New process for producing liquid methyl tetrahydro phthalic anhydride

A technology of methyltetrahydrophthalic anhydride and tetrahydrophthalic anhydride, which is applied in the field of producing liquid methyltetrahydrophthalic anhydride, can solve problems affecting product stability and yield, color deepening, etc., and achieve the goal of enhancing competitiveness and increasing product yield Effect

Inactive Publication Date: 2005-10-19
HENAN ACADEMY OF SCI CHEM RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the need for distillation after the isomerization reaction, and the distillation process still needs to maintain a higher temperature and a longer time, the isomerization reaction and side reactions are still going on, and as more products are distilled, the remaining The concentration of the catalyst in the part is increasing, causing the decomposition, polymerization and carbonization of the product to be more significant, seriously affecting the stability and yield of the product, and the color will also deepen

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Add 100g of solid methyltetrahydrophthalic anhydride into a 250ml three-necked flask, heat and melt, add 2.0g of concentrated sulfuric acid, heat up to 130°C, stir for 5 hours, then add 4.1g of calcium bicarbonate, continue to stir for 15 minutes, and then carry out Distill under reduced pressure to collect a stable fraction with a middle boiling point. The yield of the product is 90.4%, the chroma is 140 (platinum-cobalt color number), the viscosity is 41 mPa·s (25° C.), and there is no crystallization or solidification after standing at -15° C. for 15 days.

Embodiment 2

[0015] Add 100g of solid methyltetrahydrophthalic anhydride into a 250ml three-necked flask, heat and melt, add 0.5g of phosphoric acid, raise the temperature to 160°C, stir for 3 hours, then add 3.1g of sodium stearate, continue to stir for 15 minutes, and then carry out Distill under reduced pressure to collect a stable fraction with a middle boiling point. The yield of the product is 91.8%, the chroma is 120 (platinum-cobalt color number), the viscosity is 37mPa·s (25°C), and there is no crystallization or solidification after standing at -15°C for 15 days.

Embodiment 3

[0017] Add 59g of maleic anhydride in a 250ml three-necked flask, heat and melt, add mixed carbon five to it, react and release heat, keep the reaction temperature at 80-90°C, remove low boiling point substances under reduced pressure after the reaction is completed, add p-toluenesulfonate Add 1.5 g of acid, heat up to 150° C., stir and react for 1 hour, then add 1.1 g of sodium benzoate, continue stirring and reacting for 30 minutes, then carry out vacuum distillation to collect a fraction with a stable middle boiling point. The yield of the product is 88.5%, the chroma is 140 (platinum-cobalt color number), the viscosity is 43mPa·s (25°C), and there is no crystallization or solidification after standing at -15°C for 15 days.

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Abstract

The new process of producing liquid methyl tetrahydro phthalic anhydride uses solid methyl tetrahydro phthalic anhydride or coarse methyl tetrahydro phthalic anhydride produced with C5 mixture and maleic anhydride as material and through reaction in the presence of acid isomeric catalyst at 130-060 deg.c for 1-5 hr, further reaction after adding weak alkaline compound in the same equivalent as the acid catalyst for 15-30 min, and decompression distillation to obtain liquid methyl tetrahydro phthalic anhydride. Thus produced liquid methyl tetrahydro phthalic anhydride has high indexes of solidifying point, stability, viscosity, chroma, etc.

Description

technical field [0001] The invention relates to a new method for producing methyltetrahydrophthalic anhydride, in particular to a new method for producing liquid methyltetrahydrophthalic anhydride. Background technique [0002] Liquid methyltetrahydrophthalic anhydride is an excellent curing agent for epoxy resin. It has the characteristics of low melting point, low toxicity, low volatility, etc. It is easy to use, has high reactivity with epoxy resin, and has good miscibility. The cured epoxy resin has excellent electrical insulation and mechanical properties. In recent years, with the continuous improvement of the insulation performance and reliability requirements of the motor, electronics, and electrical industries, the application of this type of curing agent has developed rapidly and has a good market prospect. However, compared with similar imported products, domestic liquid methyl tetrahydrophthalic anhydride still has a large gap in quality, mainly reflected in dar...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/89
Inventor 赵东郭利兵张海洋杨瑞娜赵亮席振峰傅鹏飞
Owner HENAN ACADEMY OF SCI CHEM RES INST CO LTD
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