Solid-supported metalloporphyrin catalyst and application thereof in preparation of maleic acid

A technology of metalloporphyrins and catalysts, applied in the field of immobilized metalloporphyrin catalysts and its preparation of maleic acid, can solve the problem of insufficient yield and selectivity of maleic acid, insufficient mild reaction conditions, and long reaction time and other problems, to achieve good catalytic effect, mild reaction conditions, and reduce energy consumption

Active Publication Date: 2017-07-07
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The maleic acid yield and selectivity prepared by the above reports are not high enough, and there is a serious defect, that is, the reaction conditions are not gent

Method used

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  • Solid-supported metalloporphyrin catalyst and application thereof in preparation of maleic acid
  • Solid-supported metalloporphyrin catalyst and application thereof in preparation of maleic acid
  • Solid-supported metalloporphyrin catalyst and application thereof in preparation of maleic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] (1) Weigh 50 mg of the solid-supported metalloporphyrin catalyst FeT(p-R)PP / SBA-15 (wherein R is -Br) in a polytetrafluoroethylene lining, and add 4 mL of deionized water;

[0047] (2) The carrier SBA-15 in step (1) is replaced by MCM-41, ZSM-5;

[0048] (3) Weigh 0.282g furfural into the reaction system of step (1) and step (2), put the polytetrafluoroethylene lining into the stainless steel reaction kettle, heat to 90°C under magnetic stirring, feed oxygen, apply React with a reaction pressure of 1MPa for 6 hours. After the reaction, close the valve of the oxygen cylinder. After the reaction kettle is cooled to room temperature, slowly release the gas in it;

[0049] (4) Pipette 50 μL of the reaction solution in step (3) with a pipette gun, make the volume to 5 mL with deionized water, and measure the yield of maleic acid with a high-performance liquid chromatograph.

[0050] After measurement, the result is as figure 2 As shown, the catalysts prepared with SBA-15,...

Embodiment 2

[0061] (1) Weigh 50 mg of the solid-supported metalloporphyrin catalyst FeT(p-R)PP / SBA-15 (wherein R is -Br) in a polytetrafluoroethylene lining, and add 4 mL of deionized water;

[0062] (2) Weigh 0.282g furfural into the reaction system of step (1), put the polytetrafluoroethylene lining into the stainless steel reaction kettle, heat to 70-120°C under magnetic stirring, feed oxygen, and apply 1MPa reaction Pressure reaction for 6 hours, close the valve of the oxygen cylinder after the reaction, and slowly release the gas in the reaction kettle after it is cooled to room temperature;

[0063] (3) Take out 50 μL of the reaction solution in step (2) with a pipette gun, make the volume to 5 mL with deionized water, and measure the yield of maleic acid with a high-performance liquid chromatograph.

[0064] After measurement, the result is as image 3 Shown, when reaction temperature is 70 ℃, 80 ℃, 90 ℃, 100 ℃, 110 ℃, when 120 ℃, the productive rate of maleic acid is respectively...

Embodiment 3

[0066] (1) Weigh 50 mg of the solid-supported metalloporphyrin catalyst FeT(p-R)PP / SBA-15 (wherein R is -Br) in a polytetrafluoroethylene lining, and add 4 mL of deionized water;

[0067] (2) Weigh 0.282g of furfural into the reaction system of step (1), put the polytetrafluoroethylene lining into the stainless steel reaction kettle, heat to 100°C under magnetic stirring, feed oxygen, and apply a reaction pressure of 1MPa to react 3-8h, close the valve of the oxygen cylinder after the reaction is over, and slowly release the gas in the reactor after it cools down to room temperature;

[0068] (3) Take out 50 μL of the reaction solution in step (2) with a pipette gun, make the volume to 5 mL with deionized water, and measure the yield of maleic acid with a high-performance liquid chromatograph.

[0069] After measurement, the result is as Figure 4 As shown, when the reaction time is respectively 3h, 4h, 5h, 6h, 7h, 8h, the yield of maleic acid is respectively 35.7%, 41.6%, 44...

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Abstract

The invention discloses a solid-supported metalloporphyrin catalyst and application thereof in preparation of maleic acid, belonging to the technical field of catalytic application of metalloporphyrin. The solid-supported metalloporphyrin catalyst is used for preparing maleic acid by catalyzing furfural and has a good catalytic effect, and reaction conditions are mild, so that the energy consumption required in the prior art is greatly reduced. By utilizing the catalyst disclosed by the invention, a good microenvironment can be provided for reaction, so that the yield and selectivity of maleic acid are increased; by utilizing a method disclosed by the invention, the conversion rate of furfural is 20.4%-95.6%, the yield of maleic acid is 10%-56.1%, the selectivity of maleic acid is 43.6%-76.1%; and meanwhile, the catalyst is easy to separate, can be repeatedly and circularly utilized and is environment-friendly.

Description

technical field [0001] The invention relates to a solid-supported metalloporphyrin catalyst and its application in the preparation of maleic acid, belonging to the technical field of metalloporphyrin catalytic application. Background technique [0002] In the past few decades, human society has developed rapidly and the degree of modernization has been continuously improved, but at the same time, energy and environmental problems have become increasingly serious. Traditional fossil energy has been difficult to supply the needs of industrial development. Global warming, three wastes, Problems such as smog continue to threaten human health. Therefore, it is imminent to find clean and renewable energy to replace traditional fossil energy. Biomass, as the most widely distributed renewable energy source on earth, has attracted more and more attention from researchers. There are also more and more reports on the preparation of high value-added platform compounds through biomass-b...

Claims

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Application Information

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IPC IPC(8): B01J31/22C07C51/31C07C57/145
CPCB01J31/1633B01J31/183C07C51/313B01J2531/025B01J2531/842C07C57/145B01J29/14B01J29/46B01J29/70B01J2531/16B01J2531/26B01J2531/72B01J2531/845B01J2531/847B01J2231/70Y02P20/50B01J31/1815B01J29/40B01J31/26B01J37/04B01J37/035B01J37/009B01J37/06B01J37/0236
Inventor 王海军黄义吴春炎袁文文
Owner JIANGNAN UNIV
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