Synthesis method of phenolic epoxy resin

A novolac epoxy resin and a synthesis method technology, which are applied in the field of organic synthesis and can solve the problems that the closed-ring epoxidation reaction cannot be fully carried out, cannot meet the technical requirements of high-purity novolac epoxy resin, and is easy to emulsify.

Active Publication Date: 2013-12-25
THE NORTHWEST RES INST OF CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In the prior art, JP6153317 provides a method of dissolving novolac resin and epichlorohydrin in the presence of a solvent and a PTC catalyst and adding an alkali solution to prepare a novolac epoxy resin, but in the reaction process, the system is in the PTC It is easy to emulsify under action, and the high price of PTC results in high production costs
CN101220135A provides a kind of synthetic method of novolak epoxy resin, this method uses quaternary salt catalyst, and this catalyst can remain in resin, because there is the existence of chlorine and bromine, influences the electrical property of resin cured product
CN102827348A also adopts the reaction of phenolic resin and epichlorohydrin to prepare high-purity novolac epoxy resin, but in the embodiment, a large amount of water is used as the pH regulator to generate a large amount of phenol-containing wastewater
It can be seen from the conclusions drawn that the chlorine content of the product is still very high and cannot meet the technical requirements of high-purity novolac epoxy resin
In CN101121775A, also adopt the technique of first polycondensation and then epoxidation to synthesize novolak epoxy resin, and the hydrolyzable chlorine reaches below 200ppm, but epichlorohydrin is used as the medium solvent of etherification and ring-closure reaction, which causes the consumption of epichlorohydrin to be relatively large
[0005] In the prior art, the process of polycondensation followed by epoxidation is the most used. The polycondensation process after epoxidation first prevents the closed-loop epoxidation reaction from being fully carried out due to steric hindrance, resulting in a small amount of unreacted chlorine in the final resin. Alcohol ether, which reduces the epoxy value
It will take a long time for this process to be applied to industrialization

Method used

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  • Synthesis method of phenolic epoxy resin
  • Synthesis method of phenolic epoxy resin
  • Synthesis method of phenolic epoxy resin

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0151] Embodiment 1: the synthesis of novolac epoxy resin

[0152] The implementation steps of this embodiment are as follows:

[0153] Step A: Preparation of Alkenyl Phenyl Ether

[0154] Under the conditions of normal pressure and temperature of 10°C, in an inert atmosphere of nitrogen, let the phenolic compound of formula (I), R in its formula (I) 1 , R 3 is hydrogen, R 2 It is methyl, and sodium hydroxide catalyst A is dissolved in acetone solvent A to obtain a solution containing phenol. The amount of sodium hydroxide catalyst A is 0.1% of the phenolic formula (I) phenol compound weight. The amount of acetone solvent A is 3 times of the total weight of phenol and sodium hydroxide. Then, add 3-chloropropene (II) haloalkene compound into the solution, and the molar ratio of phenol to 3-chloropropene is 1:4.5.

[0155] Next, in the presence of sodium hydroxide catalyst A at a temperature of 65°C, let 3-chloropropene react with phenol for 0.5 h, then add chloroform extr...

Embodiment 2

[0163] Embodiment 2: the synthesis of o-butyl novolac epoxy resin

[0164] The implementation steps of this embodiment are as follows:

[0165] Under the conditions of normal pressure and temperature of 82°C, in a nitrogen inert atmosphere, let 2-butylphenol formula (I) phenol compound, the R in its formula (I) 1 , R 3 is hydrogen, R 2 Be butyl, be dissolved in 2-butanone solvent A with potassium hydroxide catalyst A, obtain a kind of solution that contains 2-butylphenol, the amount of potassium hydroxide catalyst A is 2-butylphenol formula (I) phenol 10.0% by weight of compound. The amount of 2-butanone solvent A is 3.2 times of the total weight of 2-butylphenol and potassium hydroxide. Then, add 3-bromopropene formula (II) haloalkene compound into the solution, and the molar ratio of 2-butylphenol to 3-bromopropene is 1:5.6.

[0166] Next, in the presence of potassium hydroxide catalyst A at a temperature of 70°C, let 3-bromopropene react with 2-butylphenol for 10.0 h, ...

Embodiment 3

[0174] Embodiment 3: the synthesis of o-isopropyl novolac epoxy resin

[0175] The implementation steps of this embodiment are as follows:

[0176] Step A: Preparation of Alkenyl Phenyl Ether

[0177] Under the conditions of normal pressure and temperature of 65°C, in an argon inert atmosphere, let 6-isopropylphenol formula (I) phenol compound, formula (I) in R 1 is isopropyl, R 2 , R 3 It is hydrogen, and calcium hydroxide catalyst A is dissolved in 2-pentanone solvent A to obtain a solution containing 6-propophenol. The amount of calcium hydroxide catalyst A is 0.8% of 6-propophenol weight. The amount of 2-pentanone solvent A is 4.0 times of the total weight of 6-isopropylphenol and calcium hydroxide. Then, add 4-bromobutene formula (II) haloalkene compound into the solution, and the molar ratio of 6-isopropylphenol to 4-bromobutene is 1:0.5.

[0178] Next, in the presence of a calcium hydroxide catalyst A at a temperature of 24°C, let 4-bromobutene react with 6-isopro...

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Abstract

The invention relates to a synthesis method of phenolic epoxy resin with light color and low chlorine content. The method comprises steps of preparing alkenyl alkyl phenylate, preparing phenolic resin with double bonds and preparing phenolic epoxy resin, and the like. The phenolic epoxy resin prepared by the method provided by the invention can reach regulated softening point and epoxy value, and the chloridion content is lower than 20 ppm. Since molecular extraction and short path distillation technology are adopted, the volatile matter content of the obtained phenolic epoxy resin is quite low. Meanwhile, since a film evaporation-short path distillation technology is adopted, a solvent generated in the reaction process can be repeatedly used, thereby being beneficial to protecting the environment and reducing the production cost.

Description

【Technical field】 [0001] The invention belongs to the technical field of organic synthesis. More specifically, the present invention relates to a method for synthesizing light-colored novolac epoxy resin with low chlorine content. 【Background technique】 [0002] Novolac epoxy resin is a polyfunctional glycidyl ether type epoxy resin. When the softening point of the resin changes, its epoxy value basically does not change, and the melt viscosity is quite low, which endows the molding compound resin with excellent process stability. Therefore, it is widely used in the semiconductor industry as the main bonding material for packaging materials such as LSI, VLSI integrated circuits, electronic components and civilian weak products (VTR, OP). Electronic components encapsulated with high-purity resin can maintain their good electrical insulation properties even in high temperature and humid environments. As the main raw material of epoxy molding compound, novolac epoxy resin, in...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G59/02C08G16/02
Inventor 赵杨锋辛昭张玮韩肖慧
Owner THE NORTHWEST RES INST OF CHEM IND
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