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Preparation method of epoxy resin

An epoxy resin and epichlorohydrin technology, applied in the chemical industry, can solve the problems of increasing the cost of evaporating salt from saturated brine, consuming more hydrochloric acid, environmental pollution, etc., and achieving the effects of improving toughness, simple process and low energy consumption

Active Publication Date: 2017-01-25
ANHUI XINYUAN CHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Specifically, the by-products produced during the preparation of the aliphatic epoxy resin reactive diluent are mainly salt and water, and the by-products can be separated to form saturated brine and solid salt by conventional solid-liquid separation, wherein the saturated brine Recoverable industrial-grade solid salt (NaCl) is obtained by neutralization and multi-effect evaporation, but because the saturated brine contains sodium hydroxide and a certain amount of polyhydric alcohol (wherein the mass concentrations of NaOH and polyhydric alcohol are respectively 2-10%, 1-2%, COD is about 800000mg / L), so it will consume more hydrochloric acid when neutralizing it, and at the same time, the consumed hydrochloric acid will bring in more water, which will undoubtedly increase the saturation The cost of evaporating and salting salt water, and the organic matter entrained in the saturated brine after evaporating salt is discharged in the form of solid waste, which will undoubtedly pollute the environment

Method used

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  • Preparation method of epoxy resin
  • Preparation method of epoxy resin

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Embodiment 1: the preparation of epoxy resin

[0014] 1) In a 500ml four-necked flask with an electric heating mantle, agitator, and reflux condenser, add 198.4g of saturated brine (alkali content is 4.82%, COD 149940mg / L), 46.7g of NaOH solution with a mass fraction of 32%, turn on the stirrer, add 100g of bisphenol A, fully dissolve it at 40°C, and then add 52.5g of epichlorohydrin at one time for normal pressure The reaction is carried out in seven stages: 57±4°C, 15min; 70±3°C, 15min; 80±3°C, 30min; 85±3°C, 10min; 90±3°C, 10min; 95±2°C, 20min ;97±2℃, 20min, produce crude epoxy resin;

[0015] 2) The epoxy resin crude product was washed 7 times to neutrality, then dehydrated under normal pressure conditions, and then dehydrated under -0.095MPa vacuum conditions to obtain epoxy resin products with an epoxy value of 0.1298eq / 100g.

Embodiment 2

[0016] Embodiment 2: the preparation of epoxy resin

[0017] 1) In a 500ml four-neck flask with an electric heating mantle, agitator, and reflux condenser, add 237.0g of saturated brine produced during the production of benzyl glycidyl ether (the alkali content is 9.16%, and the COD is 179820mg / L) , 9.0g of NaOH solution with a mass fraction of 32%, start the stirrer, add 100g of bisphenol A, fully dissolve it at 40°C, then add 52.5g of epichlorohydrin at one time to carry out normal pressure reaction, the reaction is divided into seven Each stage: 57±4℃, 15min; 70±3℃, 15min; 80±3℃, 30min; 85±3℃, 10min; 90±3℃, 10min; 95±2℃, 20min; 97±2℃ , 20min, generate epoxy resin crude product;

[0018] 2) The crude epoxy resin product was washed 7 times to neutrality, then dehydrated under normal pressure conditions, and then dehydrated under -0.095MPa vacuum conditions to obtain epoxy resin products with an epoxy value of 0.1277eq / 100g.

Embodiment 3

[0019] Embodiment 3: the preparation of epoxy resin

[0020] 1) Add 233.5g C 12-14 Saturated brine (alkali content is 8.89%, COD is 183930mg / L) of by-product in the alkyl glycidyl ether production process, 11.7g mass fraction is the NaOH solution of 32%, open stirrer, add 100g bisphenol A, in Dissolve it fully at 40°C, then add 52.5g of epichlorohydrin at one time for normal pressure reaction, the reaction is divided into seven stages: 57±4°C, 15min; 70±3°C, 15min; 80±3°C, 30min ;85±3°C, 10min; 90±3°C, 10min; 95±2°C, 20min; 97±2°C, 20min, to produce crude epoxy resin;

[0021] 2) The crude epoxy resin product was washed 7 times to neutrality, then dehydrated under normal pressure conditions, and then dehydrated under -0.095MPa vacuum conditions to obtain epoxy resin products with an epoxy value of 0.1251eq / 100g.

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Abstract

The invention discloses a preparation method of epoxy resin; the steps are as follows: weighing bisphenol A and NaOH mixed solution which has a mass concentration of 8% to 10%; mixing and stirring until dissolving, adding epoxy chloropropane into the dissolved solution, reacting for 2 hours to 3.5 hours under the condition of 50 degrees centigrade to 100 degrees centigrade; washing to neutral, dehydrating, then obtaining the epoxy resin product; the 8% to 10% of NaOH mixed solution is prepared by NaOH solution and saturated saline containing alkali; the saturated saline containing alkali is a byproduct generated by preparing aliphatic epoxy resin active diluents. The preparation method of epoxy resin organically combines the production of epoxy resin active diluents with production of solid epoxy resins; the saturated saline containing alkali and few polyhydric alcohols which is generated in the preparation process of the aliphatic epoxy resin active diluents is completely used as a raw material for producing the solid epoxy resins, thus not only the production cost of the solid epoxy resins is saved, but also the tenacity of the solid epoxy resin products is increased; the method is simple in technology, low in energy consumption, clean in production, and has certain economical benefits and social benefits.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a preparation method of epoxy resin. Background technique [0002] Epoxy resin refers to an organic polymer compound containing two or more epoxy groups in the molecule. It can cross-link with various types of curing agents to form an insoluble and infusible three-dimensional network structure polymer. It has excellent mechanical properties, adhesive properties, electrical insulation properties and chemical resistance properties, so it is widely used in coatings, food, chemical, anti-corrosion, machinery, electronics, electrical and other fields. Among them, bisphenol A type epoxy resin is a general-purpose epoxy resin in China at present, and its production steps are: bisphenol A and epichlorohydrin generate epoxy resin crude product and by-products NaCl and H under the action of sodium hydroxide 2 O, the crude product of epoxy resin is washed and refined ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G59/06
Inventor 朱新宝王芳姚洪何云超程振朔
Owner ANHUI XINYUAN CHEM
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