Nano zinc sulfide metalloporphyrin catalyst and preparation method and application thereof

A nano-zinc sulfide and metalloporphyrin technology, applied in the field of chemical engineering, can solve the problems of low yield of ketone alcohol, low conversion rate and the like, and achieve the effects of easy separation, improved catalytic performance and low cost

Inactive Publication Date: 2013-02-13
GUANGXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a nanometer zinc sulfide metalloporphyrin catalyst and its preparation in order to overcome the technical deficiencies of low catalyst conversion rate and low yield of ketone alcohol in the production of cyclohexanol and cyclohexanone by catalytic oxygen oxidation of cyclohexane Methods and Applications

Method used

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  • Nano zinc sulfide metalloporphyrin catalyst and preparation method and application thereof
  • Nano zinc sulfide metalloporphyrin catalyst and preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0031] 1. Preparation of zinc sulfide

[0032] Add 73.7666g of zinc sulfate heptahydrate into the dissolver, add 200g of deionized water and stir to completely dissolve it. After the sodium sulfide nonahydrate of 61.6124g is completely dissolved in the same way, slowly add to the fully dissolved ZnSO4 under stirring. 4 In the solution, a white zinc sulfide precipitate is gradually generated, and it is filtered under reduced pressure, and the filter cake is washed with a large amount of deionized water, and at the same time, it is washed with B a Cl 2 Solution tracking and detection of filtrate until there is no SO in the filtrate 4 2- ion.

[0033] 2. Preparation of nano-zinc sulfide cobalt porphyrin catalyst

[0034] The zinc sulfide obtained above was dispersed in 39g of ethanol by mechanical stirring, then 0.025g of cobalt porphyrin dissolved in 52g of ethanol was added, kept at 60°C and stirred for 6h, the organic solvent was removed by vacuum distillation, and the fi...

Embodiment 2

[0040] 1. Preparation of zinc sulfide

[0041] Add 73.7666g of zinc sulfate heptahydrate into the dissolver, add 200g of deionized water and stir to completely dissolve it. After dissolving 61.6124g of sodium sulfide nonahydrate completely in the same way, slowly add to the dissolved ZnSO 4 In the solution, a white zinc sulfide precipitate is gradually generated, and it is filtered under reduced pressure, and the filter cake is washed with a large amount of deionized water, and at the same time, it is washed with B a Cl 2 Solution tracking and detection of filtrate until there is no SO in the filtrate 4 2- ion.

[0042] 2. Preparation of nano-zinc sulfide cobalt porphyrin catalyst

[0043] The zinc sulfide obtained above was dispersed in 39g of ethanol by mechanical stirring, then 0.025g of cobalt porphyrin dissolved in 52g of ethanol was added, kept at 70°C and stirred for 5h, the organic solvent was removed by vacuum distillation, and the filter cake was filtered and wa...

Embodiment 3

[0049] 1. Preparation of zinc sulfide

[0050] Add 73.7666g of zinc sulfate heptahydrate into the dissolver, add 200g of deionized water and stir to completely dissolve it. After dissolving 61.6124g of sodium sulfide nonahydrate completely in the same way, slowly add to the dissolved ZnSO 4 In the solution, a white zinc sulfide precipitate is gradually generated, and it is filtered under reduced pressure, and the filter cake is washed with a large amount of deionized water, and at the same time, it is washed with B a Cl 2 Solution tracking and detection of filtrate until there is no SO in the filtrate 4 2- ion.

[0051] 2. Preparation of nano-zinc sulfide cobalt porphyrin catalyst

[0052] The zinc sulfide obtained above was dispersed in 39g of methanol by mechanical stirring, and then 0.025g of cobalt porphyrin dissolved in 52g of methanol was added, kept at 65°C and stirred for 5.5h, and the organic solvent was removed by vacuum distillation, and filtered, washed and fi...

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Abstract

The invention discloses a nano zinc sulfide metalloporphyrin catalyst and a preparation method and application thereof. The method comprises the following steps of: reacting zinc vitriol and sodium sulfide to obtain zinc sulfide precipitation, and reacting the zinc sulfide and metalloporphyrin to prepare the nano zinc sulfide metalloporphyrin catalyst, wherein the catalyst comprises the the following main raw materials in parts by weight: 16.198 parts of zinc vitriol, 13.529 parts of sodium sulfide, 0.006 part of metalloporphyrin, 26.350 to 32.297 parts of organic solvent and a proper quantity of deionized water. The catalyst can be used for obviously improving the conversion per pass of cyclohexane and the yield of primary products, wherein the conversion rate of the cyclohexane is 72.9 percent, the turn over number of the catalyst is 9.4*105, and the yield of ketol is 27.0 percent. The catalyst can be repeatedly recycled, the preparation method is simple, the cost is low, the metalloporphyrin is less in quantity and easy to separate, and the catalyst is an ideal bionic industrial catalyst and has good economic benefits and social benefits.

Description

technical field [0001] The invention belongs to the technical field of chemical engineering, and relates to a nano-zinc sulfide metalloporphyrin catalyst and its preparation method and application, in particular to a nano-zinc sulfide dual-type linkage (ie, ionic bond and coordination bond) tetrakis(4-carboxylate) A phenyl)metalloporphyrin catalyst, a preparation method thereof, and an application in catalytic oxygen oxidation of cyclohexane to produce cyclohexanone and cyclohexanol. Background technique [0002] The oxidation reaction of cyclohexane to prepare cyclohexanol and cyclohexanone (commonly known as KA oil) is an important reaction in industry. Cyclohexanol and cyclohexanone are the main intermediates for the preparation of caprolactam and adipic acid and then nylon-6 and nylon-66. They are also raw materials for the preparation of spices and rubber anti-aging agents. They are also used in medicine, pesticides, printing and Plastic recycling and more. Since cycl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22C07D487/04C07C27/12
CPCY02P20/584
Inventor 蒋月秀黄冠宁星星罗宗昌危素娟
Owner GUANGXI UNIV
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