Method for preparing glutaric acid through oxidation of glutaral pentanedial

A technology of glutaraldehyde and glutaric acid, which is applied in the field of glutaraldehyde oxidation to prepare glutaric acid, which can solve the problems of high price, high production cost, and difficulty in recycling

Active Publication Date: 2009-11-04
SHANGHAI HUAYI NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But the method starts with H 2 o 2 As an oxidant, tungstic acid, tungstophosphoric acid, and tungstosilicic acid, which are expensive and difficult to recycle, are used as catalysts, and the repeatability of the catalyst is poor, and the performance will be greatly reduced after being used for more than two times, and the production cost is still high
In the patent GB767416, air is used as the oxidant, and Co(OAC) 2 4H 2 O is the catalyst for the homogeneous oxidation of glutaraldehyde to produce glutaric acid, but the reaction effect is poor. After 12 hours of reaction, the yield of glutaric acid is only 75%. After crystallization and separation, the total yield of glutaric acid is only 53%.

Method used

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  • Method for preparing glutaric acid through oxidation of glutaral pentanedial
  • Method for preparing glutaric acid through oxidation of glutaral pentanedial
  • Method for preparing glutaric acid through oxidation of glutaral pentanedial

Examples

Experimental program
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Effect test

Embodiment 1～15

[0013] Catalyst preparation by co-impregnation method: Prepare a mixed aqueous solution with metered palladium nitrate, palladium chloride or palladium acetate and the soluble salt of component M, impregnate the carrier that has been shaped into 20-40 meshes and let it stand for 8 hours, and slowly evaporate to dryness at 75°C Moisture content, dried in an oven at 120°C for 12 hours, roasted at 500°C, the roasting atmosphere is nitrogen or air; after that, hydrogen is used for reduction treatment, the treatment conditions are: hydrogen pressure 0.5MPa, reduction time 2 hours, reduction temperature 400°C, hydrogen quality Airspeed 200h -1 . See Table 1 for the content of catalyst Pd and component M, M precursor, and calcination atmosphere in each embodiment.

[0014] Table 1 Pd-M / A catalyst prepared by co-impregnation method

[0015]

[0016] Catalyst preparation by step-by-step impregnation method: firstly make the measured palladium nitrate, palladium chloride or palladi...

Embodiment 16～18

[0031]The reacted product systems of Examples 12-14 were left to cool down to room temperature, and the catalyst naturally settled to the bottom of the reactor. Pour out the upper layer reaction solution, add the same material as the previous ratio to the reactor, and carry out the second reaction under the same reaction conditions, the reaction results are shown in Table 4.

[0032] The repeatability test of table 4 embodiment 12~14 catalyst

[0033]

[0034] Note: The meanings of the items in the table are the same as those in Table 3.

Embodiment 19

[0036] The product after the reaction of Example 18 was left to cool to room temperature, and the catalyst naturally settled to the bottom of the reactor. Pour out the upper reaction liquid, add the same material as the previous proportion to the reactor, and react under the same reaction conditions, the reaction results are shown in Table 4.

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Abstract

The invention provides a method for preparing glutaric acid through the oxidation of glutaral pentanedial. The method takes a load type solid catalyst containing an active component Pd, takes air as an oxidant, and oxidizes glutaral pentanedial into glutaric acid in a gas-liquid-solid three-phase intermittent or continuous reaction mode under moderate conditions. The method has high glutaral pentanedial conversion rate and high glutaric acid selectivity, easy separation of the catalyst from the raw materials and products, simple and feasible operation, the air oxidant which is easily obtainedand has low price, low production cost, green and environmental protection reaction process, and easy large-scale industrialized production.

Description

technical field [0001] The invention relates to a method for preparing glutaric acid by oxidation of glutaraldehyde, in particular to a supported solid catalyst for oxidation of glutaraldehyde and a preparation method thereof, as well as a gas-liquid-solid three-phase reaction process using air as an oxidant and method. Background technique [0002] Glutaric acid is an important chemical raw material, which can be used to prepare glutaric anhydride, α-ketoglutaric acid, peroxyglutaric acid, β-(4-chlorophenyl)glutaric acid and antihypertensive agents Intermediates, etc.; commonly used as initiators in the field of synthetic resins and synthetic rubbers; commonly used as plasticizers in the plastics industry; in medicine, because of its broad-spectrum bactericidal ability, it is used to prepare various sterilizing lotions and medicines; In addition, glutaric acid also has good compatibility and mild chemical properties, and can be used as a cleaning agent, etc.; glutaric acid...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C55/12C07C51/235B01J23/89B01J23/63B01J23/644B01J23/652B01J23/656B01J29/76B01J29/46B01J37/02
Inventor 罗鸽刘歆文施觊敏印俊
Owner SHANGHAI HUAYI NEW MATERIAL
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