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Method for preparing acrylic acid by carrying out liquid phase catalytic oxidation on acrylic aldehyde

A technology of catalytic oxidation and acrolein liquid, applied in chemical instruments and methods, preparation of organic compounds, preparation of carboxylate, etc., can solve the problems of strong exothermic reaction system, catalyst deactivation reaction cost, increase, etc., and achieve stability Good performance, improved economic feasibility, and simple operation process

Inactive Publication Date: 2017-09-15
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is to solve the problem that in the current process of preparing acrylic acid by gas-phase oxidation of acrolein, high temperature (generally above 220°C) causes strong heat release in the reaction system, resulting in deactivation of the catalyst and increase in reaction cost, and provides an acrolein Method for preparing acrylic acid by liquid-phase catalytic oxidation

Method used

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  • Method for preparing acrylic acid by carrying out liquid phase catalytic oxidation on acrylic aldehyde
  • Method for preparing acrylic acid by carrying out liquid phase catalytic oxidation on acrylic aldehyde
  • Method for preparing acrylic acid by carrying out liquid phase catalytic oxidation on acrylic aldehyde

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Experimental program
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Effect test

Embodiment 1～5

[0027] Add 30mL of 1,2-dichloroethane, 2.6g of o-dichlorobenzene (internal standard), 2.69g of acrolein and 100mg of nitrogen-doped carbon nanotubes (N content is 4.34at%) into the autoclave and stir Heating to the temperature shown in Table 1, feeding oxygen, starting timing (t=0), and maintaining its pressure during the reaction is 1MPa; after reacting for 4h, stop timing, the reactor is cooled to room temperature, and filter the liquid solid phase mixture to obtain a solid catalyst and a liquid phase mixture containing unreacted reactants and reaction products.

Embodiment 2

[0028] The gas chromatogram of the liquid phase mixture containing unreacted reactant and reaction product after the reaction of embodiment 2 is as follows image 3 shown. Depend on image 3 It can be seen that the retention times t of acrolein, acrylic acid and the internal standard o-dichlorobenzene are 1.688, 2.872 and 8.020 min respectively, and the conversion rate of acrolein and the selectivity of acrylic acid are calculated by the standard curves of acrolein and acrylic acid.

[0029] The liquid phase mixture containing unreacted reactants and reaction products was detected and analyzed by gas chromatography (GC), and the GC detection results are shown in Table 1 (the influence of reaction temperature on the liquid phase oxidation reaction of acrolein).

[0030] The GC detection result of table 1 embodiment 1~5

[0031]

[0032] It can be seen from Table 1 that increasing the temperature is beneficial to increase the conversion rate of acrolein, but when the temper...

Embodiment 6～12

[0034] Add 30mL of 1,2-dichloroethane, 2.6g of o-dichlorobenzene (internal standard), 2.69g of acrolein and 100mg of nitrogen-doped carbon nanotubes (the N content is 4.34at%) into the autoclave, stir and heat To 85°C, feed oxygen, start timing (t=0), and maintain its pressure during the reaction to be 1MPa; after reacting to the time shown in Table 2, stop timing, cool the reactor to room temperature, filter the liquid solid phase mixture to obtain a solid catalyst and a liquid phase mixture containing unreacted reactants and reaction products.

[0035] The liquid phase mixture containing unreacted reactants and reaction products was detected and analyzed by gas chromatography (GC), and the GC detection results are shown in Table 2 (the influence of reaction time on the liquid phase oxidation reaction of acrolein).

[0036] The GC detection result of table 2 embodiment 6~12

[0037]

[0038] Analysis of the data in Table 2 shows that the conversion rate of acrolein increa...

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Abstract

The invention discloses a method for preparing acrylic acid by carrying out liquid phase catalytic oxidation on acrylic aldehyde. The method disclosed by the invention comprises the following steps: taking an organic solvent as a reaction solvent system, adding acrylic aldehyde and nitrogen-doped carbon nanotubes, introducing oxygen, stirring and reacting for 0.1-24 hours at the pressure of 0.1-2MPa and at the temperature of 80-100 DEG C, and oxidizing the acrylic aldehyde into acrylic acid. The method disclosed by the invention has the advantages of high acrylic acid selectivity, mild reaction conditions, simple operation, low cost, simple and easily available catalyst, easiness in recycling and good stability; and the conversion rate of the acrylic aldehyde reaches more than 20%, and the selectivity of the acrylic acid reaches more than 60%.

Description

technical field [0001] The invention relates to the technical field of acrylic acid preparation, in particular to a method for preparing acrylic acid by liquid-phase catalytic oxidation of acrolein. Background technique [0002] Acrylic acid (AA), as the simplest unsaturated monocarboxylic acid, is a widely used industrial raw material. The main use of acrylic acid in industry is to manufacture acrylates with high added value. Its applications involve building materials, adhesives, coatings, superabsorbent resins, leather, chemical fibers, papermaking, additives, detergents, curing agents and printing. All walks of life; acrylic acid is also prone to homopolymerization or copolymerization reaction to form polyacrylate, which can be used as common additives such as various softeners, food preservatives and thickeners. [0003] Since the late 1960s, the gas-phase catalytic oxidation of acrolein to acrylic acid has received extensive attention. Composite metal oxides are cata...

Claims

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Application Information

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IPC IPC(8): C07C51/235C07C57/045
CPCY02P20/584C07C51/235C07C57/04
Inventor 余皓曹永海侯萌萌彭峰王红娟
Owner SOUTH CHINA UNIV OF TECH
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