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Synthesis method of low-molecular weight epoxy resin

A synthesis method and low molecular weight technology, applied in the direction of organic chemistry, can solve the problems of low epoxy value, large amount of waste water, high viscosity and other problems of liquid epoxy resin, and achieve fast reaction speed, extended production cycle and long reaction steps Effect

Inactive Publication Date: 2011-05-04
HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Abstract
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Problems solved by technology

[0006] The invention provides a method for synthesizing low-molecular-weight epoxy resin. The method replaces industrial potassium carbonate and sodium hydroxide with nano-potassium carbonate, and solves the problem of low epoxy value and high viscosity of the liquid epoxy resin prepared by the existing synthesis process. Problems with large volumes of process wastewater

Method used

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  • Synthesis method of low-molecular weight epoxy resin
  • Synthesis method of low-molecular weight epoxy resin
  • Synthesis method of low-molecular weight epoxy resin

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preparation example Construction

[0028] The preparation embodiment of nano potassium carbonate:

[0029] Anhydrous low-carbon alcohol, such as absolute ethanol or absolute methanol, needs to be used in the preparation of nanopotassium carbonate, and its molar ratio to potassium hydroxide is 5~50:1.

[0030] Dissolve 0.3 mole of potassium hydroxide in 300ml of absolute ethanol with stirring, filter to remove insoluble mechanical impurities, put it into the reactor, feed carbon dioxide through the gas distributor, and carry out the reaction at 30°C. The progress of the reaction was monitored by acid-base titration. After the reaction of potassium hydroxide is complete, cool to 20°C. Filter, when the liquid is close to the solid liquid level (the solid must not be drained during the filtration process), wash the solid with cold absolute ethanol quickly until the moisture in the filtrate is lower than 0.1%, and immediately transfer the solid to absolute ethanol. 36g of nano-potassium carbonate was obtained, wit...

Embodiment 1

[0034] Add 1 mole of bisphenol A, 4 moles of epichlorohydrin, 2.5 moles of nano-potassium carbonate prepared by the above method and 70 ml of absolute ethanol into the reactor, raise the temperature to 60°C, and finish the reaction after 10 minutes. The reaction liquid is recovered by atmospheric distillation first. Ethanol, then vacuum distillation reclaims excessive epichlorohydrin, finally obtains bisphenol A type colorless low molecular weight liquid epoxy resin (342 grams), the product content of n=0 is greater than 90%, and epoxy value is 0.581.

Embodiment 2

[0036] Add 1 mole of bisphenol A, 10 moles of epichlorohydrin, 4 moles of nano-potassium carbonate prepared by the above method and 70 ml of anhydrous methanol into the reactor, and react at 20°C for 60 minutes. A small amount of epichlorohydrin was recovered by distillation to finally obtain bisphenol A type colorless low molecular weight liquid epoxy resin (340 grams), the product content of n=0 was greater than 90%, and the epoxy value was 0.580.

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Abstract

The invention provides a preparation method of low-molecular weight epoxy resin. The method comprises the following steps: adding bisphenol A, epoxy chloropropane, potassium carbonate having grain size of 100-300 nanometer and solvent into a reactor for reaction; and distilling or rectifying the reaction liquid, and recycling the solvent to obtain the low-molecular weight colorless liquid bisphenol A type epoxy resin. The same effect is obtained by replacing bisphenol A with bisphenol S, bisphenol F or bisphenol fluorene to synthesize corresponding bisphenol S, bisphenol F or bisphenol fluorene type low-molecular weight epoxyresin. The method for synthesizing the low-molecular weight epoxy resin has the advantages of low reaction temperature, short reaction time, simple operation, high epoxy value of product, no production of industrial wastewater and good industrial prospect.

Description

technical field [0001] The invention relates to a synthesis method of epoxy resin, in particular to a synthesis method of low molecular weight epoxy resin. Background technique [0002] Low molecular weight epoxy resin has the smallest molecular weight among epoxy resins. It has direct application in many aspects and is also the raw material for synthetic epoxy resin. Its quality not only affects its own performance, but also affects high molecular weight epoxy resin. quality. [0003] At present, low molecular weight epoxy resins generally adopt the synthesis process of NaOH as the base: first, bisphenol A and epichlorohydrin are added to the reactor, heated to about 70°C to dissolve; then phase transfer catalysts such as quaternary ammonium salts are added, and NaOH aqueous solution is slowly added Reaction, during this process, the addition rate is strictly controlled to prevent side reactions such as the hydrolysis of epichlorohydrin. After the reaction is complete, ex...

Claims

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Application Information

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IPC IPC(8): C07D303/27C07D301/28C08G59/06
Inventor 刘守信李军章张燕南谷中芳
Owner HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY
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