 0.095, and when the system temperature is stable at 60 ° C ~ 62 ° C, start to drop NaOH with a mass fraction of 50%, which is mixed with bisphenol A. The molar ratio is 2.1:1, and the dropping time is 3 hours. After the alkali addition is completed, continue to maintain the reaction until the system temperature drops below 40°C to stop the reaction.

[0020] In the post-treatment, first...

Embodiment 3

[0022] Add bisphenol A and epichlorohydrin into a four-necked flask according to the monomer molar ratio of 1:6, stir under nitrogen protection to completely dissolve bisphenol A in epichlorohydrin, and add tetramethyl bromide after heating up to 70°C Ammonium chloride (mass fraction is 8‰ of bisphenol A), and etherification reaction at constant temperature for 240 minutes under the protection of nitrogen. After the etherification reaction is completed, remove the nitrogen filling device, carry out decompression and vacuum pumping, so that the vacuum degree of the system is maintained at about 0.095, and when the system temperature is stable at 60-62 ° C, start to drop NaOH aqueous solution (NaOH mass fraction 35%, mixed with bisphenol The molar ratio of A is 1.98:1), and the time for adding the base is 3 hours. After adding the alkali, continue to maintain the reaction until the temperature of the system drops below 40° C. to stop the reaction.

[0023] In the post-treatment,...

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PUM

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Abstract

The invention relates to a method for preparing bisphenol-A liquid epoxy resin, and belongs to the field of high polymer preparation. The method comprises the following steps: 1) adding a quaternary ammonium salt phase-transfer catalyst, and performing etherification at a temperature of between 70 and 85 DEG C for 45 to 240 minutes; 2) at a constant temperature of between 60 and 70DEG C, droppingalkali by NaOH aqueous solution for 1.5 to 4 hours, keeping epoxy chloropropane refluxing in the alkali dropping period, and discharging water out of a reaction system; and 3) separating unreacted epoxy chloropropane by a rotary evaporator at a temperature of 135DEG C, dissolving a mixture of resin and salt, removing solid salt by a filter, washing the resin for 3 to 5 times by water, separating solvent, and obtaining the final product. The prepared epoxy resin has the epoxy value between 0.55 and 0.56 through titration by hydrochloric acid acetone solution, low viscosity (between 7,000 and 10,000mPas), and the epoxy index between 0.595 and 0.622 through infrared spectroscopic analysis, and comprises 91 to 92 percent of micro molecular epoxy resin.

Description

Technical field: [0001] The invention belongs to the field of polymer preparation, in particular to a method for preparing bisphenol A liquid epoxy resin. Background technique: [0002] Bisphenol A type epoxy resin, as the most common representative variety of epoxy resin, has many excellent characteristics, such as high bonding strength, wide bonding surface, low shrinkage, good stability and electrical insulation, etc. The epoxy group is the characteristic group of epoxy resin, and its content is the most important index of this resin. [0003] Patent No. CN1544502A pointed out that at a temperature of 40-50°C, bisphenol A, epichlorohydrin and a small amount of NaOH aqueous solution were pre-reacted for 150-240 minutes, and then the pre-reacted materials were fed into the reactor, At a temperature of ~70°C and a vacuum with an absolute pressure of 20-30KPa, NaOH aqueous solution is added at a certain flow rate to carry out the reaction. The water and epichlorohydrin steam...

Claims

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Application Information

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IPC IPC(8): C08G59/06
Inventor 程珏宁研唐光斌刘岳辉喻林庄宏清
Owner CHINA PETROCHEMICAL CORP
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