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A metal-organic framework-supported phosphotungstic acid catalyst, preparation method and application of catalytic synthesis of adipic acid

A metal-organic framework, phosphotungstic acid technology, used in the preparation of organic compounds, organic compound/hydride/coordination complex catalysts, heterogeneous catalyst chemical elements, etc., can solve the problem that the active component phosphotungstic acid cannot effectively Dispersion, difficult catalyst recycling, complex catalyst preparation process, etc., to achieve the effect of recyclable preparation process, green and clean production process, and easy separation and purification

Active Publication Date: 2020-09-25
CHONGQING UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When tungstate or phosphotungstic acid is directly used as a catalyst, due to the existence of "pseudo-liquid phase" behavior, it is very difficult to recycle the catalyst, and the product contains more impurities
[0004] Patent CN102614920 introduces a catalyst preparation method of immobilizing tungstate on a silica or polystyrene resin carrier, and uses the catalyst to catalyze the oxidation of cyclohexene to synthesize adipic acid. The catalyst realizes recycling, but the catalyst The preparation process is relatively complicated, and the patent does not involve the synthesis of adipic acid using cyclohexanol or cyclohexanone as raw materials
It has also been reported to use solid-supported phosphotungstic acid such as alumina and silica as catalysts (Industrial Catalysis, 2009, 17(7), 46-48; Journal of Xi'an Engineering University, 2017, 31(1), 36-40), which can Realize the recovery and utilization of catalysts, but the specific surface area of ​​these conventional supports is small, the active component phosphotungstic acid cannot be effectively dispersed on the surface of the support, and agglomeration is easy to occur during the reaction process, resulting in poor stability of the catalyst

Method used

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  • A metal-organic framework-supported phosphotungstic acid catalyst, preparation method and application of catalytic synthesis of adipic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) Preparation of metal-organic framework-supported phosphotungstic acid catalyst

[0025] According to method A, add 1.6g of metal-organic framework UiO-66 and 100mL of anhydrous n-hexane into the round bottom flask, ultrasonically disperse for 30min, and add 686μL of phosphotungstic acid aqueous solution with a concentration of 1g / mL dropwise under rapid stirring (that is, metal The mass ratio of organic framework to phosphotungstic acid is 2.3:1), continue to stir for 8 hours, and filter with suction. The obtained solid is vacuum-dried at 120°C for 10 hours, and the metal-organic framework-supported phosphotungstic acid catalyst is prepared, which is marked as catalyst A.

[0026] (2) Synthesis of adipic acid

[0027] Add 0.5g of catalyst A, 0.056g of oxalic acid (0.62mmol) and 15.9mL of 30% hydrogen peroxide (155mmol) into the round bottom flask, stir well and then add 3g of cyclohexanone (31mmol), and stir at 90°C After reacting for 8 hours, the reacted mixture w...

Embodiment 2

[0029] The operation steps are the same as in Example 1, except that 3.1 g of cyclohexanol (31 mmol) is added to replace cyclohexanone during the synthesis of adipic acid, and the yield of adipic acid is 72.90%.

Embodiment 3

[0031] The operation steps are the same as in Example 1, the difference is that the amount of oxalic acid added is 0 when adipic acid is synthesized, and the yield of adipic acid is 61.20%.

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Abstract

The invention discloses a metal-organic framework-loaded phosphotungstic acid catalyst, which includes a carrier and an active component loaded on the carrier: wherein the carrier is a metal-organic framework, and the active component is phosphotungstic acid. The invention also Disclosed are a preparation method for a metal-organic framework-supported phosphotungstic acid catalyst and its application in catalytically synthesizing adipic acid. The catalyst prepared by the invention maintains the characteristics of a high specific surface area of ​​the carrier, is environmentally friendly, has mild reaction conditions, is highly efficient and has good stability, and the catalyst can be recycled.

Description

technical field [0001] The invention belongs to the field of chemical synthesis and relates to a metal-organic framework composite catalyst for synthesizing adipic acid. The invention specifically relates to a metal-organic framework-loaded phosphotungstic acid catalyst, a preparation method and an application for catalytically synthesizing adipic acid. Background technique [0002] Adipic acid, also known as fatty acid, is an important basic chemical raw material and organic synthesis intermediate. It is mainly used as a raw material for the production of synthetic fibers (such as nylon-66), polyester foam and synthetic resins, and can also be used for the production of esters. Plasticizers, lubricating oil additives, food additives and textile treatment agents, etc. The traditional adipic acid production process mainly adopts the nitric acid oxidation method, and oxidizes cyclohexanol and cyclohexanone (KA oil) with strong oxidizing concentrated nitric acid to obtain adipi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/22B01J27/188C07C51/285C07C55/14
CPCC07C51/285B01J27/188B01J31/1691B01J2231/70B01J2523/48B01J35/396C07C55/14Y02P20/584
Inventor 冯建钟艳辉戴松桓
Owner CHONGQING UNIVERSITY OF SCIENCE AND TECHNOLOGY
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