Preparation method of 4,4'-biphenol diglycidyl ether

A technology of diglycidyl ether and biphenol, which is applied in 4 fields, can solve the problems of cumbersome processing, and achieve the effects of simple reaction steps, avoiding growth, and improving yield

Active Publication Date: 2011-04-27
兰州精细化工有限责任公司
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  • Abstract
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Problems solved by technology

[0004] The traditional process for preparing 4,4'-biphenol diglycidyl ether is mainly prepared by the NaOH method, but in order to obtain a product with an epoxy equivalent close to the theoretical value, there are strict requirements on the way of adding NaOH, and in production The post-processing is quite cumbersome, which brings great disadvantages to industrial production.

Method used

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  • Preparation method of 4,4'-biphenol diglycidyl ether
  • Preparation method of 4,4'-biphenol diglycidyl ether

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Effect test

Embodiment 1

[0060] Ring-opening etherification reaction process: Add 20 grams of 4,4'-biphenol, 320 grams of epichlorohydrin, and 0.2 grams of phase transfer catalyst benzyltriethylammonium chloride into a three-necked flask with a water separator , nitrogen protection, heating up at 80°C, reacting for 5.0 hours, using high performance liquid chromatography to detect the reaction raw material 4,4'-diphenol content is less than 0.5% (mass percentage), start vacuum distillation epichlorohydrin, and finally The distillation temperature reaches 100°C and the vacuum degree is 0.075MPa.

[0061] Ring-closing reaction process: Then add 400 grams of toluene to the system, and then add 13 grams of NaOH in three times. After reacting at 80°C for 1 hour, raise the temperature to 110°C to let the toluene reflux under normal pressure, and use the lower water separator to separate continuously. The water generated by the reaction in the system is detected by high performance liquid chromatography after...

Embodiment 2

[0063] Ring-opening etherification reaction process: Add 20 grams of 4,4'-biphenol, 400 grams of epichlorohydrin, and 0.2 grams of phase transfer catalyst benzyltriethylammonium chloride into a three-necked flask with a water separator , nitrogen protection, heating up at 100°C, reacting for 3.0 hours, using high performance liquid chromatography to detect the reaction raw material 4,4'-diphenol content is less than 0.5% (mass percentage), start vacuum distillation epichlorohydrin, and finally The distillation temperature reaches 100°C and the vacuum degree is 0.075MPa.

[0064] Ring-closing reaction process: Then add 400 grams of toluene and 13 grams of NaOH to the system, react at 80°C for 1 hour, raise the temperature at 110°C to let the toluene reflux, and use the lower water separator to continuously separate the water generated by the reaction in the system. After 8 hours, it was detected by high-performance liquid chromatography, and the content of 4,4-biphenol diglycid...

Embodiment 3

[0066] Ring-opening etherification reaction process: Add 20 grams of 4,4'-biphenol, 400 grams of epichlorohydrin, and 0.2 grams of phase transfer catalyst benzyltriethylammonium chloride into a three-necked flask with a water separator , nitrogen protection, heating up at 90°C, reacting for 4.0 hours, using high performance liquid chromatography to detect the reaction raw material 4,4'-diphenol content is less than 0.5% (mass percentage), start vacuum distillation epichlorohydrin, and finally The distillation temperature reaches 115°C and the vacuum degree is 0.075MPa.

[0067] Ring-closing reaction process: Then add 400 grams of toluene and 13 grams of NaOH to the system, react at 80 ° C for 1 hour, raise the temperature at 110 ° C to let the toluene reflux and use the lower water separator to continuously separate the water generated by the reaction in the system, reaction 8 After one hour, it was detected by high-performance liquid chromatography, and the content of 4,4-bip...

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Abstract

The invention discloses a preparation method of 4,4'-biphenol diglycidyl ether. In the preparation method provided by the invention, 4,4'-biphenol and epichlorohydrin are used as raw materials to be synthesized by a two-step method under the effect of a heterogeneous catalyst. The preparation method comprises the following steps: firstly, carrying out a ring-opening etherifying reaction, then carrying out a ring-closing reaction, and in the alkalizing process, separating out water generated in the reaction by a water-separating technique, so that the reaction shifts to the right at equilibrium, and various hydrolysis secondary reactions in the system can be controlled. The product obtained by the technique has high epoxide equivalent and high yield, the technique has simple reaction steps and is convenient for posttreatment, and experimental results show that the epoxide number is 0.65-0.67, and the melting range is 159.1-160.4 DEG C.

Description

technical field [0001] The present invention provides a new raw material intermediate for high-performance thermosetting digital resin, specifically a preparation method of 4,4'-biphenol diglycidyl ether. Background technique [0002] 4,4-Biphenyldiphenol diglycidyl ether has the characteristics of good toughness, low viscosity and high filling ability, and is widely used in the fields of adhesives, powder coatings, epoxy molding compounds, etc., especially in the field of high-performance electronic plastic packaging. application prospects. [0003] Epoxy resin is a widely used thermosetting polymer material with excellent physical, mechanical and electrical properties. With the rapid development of electronic cutting-edge fields, epoxy resin is used as an electronic packaging material. Because the price of epoxy resin is relatively cheap, the molding process is simple, it is suitable for large-scale production, and its reliability is comparable to that of metal and cerami...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D303/27C07D301/26
Inventor 李春新霍利春王鹏张鹏云刘茵巨雪霞
Owner 兰州精细化工有限责任公司
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