Environment-friendly high-efficiency method for synthesizing adipic acid by catalytically oxidating adipic dialdehyde

A catalytic oxidation, environment-friendly technology, applied in the direction of chemical instruments and methods, preparation of organic compounds, physical/chemical process catalysts, etc., can solve the problems of environmental pollution, high price, high cost, etc., and achieve an environmentally friendly catalytic conversion process, significantly Industrial application value, low cost effect

Inactive Publication Date: 2013-12-18
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, if concentrated nitric acid is used as an oxidant to oxidize adipaldehyde to prepare adipic acid, there is also a serious problem of environmental pollution.
[000

Method used

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  • Environment-friendly high-efficiency method for synthesizing adipic acid by catalytically oxidating adipic dialdehyde

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Example 1: h 2 WO 4 -1 # catalyst

[0013] In a 25 ml three-neck round bottom flask equipped with stirring, reflux condensation and a thermometer, add 0.25 mmol tungstic acid H 2 WO 4 and 0.02 mol of hydrogen peroxide at a concentration of 30%, and stirred at room temperature for 50 minutes. After adding 0.01 mole of adipaldehyde solution dropwise, the stirring speed was increased. By heating in a water bath, the temperature of the bath was controlled to rise from 65°C to 95°C in about 2 hours, and the reflux of the reactant was maintained. After the reaction is completed, the analysis results are shown in Table 1.

Embodiment 2

[0014] Example 2: h 3 [P(W 3 o 10 ) 4 ]·10H 2 O-2 # catalyst

[0015] In a 25ml three-neck round bottom flask equipped with stirring, reflux condensation and thermometer, add 0.02mmol of phosphotungstic acid and 0.022mol of hydrogen peroxide with a concentration of 10%, respectively, and stir at room temperature for 30 minutes. After adding 0.01 mole of adipaldehyde solution dropwise, the stirring speed was increased. By heating in a water bath, the temperature of the bath was controlled to rise from 40°C to 90°C in about 3 hours, and the reflux of the reactants was maintained. After the reaction is completed, the analysis results are shown in Table 1.

Embodiment 3

[0016] Example 3: 20% WO 3 / SnO 2 -3 # catalyst

[0017] In a 25 ml three-neck round bottom flask equipped with stirring, reflux condensation and a thermometer, add 20% WO with a tungsten content of 1% relative to the molar content of adipaldehyde 3 / SnO 2 And after 0.02 mol of hydrogen peroxide with a concentration of 50%, stir at room temperature. After adding 0.01 mole of adipaldehyde solution dropwise, the stirring speed was increased. By heating in a water bath, the temperature of the bath was controlled to rise from 60°C to 92°C in about 2 hours, and the reflux of the reactants was maintained. After the reaction is completed, the analysis results are shown in Table 1.

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Abstract

The invention belongs to the technical field of chemical engineering, and particularly relates to an environment-friendly high-efficiency method for synthesizing adipic acid by catalytically oxidating adipic dialdehyde. According to the invention, by using a tungsten-base material as a catalyst and a 10-70 wt% hydrogen peroxide aqueous solution as an oxidant, the adipic dialdehyde is aqueous catalytically oxidated to synthesize the adipic acid. The method provided by the invention has the advantages of mild conditions, simple technique, low cost and high yield. The yield of the adipic acid is up to 95-99%, and the purity is at least 99.0%. Due to the adoption of the hydrogen peroxide aqueous solution as the oxidant, the reaction is a solventless system, thereby solving the problem of environment friendliness in the traditional nitric acid oxidation process, and achieving the goal of an environment-friendly catalytic conversion technique.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to an environmentally friendly method for synthesizing adipic acid by catalytically oxidizing adipaldehyde with aqueous hydrogen peroxide solution. Background technique [0002] Adipic acid is an important organic dibasic acid, which is mainly used in the manufacture of nylon-66 fibers and resins. It can also be used in the production of lubricants, plasticizers, and medicine. It has a wide range of uses. The traditional nitric acid oxidation method is seriously corroded due to equipment. and generate a large number of N 2 O pollutants are gradually phased out. In recent years, there are also reports on the air oxidation of cyclohexane (ChemSusChem. 2012, 5, 1213-1217) and biological methods (Biotechnol. Prog. 2002, 18, 201-211; CN 102482638A) to prepare adipic acid, but The operation process is expensive, the device is huge, and the yield of adipic acid is ...

Claims

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Application Information

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IPC IPC(8): C07C55/14C07C51/285B01J23/30B01J27/188
Inventor 戴维林张召艳宗保宁
Owner FUDAN UNIV
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