Method for preparing adipic acid from glucaric acid

A technology of glucaric acid and adipic acid is applied in the preparation of carboxylate, carboxylate, and carboxylate/lactone, etc., and can solve the problems of unfriendly environment, high equipment corrosion and high production cost, Achieve the effect of reducing production cost and high catalytic performance

Active Publication Date: 2018-01-09
PEKING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, there is only one patent (US8669397B2) that reports the process of catalytically converting glucaric acid into adipic acid, but uses acetic acid as a solvent in its method and adds halogen elements
This process not only has high production costs, but also is highly corrosive to equipment and is not friendly to the environment.

Method used

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  • Method for preparing adipic acid from glucaric acid

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preparation example Construction

[0034] 1. Preparation of supported Pd catalyst

[0035] The preparation of 0.25% Pd / AC catalyst is taken as an example for non-limiting illustration.

[0036] 68 μL of 10wt% Pd(NH 3 ) 4 (NO 3 ) 2 Mix the aqueous solution with 10.0mL deionized water, stir evenly, then add 1.00g of AC carrier (the Chinese name is activated carbon) into the mixture, stir and impregnate at room temperature for 10 hours, evaporate the water to dryness, and then dry it in an oven at 110°C After 12 hours, a catalyst precursor was obtained. The loading amount of Pd is 0.25% (mass percentage). The precursor prepared in the above steps was placed in a quartz tube, first calcined in nitrogen at 500 ° C for 2 h, and then in 20% H 2 +N 2 Reduction at a temperature of 300° C. for 1 h to obtain a supported 0.25% Pd / AC catalyst.

[0037] 2. Preparation of supported ReOx catalyst

[0038] With 5%ReOx / TiO 2 The preparation of the catalyst is used as an example for non-limiting illustration.

[0039] ...

Embodiment 1

[0047] Embodiment 1, prepare adipic acid in aqueous solution

[0048] With 5%ReOx / TiO 2 and 0.25% Pd / AC mechanically mixed catalyst as an example for non-limiting illustration.

[0049] In a 50mL autoclave, add 0.2g of 5%ReOx / TiO 2 , 0.2g of 0.25% Pd / AC catalyst and 15mL of 2% glucaric acid aqueous solution in mass percentage, after the reactor was sealed, filled with 1MPa hydrogen to replace the residual air in the reactor, after repeating three times, pour into the reactor 1MPa hydrogen gas was filled, the reaction kettle was placed on a heating furnace to be heated to a reaction temperature of 130°C, and the reaction was stirred for 10 hours at a rotation speed of 700rpm. After the reaction finished, take out the reaction kettle from the heating furnace, cool to room temperature, reduce the pressure in the kettle to normal pressure, open the lid, take out the liquid-solid mixture and separate it by suction filtration, and analyze the liquid obtained by liquid chromatograp...

Embodiment 2

[0050] Embodiment 2, prepare adipic acid in aqueous solution

[0051] The 5%ReOx-0.25%Pd / AC co-supported catalyst is taken as an example for non-limiting illustration.

[0052] In a 50mL autoclave, add 0.2g of the above-mentioned 5%ReOx-0.25%Pd / AC catalyst and 15mL of a 2% glucaric acid aqueous solution by mass percentage, and after the autoclave is sealed, fill it into a 1MPa hydrogen replacement autoclave After three repetitions, the reactor was filled with 1MPa hydrogen, and the reactor was placed on a heating furnace to be heated to a reaction temperature of 130° C., and the reaction was stirred at a speed of 700 rpm for 10 hours. After the reaction finished, take out the reaction kettle from the heating furnace, cool to room temperature, reduce the pressure in the kettle to normal pressure, open the lid, take out the liquid-solid mixture and separate it by suction filtration, and analyze the liquid obtained by liquid chromatography. And calculate the conversion and produ...

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Abstract

The invention discloses a method for preparing adipic acid from glucaric acid. The method comprises the following steps: making glucaric acid react with hydrogen in a water solution or an alcoholic solution to obtain the adipic acid. When the glucaric acid reacts with the hydrogen in the water solution, a system utilizes a hydrodeoxygenation catalyst to perform hydrodeoxygenation reaction; when the glucaric acid reacts with the hydrogen in the alcoholic solution, an esterification catalyst, the hydrodeoxygenation catalyst and a hydrolysis catalyst are sequentially added into the system to respectively perform esterification reaction, the hydrodeoxygenation reaction and hydrolysis reaction. The method disclosed by the invention has the advantages of green and pollution-free reaction processand environmental friendliness; furthermore, production cost is reduced.

Description

technical field [0001] The invention relates to a method for preparing adipic acid from glucaric acid, which belongs to the field of preparation of chemical raw materials. Background technique [0002] Adipic acid is an important chemical raw material for the production of nylon 66, polyurethane, synthetic resin, engineering plastics, adhesives, etc. It can also be used in food additives, flavoring agents, etc. The current annual output is more than 3 million tons, ranking second among all dicarboxylic acids. In recent years, the demand for adipic acid in my country has been strong, and domestic production cannot meet the market demand, so a large amount of adipic acid is imported from abroad every year. The current industrial production method of more than 90% of adipic acid mainly uses cyclohexanol and cyclohexanone (KA oil) as the nitric acid oxidation method of raw materials, the oxidant nitric acid has strong corrosion to the reaction equipment, and produces a large am...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C55/14C07C51/377C07C67/08C07C69/675C07C67/327C07C69/44C07C51/09B01J23/44B01J23/36B01J23/656B01J37/02B01J37/08B01J37/18
Inventor 刘海超王丰鑫
Owner PEKING UNIV
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