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Preparation method and application for chitosan-grafted quadri(p-carboxylphenyl) metalloporphyrin

A carboxyphenyl, metalloporphyrin technology, applied in the field of catalyst preparation, can solve the problems of long reaction time, large pollution, low metalloporphyrin reuse rate and the like, and achieves simple preparation, low cost, and improved reuse efficiency. Effect

Inactive Publication Date: 2014-02-05
GUANGXI UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to use tetrakis (4-methoxycarbonylphenyl) metal porphyrin as the core catalyst, and graft it on chitosan by amidation to obtain chitosan grafted tetrakis (p-carboxyphenyl) metal porphyrin Porphyrin, under environment-friendly catalytic conditions, catalyzes air oxidation of ethylbenzene to generate acetophenone and DL-1-phenylethanol, to overcome the large amount of metalloporphyrin existing in the current ethylbenzene oxidation process, too long reaction time, pollution Large, low reuse rate of metalloporphyrins

Method used

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  • Preparation method and application for chitosan-grafted quadri(p-carboxylphenyl) metalloporphyrin
  • Preparation method and application for chitosan-grafted quadri(p-carboxylphenyl) metalloporphyrin
  • Preparation method and application for chitosan-grafted quadri(p-carboxylphenyl) metalloporphyrin

Examples

Experimental program
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Effect test

Embodiment 1

[0029] 1. Preparation of chitosan-grafted tetrakis(p-carboxyphenyl)cobalt porphyrin

[0030] Weigh 0.0209 parts of Co TCPP Cl and add 133.6 parts of dichloromethane and 0.948 parts of N,N-dimethylformamide into a three-neck flask, blow dry nitrogen, heat and stir, add 0.82 parts of thionyl chloride, and heat to reflux for 2 hours . Then add 10 parts of chitosan powder and 200.4 parts of dichloromethane, stir and reflux, react for 3 hours, and stop heating. Filter with suction and wash the filter cake with dichloromethane. The filter cake was then washed with dichloromethane using a Soxhlet extractor to remove unamidated metalloporphyrins. The product was vacuum-dried at 65°C and 0.007MPa for 7 hours to prepare chitosan-grafted tetrakis(p-carboxyphenyl)cobalt porphyrin.

[0031] 2. Application of chitosan grafted tetrakis (p-carboxyphenyl) cobalt porphyrin

[0032] (1) chitosan grafted tetrakis (p-carboxyphenyl) cobalt porphyrin equivalent of 1.0mg tetrakis (p-carboxyphenyl...

Embodiment 2

[0044] Reuse of chitosan grafted tetra(p-carboxyphenyl)cobalt porphyrin

[0045] Chitosan grafted tetrakis (p-carboxyphenyl) cobalt porphyrin equivalent of 0.3 mg tetrakis (p-carboxyphenyl) cobalt porphyrin is put into a 250ml reactor, 200ml ethylbenzene is added, and the reaction temperature is 140 ℃, air pressure 0.8MPa, stirring speed 250 rpm, reaction time 4h, air flow 0.03m 3 / h, the conversion rate of ethylbenzene is 15.81%, the selectivity of alcohol and ketone is 83.23%, and the catalyst conversion number is 6.10×10 5 , The yield of alcohol and ketone is 13.15%. After stopping the catalytic reaction each time, after waiting for the natural sedimentation and separation of the catalytic material and the reaction mixture, filter it, wash it with ethanol, then dry it naturally, reclaim the catalytic material, and then use it to catalyze the air oxidation of ethylbenzene under the same reaction conditions. The repeated utilization of benzene can reach 4 times, and the con...

Embodiment 3

[0047] 1. Preparation of chitosan-grafted tetrakis(p-carboxyphenyl)manganese porphyrin

[0048] Weigh 0.0313 parts of Mn TCPP Cl, add to a three-necked flask containing 133.6 parts of dichloromethane and 1.422 parts of N,N-dimethylformamide, blow in dry nitrogen, stir and heat. Then add 1.23 parts of thionyl chloride and react for 3 hours. Add 200.4 parts of dichloromethane, and then add 15 parts of chitosan powder. After reflux for 3h, filter and wash the filter cake with dichloromethane. Then the filter cake is reflux washed with dichloromethane in a Soxhlet extractor, and the grafted product is then vacuum-dried at a temperature of 56° C., a vacuum degree of 0.010 MPa, and a time of 7 hours to obtain chitosan grafted tetra(p-carboxy phenyl) manganese porphyrin.

[0049] 2. Application of chitosan grafted tetrakis(p-carboxyphenyl)manganese porphyrin

[0050] (1) Chitosan grafted tetrakis (p-carboxyphenyl) manganese porphyrin equivalent of 1.0mg tetrakis (p-carboxyphenyl)...

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Abstract

The invention discloses a preparation method and an application for chitosan-grafted quadri(p-carboxylphenyl) metalloporphyrin. The preparation method comprises the following steps: adding metalloporphyrin in a three-neck flask filled with dichloromethane and N,N-dimethylformamide, charging dry nitrogen, adding thionyl chloride, and heating and stirring; adding chitosan powder and dichloromethane, reacting under heating reflux; performing suction filtration, washing by dichloromethane, then washing off the unamidated metalloporphyrin in a filter cake in a Soxhlet extractor; and performing vacuum drying on the filter cake to obtain the chitosan-grafted quadri(p-carboxylphenyl) metalloporphyrin. The catalytic material, namely the chitosan-grafted quadri(p-carboxylphenyl) metalloporphyrin is simple in preparation method and used for catalyzing ethylbenzene oxidation, easy to separate from a catalytic oxidation product, and capable of being recovered and repeatedly used for catalyzing for at least four times, as well as has an average conversion rate of 13.79-18.42% for ethylbenzene and an average productivity of 10.87-15.51% of ketone alcohol (the sum of acetophenone and 1-phenethyl alcohol).

Description

technical field [0001] The invention relates to a preparation method and application of a catalyst, in particular to a preparation method and application of chitosan grafted tetrakis(p-carboxyphenyl) metalloporphyrin. Background technique [0002] Acetophenone and DL-1-phenylethanol are important chemical raw materials, and have broad application prospects in medicine, pesticides, spices, etc. The traditional method of producing acetophenone is to use benzene as a raw material, and use acetyl chloride or acetic anhydride in a homogeneous Lewis acid (AlCl 3 ,BF 3 ,FeCl 3 ,ZnCl 2 ,SnCl 4 ,TiCl 4 ) or strong protic acid (H 2 SO 4 , HF) catalytic system, which is produced by Friedel-Crafts acylation reaction, which also produces a large amount of toxic and corrosive wastewater. In the past ten years, mesoporous molecular sieves containing cobalt or manganese have been used to catalyze air oxidation of ethylbenzene in acetic acid medium to obtain 25-30% yield of acetophen...

Claims

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Application Information

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IPC IPC(8): C08B37/08B01J31/22C07C27/12C07C49/78C07C45/36C07C33/22C07C29/50
Inventor 黄冠彭艳蔡景莉曾凯危素娟郭勇安赵树凯
Owner GUANGXI UNIV
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