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Method for synthesizing high purity 3, 3 ', 5, 5'-tetramethyl-4, 4'-diphenol

A technology of biphenol and dimethylphenol, which is applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems that have not been effectively solved and the product purity is difficult to meet the requirements and needs of the rapid development of electronic packaging materials. And other issues

Inactive Publication Date: 2017-06-13
XIANGTAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

3,3',5,5'-tetramethyl-4,4'-diphenol is a synthetic 3,3',5,5'-tetramethyl-4,4'-biphenyldiphenol The monomer of glyceryl ether can be synthesized by oxidative coupling of 2,6-dimethylphenol into 3,3',5,5'-tetramethyl-4,4'-biphenyldiphenol. The reaction technology has not been effective yet. Solution, the purity of its products is also difficult to meet the requirements and needs of the rapid development of electronic packaging materials in the microelectronics industry

Method used

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  • Method for synthesizing high purity 3, 3 ', 5, 5'-tetramethyl-4, 4'-diphenol
  • Method for synthesizing high purity 3, 3 ', 5, 5'-tetramethyl-4, 4'-diphenol

Examples

Experimental program
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Effect test

Embodiment 1

[0025] Example 1 Add 0.05g of anionic surfactant compounded with sodium dodecyl sulfonate and sodium dodecylbenzene sulfonate with a mass ratio of 1:1 and 180ml of deionized water into a thermometer and agitator. In the three-necked flask, slowly raise the temperature to 50°C under stirring to form an emulsion, then add borax to adjust the pH value of the emulsion to 9, then slowly add 12.20 g of the reaction raw material 2,6-dimethylphenol under stirring, and use 2 L / (min*L reaction liquid) gas velocity through oxygen reaction, and at the same time, slowly raise the temperature to 80°C at a heating rate of 2°C / min, then add copper acetate and copper sulfate with a concentration of 25g / L and a mass ratio of 1:1 20ml of the compound copper salt catalyst aqueous solution, continue to react with oxygen at a gas rate of 2L / (min*L reaction solution) for 3h under stirring and constant temperature of 80°C, then stop feeding oxygen, keep stirring and constant temperature of 80°C for c...

Embodiment 2

[0026] Example 2 Add 0.10 g of anionic surfactant compounded with sodium dodecyl sulfonate and sodium dodecyl benzene sulfonate with a mass ratio of 1:1 and 180 ml of deionized water into a thermometer and agitator. In the three-necked flask, slowly raise the temperature to 50°C under stirring to form an emulsion, then add borax to adjust the pH value of the emulsion to 9, then slowly add 12.20 g of the reaction raw material 2,6-dimethylphenol under stirring, and use 2 L / (min*L reaction liquid) gas velocity through oxygen reaction, and at the same time, slowly raise the temperature to 80°C at a heating rate of 2°C / min, then add copper acetate and copper sulfate with a concentration of 25g / L and a mass ratio of 1:1 20ml of the compound copper salt catalyst aqueous solution, continue to react with oxygen at a gas rate of 2L / (min*L reaction solution) for 3h under stirring and constant temperature of 80°C, then stop feeding oxygen, keep stirring and constant temperature of 80°C fo...

Embodiment 3

[0027] Example 3 Add 0.15 g of anionic surfactant compounded with sodium dodecyl sulfonate and sodium dodecyl benzene sulfonate with a mass ratio of 1:1 and 180 ml of deionized water into a thermometer and agitator. In the three-necked flask, slowly raise the temperature to 50°C under stirring to form an emulsion, then add borax to adjust the pH value of the emulsion to 9, then slowly add 12.20 g of the reaction raw material 2,6-dimethylphenol under stirring, and use 2 L / (min*L reaction liquid) gas velocity through oxygen reaction, and at the same time, slowly raise the temperature to 80°C at a heating rate of 2°C / min, then add copper acetate and copper sulfate with a concentration of 25g / L and a mass ratio of 1:1 20ml of the compound copper salt catalyst aqueous solution, continue to react with oxygen at a gas rate of 2L / (min*L reaction solution) for 3h under stirring and constant temperature of 80°C, then stop feeding oxygen, keep stirring and constant temperature of 80°C fo...

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Abstract

The invention discloses a method for synthesizing high purity 3, 3 ', 5, 5'-tetramethyl-4, 4'-diphenol. In alkaline emulsion reaction conditions, three stages of combination reactions are performed, 2,6-dimethylphenol is oxidized and coupled into 3, 3 ', 5, 5'-tetramethyl-4, 4'-diphenol, the 3, 3 ', 5, 5'-tetramethyl-4, 4'-diphenol is cooled to form a 3, 3 ', 5, 5'-tetramethyl-4, 4'-diphenol precipitation product in alkaline emulsion, the 3, 3 ', 5, 5'-tetramethyl-4, 4'-diphenol precipitation product is filtered and washed with water to obtain the high purity 3, 3 ', 5, 5'-tetramethyl-4, 4'-diphenol product with the product yield of 60-70% and purity mass percent up to 99%, alkaline emulsion filtrate and water washing liquid are recycled after recovery and deployment, a copper salt catalyst is small in amount, soluble in water and easy to remove, and product quality requirements of 3, 3 ', 5, 5'-tetramethyl-4, 4'-diphenol diglycidyl ether biphenyl epoxy molding compounds in microelectronics industry can be met.

Description

technical field [0001] The invention belongs to the field of organic synthesis and relates to a method for synthesizing high-purity 3,3',5,5'-tetramethyl-4,4'-biphenyldiol. Background technique [0002] In recent years, with the rapid development of the microelectronics industry, the requirements and demands for electronic packaging materials have been increasing, and the plastic packaging materials have accounted for about 95% of the entire packaging materials, especially the epoxy plastic packaging materials with high reliability, low production cost, and high technology. It is simple and suitable for mass production, and its use accounts for about 90% of the plastic packaging compound. 3,3',5,5'-Tetramethyl-4,4'-biphenyldiol diglycidyl ether is a kind of biphenyl type epoxy resin, because it contains biphenyl structure, its biphenyl skeleton makes epoxy The resin has high toughness, and the special dihydroxy functional group improves its heat resistance and has better in...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C37/11C07C37/07C07C37/68C07C37/70C07C39/15
CPCC07C37/11C07C37/07C07C37/685C07C37/70C07C39/15
Inventor 刘跃进徐文质吴志明李胜国伍巍韩嫣江晓蓉
Owner XIANGTAN UNIV
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