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Method for preparing butanedioic acid through catalytic oxidation cracking of acetylpropionic acid

A technology for catalytic oxidation of levulinic acid, applied in carboxylate preparation, chemical instruments and methods, preparation of organic compounds, etc., can solve the problem of reduced catalytic activity, low selectivity of the product succinic acid, easy deactivation with water, etc. problem, to achieve the effect of improving selectivity and suppressing adverse effects

Active Publication Date: 2016-06-29
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

Homogeneous manganese compounds are easily deactivated by water in the oxidation reaction, and the surface of manganese oxides will absorb water, resulting in a significant decrease in their catalytic activity. Therefore, the catalysts in previous studies cannot be recycled or the selectivity of the product succinic acid is low.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Material M(MnPh-SiO 2 ) preparation

[0026] Mix 15g sodium dodecylbenzenesulfonate, 35g n-hexane, 6g n-hexanol and 0.5g ammonia water to obtain solution A; dissolve 0.02g manganese acetate in 3g deionized water to obtain solution B; Mix phenyltriethoxysilane to obtain solution C; add solution B and solution C to solution A under stirring conditions, and age for 20 hours; add 15 mL of acetone, stir for 20 minutes, and take the solid after centrifugation; add 80 mL of ethanol to the solid , heated and stirred for 20min, and centrifuged; repeat this step several times until the surfactant is removed; vacuum-dried at 100°C to obtain the nanomaterial MnPh-SiO 2 .

[0027] Levulinic Acid Oxidation:

[0028] With 5g levulinic acid, 5wt% (relative to levulinic acid) MnPh-SiO 2Add it into a 50mL reactor, fill it with oxygen to 1.0MPa, raise the temperature to 150°C under constant stirring, and keep it for 10h. Then cool to room temperature. Methanol is added to fully diss...

Embodiment 2

[0032] Example 2: Mix 20g Np-10, 25g cyclohexane and 3g n-octanol to obtain solution A; dissolve 0.02g manganese chloride in 3g deionized water, and add 0.5g ammonia water to obtain solution B; 1g ethyl orthosilicate Mix ester and 0.2g heptadecanyltriethoxysilane to obtain solution C; pour solution B into solution A to obtain solution D, add solution C to solution D under vigorous stirring, and age for 8 hours; then, add 10mL Acetone, stirred for 30 min, and centrifuged to take out the solid; add 30 mL of ethanol to the solid, heat and stir for 10 min, and centrifuge; repeat this step several times until the surfactant is completely removed; dry at 80 ° C to obtain the final nanomaterial HF-Mn- SiO 2 .

[0033] Levulinic Acid Oxidation:

[0034] With 5g levulinic acid, 5wt% (relative to levulinic acid) HF-Mn-SiO 2 Add it into a 50mL reactor, fill it with oxygen to 0.5MPa, raise the temperature to 150°C under constant stirring, and keep it for 5h. Then cool to room temperat...

Embodiment 3

[0035] Embodiment 3: get 20g ethanol and 0.9g ammonia water and mix to obtain solution A; 0.03g manganese sulfate is dissolved in 5g deionized water to obtain solution B; Solution C; add solution B and solution C to solution A under stirring conditions, and age for 20 hours; take the solid after centrifugation; add 60 mL of ethanol to the solid, heat and stir for 15 minutes, and centrifuge; dry at 100 ° C to obtain the final nanomaterial Pr-Mn-SiO 2 .

[0036] Levulinic Acid Oxidation:

[0037] With 5g levulinic acid, 10wt% (relative to levulinic acid) Pr-Mn-SiO 2 Add it into a 50mL reactor, fill it with oxygen to 1.5MPa, raise the temperature to 120°C with constant stirring, and keep it for 15h. Then cool to room temperature. Methanol is added to fully dissolve the organic matter, the solid catalyst is filtered after centrifugation, and the conversion rate of the raw material and the selectivity of the product succinic acid are obtained through liquid chromatography analy...

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Abstract

A method for preparing butanedioic acid through catalytic oxidation cracking of acetylpropionic acid is provided; according to the method, a manganese-containing composite oxide material modified by a hydrophobic group is used as a catalyst, molecular oxygen is used as an oxygen source, and acetylpropionic acid is oxidized into butanedioic acid under a solvent-free condition. The hydrophobic properties of the catalyst can inhibit adsorption of oxidation by-product water on the catalyst surface, and the catalyst stability is improved; at the same time, through control of adsorption of raw materials and products on the catalyst surface, the selectivity of the target product butanedioic acid is improved.

Description

technical field [0001] The invention belongs to the application of nanometer materials in catalytic oxidation reaction, and specifically applies hydrophobic manganese-containing nanometer composite oxide materials to the reaction of levulinic acid oxidation to prepare succinic acid, so as to improve catalyst stability and product selectivity. Background technique [0002] Succinic acid is an important fine chemical intermediate, which can be used in the production of 1,4-butanediol, tetrahydrofuran, γ-butyrolactone and N-methylpyrrolidone, etc., in food, spices, medicine, coatings, rubber and Plastic industry has a wide range of applications. Succinic acid and 1,4-butanediol can be polymerized into polybutylene succinate as monomers. This material has good biodegradability, has important application value and broad development prospects. [0003] At present, the production method of succinic acid mainly uses benzene or butane as raw materials, firstly obtains maleic anhydri...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C55/10C07C51/23B01J23/34
CPCY02P20/584
Inventor 杜中田徐杰马阳阳夏飞苗虹黄义争
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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