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Synthesis method of 2-hydroxy-2-methylsuccinic acid without metal participation

A technique for the synthesis of methylsuccinic acid and its synthesis method, which is applied in the field of synthesis of 2-hydroxy-2-methylsuccinic acid, and can solve the problem of low efficiency, high cost and 2-hydroxy-2-methylsuccinic acid production process Complicated problems, to achieve the effect of simple process equipment requirements, mild operating conditions, and large industrial application prospects

Active Publication Date: 2022-08-02
NANCHANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The object of the invention is to solve the shortcomings of 2-hydroxy-2-methylsuccinic acid production process complexity, high cost, low efficiency, etc., the invention provides a kind of 2-hydroxy-2-methylsuccinic acid without metal participation resolve resolution

Method used

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  • Synthesis method of 2-hydroxy-2-methylsuccinic acid without metal participation

Examples

Experimental program
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Effect test

Embodiment 1

[0020] Add 0.15mmol levulinic acid, 50mg CaO, 50mg activated carbon in sequence to a 10mL high temperature and high pressure reaction kettle, seal the reaction kettle, fill with oxygen (0.5Mpa), stir and heat to 90°C for 0.5h. The reaction kettle was cooled to room temperature in an ice-water bath, and the aqueous phase was collected and detected. The conversion rate of levulinic acid was 96%, and the yield of 2-hydroxy-2-methylsuccinic acid was 89%. The product was detected by H NMR and C NMR. confirmed.

[0021] The levulinic acid conversion rate, the detection and calculation of the 2-hydroxy-2-methylsuccinic acid yield are carried out according to the following methods:

[0022] The detection instrument for the concentration of levulinic acid and 2-hydroxy-2-methylsuccinic acid is a liquid chromatograph Waters AcquityHclass (Coregel 107 chromatographic column: 7.8mm*300mm).

[0023] Calculation of levulinic acid conversion:

[0024] Conversion rate of levulinic acid=(1-l...

Embodiment 2

[0028] Add 0.75mmol levulinic acid, 250mg CaO, 250mg activated carbon powder in sequence to a 50mL high temperature and high pressure reaction kettle, seal the reaction kettle, fill with oxygen (0.5Mpa), stir and heat to 90°C for 0.5h. The reaction kettle was cooled to room temperature in an ice-water bath, and the aqueous phase was collected and detected. The conversion rate of levulinic acid was 95%, and the yield of 2-hydroxy-2-methylsuccinic acid was 81%. The product was detected by H NMR and C NMR. confirmed.

Embodiment 3

[0030] Add 0.15mmol levulinic acid, 50mg CaO, 50mg activated carbon calcined at 900°C for 4h in nitrogen atmosphere into a 10mL high temperature and high pressure reaction kettle in turn, seal the reaction kettle, fill with oxygen (0.5Mpa), stir and heat to 90°C for 0.5h . The reaction kettle was cooled to room temperature in an ice-water bath, and the aqueous phase was collected and detected. The conversion rate of levulinic acid was 86%, and the yield of 2-hydroxy-2-methylsuccinic acid was 56%. The product was detected by H NMR and C NMR. confirmed.

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Abstract

The invention relates to a metal-free synthetic method of 2-hydroxy-2-methylsuccinic acid, which is characterized in that a metal-free loaded carbon-based material is used for activating an oxygen source, levulinic acid is promoted to efficiently convert, the 2-hydroxy-2-methylsuccinic acid is obtained with high selectivity, and the product yield can reach 89%. The preparation method comprises the following specific steps: sequentially adding a carbon-based material, calcium oxide and a levulinic acid solution into a high-temperature-resistant and high-pressure-resistant reaction kettle, then introducing oxygen, heating to a reaction temperature, stirring, and cooling to room temperature after the reaction time is up; and filtering the reaction liquid, and carrying out reduced pressure rotary evaporation to obtain crude 2-hydroxy-2-methylsuccinic acid. The reactants used in the invention can be prepared from biomass, the catalyst used in the invention has the advantages of low cost, mild reaction conditions, short time, simple operation and simple post-treatment, and has very important application prospects.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, in particular to a method for synthesizing 2-hydroxy-2methylsuccinic acid without metal participation. Background technique [0002] In recent years, due to the large-scale use of plastics, the problem of white pollution has become increasingly serious, and the research and development of biodegradable materials has received extensive attention. Among a wide range of oxygen-containing chemicals, organic acids, especially dicarboxylic acids derived from biomass and its derivatives, have received considerable attention and can be applied to almost all aspects of social production and life, such as food and fuel additives , cosmetic and pharmaceutical synthesis, biopolymer and polyester manufacturing, etc. [0003] Biomass-based products are selectively converted to dicarboxylic acids. The commonly used method is catalytic conversion of metal catalysts, which involves the use of noble metals, tran...

Claims

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Application Information

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IPC IPC(8): C07C51/245C07C59/245
CPCC07C51/245C07C59/245Y02E50/10
Inventor 杨维冉王艳涛段亚琪
Owner NANCHANG UNIV
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