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Preparation method and use of cadmium sulfide-immobilized tetra(4-carboxyphenyl)ferriporphyrin catalysis material

A porphyrin catalytic material, carboxyphenyl technology, applied in the field of preparation of cadmium sulfide-immobilized tetrairon porphyrin catalytic material, can solve the problems of no significant reduction in catalytic efficiency, low catalytic efficiency of metalloporphyrin, and many times of repeated use , to achieve the effects of less metalloporphyrin dosage, improved metalloporphyrin performance and good stability

Active Publication Date: 2016-11-09
GUANGXI UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The present invention provides a preparation of cadmium sulfide-immobilized tetrakis(4-carboxyphenyl)iron porphyrin catalytic material in order to overcome the problems of low catalytic oxidation conversion rate of cyclohexane, low metalloporphyrin catalytic efficiency and low reuse rate etc. Method and application thereof, the prepared cadmium sulfide immobilized tetrakis (4-carboxyphenyl) iron porphyrin catalytic material has the advantages of less metal porphyrin consumption, more reusable times, and no significant reduction in catalytic efficiency after repeated repetitions The advantages

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  • Preparation method and use of cadmium sulfide-immobilized tetra(4-carboxyphenyl)ferriporphyrin catalysis material
  • Preparation method and use of cadmium sulfide-immobilized tetra(4-carboxyphenyl)ferriporphyrin catalysis material
  • Preparation method and use of cadmium sulfide-immobilized tetra(4-carboxyphenyl)ferriporphyrin catalysis material

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Embodiment 1

[0026] A cadmium sulfide immobilized tetrakis (4-carboxyphenyl) iron porphyrin catalytic material is composed of the following raw materials in parts by weight: 124 parts of cadmium nitrate tetrahydrate, 30 parts of thioacetamide, 1780 parts of ethylene glycol, tetra( 0.030 parts of 4-carboxyphenyl) iron porphyrin, 240 parts of absolute ethanol, 118 parts of cyclohexane and 200 parts of deionized water.

[0027] The preparation method of described cadmium sulfide immobilized tetrakis (4-carboxyphenyl) iron porphyrin catalytic material comprises the following steps:

[0028] (1) Preparation of cadmium sulfide: Weigh 124 parts of cadmium nitrate tetrahydrate and 30 parts of thioacetamide respectively, dissolve them in 1780 parts of ethylene glycol, stir magnetically for 4 minutes, heat with microwave for 20 seconds, stop 60s, reheated for 20s, stopped for 60s, repeated heating cycle 19 times, cooled naturally to room temperature, put it in a centrifuge with a rotating speed of 9...

Embodiment 2

[0034] A cadmium sulfide immobilized tetrakis (4-carboxyphenyl) iron porphyrin catalytic material is composed of the following raw materials in parts by weight: 123 parts of cadmium nitrate tetrahydrate, 31 parts of thioacetamide, 1778 parts of ethylene glycol, tetra( 0.032 parts of 4-carboxyphenyl) iron porphyrin, 254 parts of absolute ethanol, 116 parts of cyclohexane and 210 parts of deionized water.

[0035] The preparation method of described cadmium sulfide immobilized tetrakis (4-carboxyphenyl) iron porphyrin catalytic material comprises the following steps:

[0036] (1) Preparation of cadmium sulfide: Weigh 123 parts of cadmium nitrate tetrahydrate and 31 parts of thioacetamide respectively, dissolve them in 1778 parts of ethylene glycol, stir magnetically for 3 minutes, heat with microwave for 21 seconds, stop 61s, reheat for 21s, stop for 61s, and repeat the heating cycle for 18 times, naturally cool to room temperature, put it into a centrifuge with a rotation speed...

Embodiment 3

[0041] A cadmium sulfide immobilized tetrakis(4-carboxyphenyl)iron porphyrin catalytic material is composed of the following raw materials in parts by weight: 125 parts of cadmium nitrate tetrahydrate, 32 parts of thioacetamide, 1779 parts of ethylene glycol, tetra( 0.031 parts of 4-carboxyphenyl) iron porphyrin, 247 parts of absolute ethanol, 120 parts of cyclohexane and 205 parts of deionized water.

[0042] The preparation method of described cadmium sulfide immobilized tetrakis (4-carboxyphenyl) iron porphyrin catalytic material comprises the following steps:

[0043] (1) Preparation of cadmium sulfide: Weigh 125 parts of cadmium nitrate tetrahydrate and 32 parts of thioacetamide respectively, dissolve them in 1779 parts of ethylene glycol, stir magnetically for 5 minutes, heat with microwave for 22 seconds, stop 62s, reheat for 22s, stop for 62s, repeat the heating cycle for 20 times, cool down to room temperature naturally, put it in a centrifuge with a rotation speed of...

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Abstract

The invention discloses a preparation method and use of a cadmium sulfide-immobilized tetra(4-carboxyphenyl)ferriporphyrin catalysis material. The preparation method comprises preparing cadmium sulfide through a microwave method, stirring and dispersing the generated cadmium sulfide in waterless ethanol, adding a waterless ethanol solution of tetra(4-carboxyphenyl)ferriporphyrin into the waterless ethanol solution of cadmium sulfide, heating the mixed solution to a temperature of 60-70 DEG C, carrying out stirring for 5-6h, carrying out pressure reduction pumping filtration to obtain filter cake, carrying out Soxhlet extraction on the filter cake through cyclohexane until the filtrate is colorless, and drying the obtained solids at a temperature of 120-140 DEG C for 10-12h to obtain the catalysis material. The preparation method has simple processes, low energy consumption and a low cost, can be used for production of cyclohexanol and cyclohexanone through catalytic oxygen oxidation of cyclohexane and has a conversion rate of 27.3%. The catalysis material has good catalysis effects, basically keeps catalysis efficiency after cyclic catalysis eight times, has a practical application value and is an ideal biomimetic catalyst.

Description

technical field [0001] The invention relates to the technical field of catalytic materials, in particular to a preparation method and application of a cadmium sulfide immobilized tetrakis(4-carboxyphenyl)iron porphyrin catalytic material. Background technique [0002] The oxidation reaction of cyclohexane mainly produces cyclohexanone and cyclohexanol, both of which are important chemical raw materials, and the mixture of the two is commonly known as KA oil. Cyclohexanone and cyclohexanol are intermediates for the preparation of adipic acid, caprolactam, dyes, paints, pharmaceuticals and other chemicals, and can also be used to prepare rubber anti-aging agents, spices and fruit anti-fungal agents such as phenylphenol. At present, the domestic and international demand for cyclohexanone is very large, and the application of cyclohexanone in the downstream market is becoming more and more extensive. 90% of cyclohexanone in the world is produced by oxidation of cyclohexane. At...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22C07C29/50C07C35/08C07C45/33C07C49/403
CPCB01J31/22B01J2231/72B01J2531/0238B01J2531/842C07C29/50C07C45/33C07C35/08C07C49/403Y02P20/50
Inventor 黄冠刘垚王未来赵树凯郭勇安危素娟
Owner GUANGXI UNIV
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