Method for preparing epoxy succinate

A technology of epoxy succinate and maleic acid disodium salt, applied in the chemical field, can solve the problems of the impact of epoxy succinate production cost, severe reaction process, difficult temperature control, etc., and achieve easy control of product quality , The effect of high solid content in the product and cheap raw materials

Active Publication Date: 2015-01-07
QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In the above synthesis process of epoxy succinate, sodium hydroxide is usually used as a raw material. Sodium hydroxide is a strong basic compound. When mixed with the acidic compound maleic anhydride, a neutralization reaction occurs, generating a large amount of heat of reaction, and the reaction process is violent. , it is difficult to control the temperature during the reaction
At the same time, sodium hydroxide is the main chemical raw material of this process, and its price is relatively high, which has a great impact on the production cost of epoxy succinate

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0010] In a 500mL four-necked flask equipped with a stirrer and a reflux condenser, add 49g (0.5 moles) of maleic anhydride and 100ml of water, and slowly add about 35g of Na 2 CO 3 solid. Use a water bath to control the temperature of the system below 55°C. Use a metering pump to continuously add hydrogen peroxide aqueous solution, and add 68g of hydrogen peroxide (30% aqueous solution) within 30 minutes. At the same time, use sodium carbonate to control the pH to maintain pH = 6 to 6.5, and keep the temperature at 60 ° C for 1.5 hours to obtain epoxy succinic acid sodium. Tested by ion chromatography, the purity of epoxysuccinic acid reaches 91.64%.

Embodiment 2

[0012] In a 500mL four-necked flask equipped with a stirrer and a reflux condenser, add 49g (0.5 moles) of maleic anhydride and 100ml of water, and slowly add about 45g of Na 2 CO 3 solid. Use a water bath to control the temperature of the system below 55°C. Use a metering pump to continuously add aqueous hydrogen peroxide solution, and add 68g of hydrogen peroxide (30% aqueous solution) within 30 minutes. At the same time, use sodium carbonate to control pH = 6.5-7, and keep the temperature at 65°C for 1.5 hours to obtain sodium epoxy succinate. Tested by ion chromatography, the purity of epoxysuccinic acid reaches 92.60%.

Embodiment 3

[0014] In a 500mL four-necked flask equipped with a stirrer and a reflux condenser, add 49g (0.5 moles) of maleic anhydride and 100g of water, and slowly add about 60g of NaHCO under stirring. 3 solid. Use a water bath to control the temperature of the system below 55°C. Add 68g of hydrogen peroxide (30% aqueous solution) within 30min, while using NaHCO 3 Control pH=6~6.5, keep temperature at 60°C for 1.5h to obtain sodium epoxysuccinate. Through testing, the purity of epoxysuccinic acid reaches 90.60%.

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PUM

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Abstract

The invention relates to a method for preparing epoxy succinate, which comprises the following steps of: producing a maleic acid disodium salt by using sodium carbonate or sodium bicarbonate, water and maleic anhydride as raw materials; and under the condition of using sodium tungstate as a catalyst, synthetizing the epoxy succinate by using hydrogen peroxide as the raw material. Due to the adoption of sodium carbonate or sodium bicarbonate which is used as the raw material, the reaction process is more mild and controllable, a system is more stable to operate, the raw materials are relatively cheap, a small quantity of water is produced in the reaction process, the epoxy succinate has high solid content, and the quality of the epoxy succinate is easier to control.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a preparation method of epoxy succinate. Background technique [0002] Epoxysuccinate is an important chemical raw material and an intermediate in the synthesis of polyepoxysuccinic acid. In the study of polyepoxysuccinic acid, the part about the synthesis of epoxysuccinate is more representative of U.S. Patent No. 4,654,159. Its process route is to dissolve maleic anhydride in water, and then add sodium hydroxide to generate Sodium maleate, sodium tungstate is added as a catalyst, hydrogen peroxide is added continuously, and sodium hydroxide is used to adjust and keep the pH of the reaction process at 5-7 to synthesize sodium epoxysuccinate. In the claims of the domestic related patent CN1470493A, it is proposed to dissolve maleic anhydride in water to generate maleic acid, add sodium hydroxide aqueous solution until pH = 5-7, add a certain amount of sodiu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D303/48C07D301/12
Inventor 吴怀之李霞秦建光吴美玲
Owner QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
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