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A kind of method of aqueous phase catalytic synthesis methylsuccinic acid

A technology of methyl succinic acid and water phase, applied in chemical instruments and methods, ozonation to prepare carboxylic acid, physical/chemical process catalysts, etc., can solve the problems of difficult separation of catalysts, long reaction time, low yield, etc.

Active Publication Date: 2019-11-12
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Oxidation method is adopted to prepare methylsuccinic acid, but the method yield is not higher than 59%, and the reaction requires a long reaction time (60h) (JP 08-081410); the process of ester hydrolysis is complicated and the yield is low (JP07- 258149); esterification hydrogenation is another method, but the operation steps are more complicated, the cost is high, and the yield is low (CN10171169A)
Hydrogenation is a method with relatively high atom economy. At present, most reports use homogeneous catalysis methods, such as using metal complexes such as Rh, Ru, and Pd as catalysts. However, in homogeneous reactions, catalysts Difficult to separate and easier to lose active metals (J.Mol.Catal.A, 1996, 109(1), 45–50); Tetrahedron: Asymmetry 1995, 6(10) 2535-2546)
In addition, heterogeneous catalysts such as Pd / C catalyst and Ni catalyst are also reported, but all adopt organic solvents such as ethanol or THF; 102617326A; CN100412840C)
[0004] In view of the limitations in the prior art of hydrogenation of itaconic acid to methylsuccinic acid mentioned in the above documents, the present invention provides a method for the catalytic synthesis of methylsuccinic acid in aqueous phase

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Example 1: After the activated carbon carrier was ground and sieved to 100 mesh, it was placed in an oven at 120°C and dried overnight; an equal-volume impregnation method was used to prepare a ruthenium trichloride precursor impregnation solution with a concentration of 1.4 mg / ml, and the carrier was added during stirring to make It was mixed evenly, and after ultrasonic treatment, it was left to stand for 24 hours, and then dried overnight in an oven at 110°C. The loading amount of Ru is 5 wt.%.

Embodiment 2

[0022] Example 2: 0.25 g of the Ru / C catalyst prepared in Example 1 was weighed and placed in a tube furnace for reduction at a temperature of 450° C. for 3 hours. Add the reduced catalyst and 20 g of itaconic acid aqueous solution with a mass concentration of 6% into the reaction kettle, and stir to disperse evenly. After replacing the air with hydrogen gas for 3-5 times, heat to 100°C and keep a constant pressure of 3MPa. After reacting for 2 hours, take a sample for liquid chromatography analysis. The conversion rate of itaconic acid is 99%, and the selectivity of methylsuccinic acid is 99%.

Embodiment 3

[0023] Embodiment 3: According to the method in embodiment 1, activated carbon support is replaced by SiO 2 , to prepare Ru / SiO 2 . Then weigh 0.25g of the prepared Ru / SiO 2 The catalyst was reduced with hydrogen, the reduction temperature was 400°C, and the reduction time was 3h. Add the reduced catalyst and 20 g of itaconic acid aqueous solution with a mass concentration of 10% into the reaction kettle, and stir to disperse evenly. After replacing the air with hydrogen for 5 times, it was heated to 80° C. under a constant pressure of 3 MPa. After reacting for 2 hours, a sample was taken for liquid chromatography analysis. The conversion rate of itaconic acid was 98%, and the selectivity of methylsuccinic acid was 99%.

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Abstract

The invention discloses a method for synthesizing methylsuccinic acid by water phase catalysis. Methyl succinic acid is an important intermediate in organic synthesis and has a wide range of applications. The present invention adopts Ru-based catalyst to carry out catalytic hydrogenation reaction to itaconic acid to produce methylsuccinic acid in water phase and under mild reaction conditions, the conversion rate and selectivity can reach 99%, and the catalyst can be used multiple times. recycle.

Description

technical field [0001] The invention relates to the field of chemistry and chemical engineering, in particular to a method for synthesizing methylsuccinic acid by aqueous catalysis. Background technique [0002] Itaconic acid is an unsaturated organic dibasic acid, which is mainly obtained through the biological fermentation of sugar compounds; in addition, itaconic acid is also prepared from citric acid or maleic anhydride as raw materials. At present, my country is the fourth itaconic acid producer and the main itaconic acid exporter in the world after the United States, Japan, and Russia. It is estimated that the annual demand growth rate of itaconic acid will be about 10% in the next few years, and the domestic and foreign markets have broad prospects. Itaconic acid is mainly used as a synthetic monomer for unsaturated polyesters and resins. It is of great research significance to use catalytic conversion technology to develop downstream products of itaconic acid, impr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C51/36C07C55/10B01J23/46
CPCB01J23/462C07C51/36C07C55/10Y02P20/584
Inventor 于维强徐杰黄倩倩路芳苗虹
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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