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Method for preparing catalysis material for synthesizing tetraphenylporphyrin

A technology of tetraphenylporphyrin and catalytic material, applied in chemical instruments and methods, organic compound/hydride/coordination complex catalyst, physical/chemical process catalyst, etc., can solve the problem of small effective catalytic area and reduced yield , easy residue and other problems, to achieve uniform and controllable pH, reduce waste of raw materials, and good chemical resistance.

Inactive Publication Date: 2018-06-15
孝感市锐思新材科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The existing tetraphenylporphyrin production process mostly uses a single acid catalyst to catalyze the synthesis reaction, which has the disadvantages of being easy to remain in the product, the effective catalytic area is small, and the acidity is too strong to cause the protonation of pyrrole and reduce the yield. A new type of porphyrin is developed. The catalyst is beneficial to simplify the process of producing tetraphenylporphyrin products and improve its yield

Method used

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  • Method for preparing catalysis material for synthesizing tetraphenylporphyrin

Examples

Experimental program
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Effect test

Embodiment 1

[0016] Step 1. Preparation of the composition

[0017] In the reaction kettle, add 1000g of N,N-dimethylformamide, 60g of p-phenylazoamine-4-sulfonic acid, 27.5g of 3,3'-dicarboxydiphenyl disulfide, 1-propylsulfonic acid Acid-3-methylimidazolium trifluoromethanesulfonate 0.05 g, (S)-2-(diphenyl(trimethylsilyloxy)methyl)pyrrolidine 0.05 g, and mix well at room temperature.

[0018] Step 2. Preparation of Catalyst

[0019] Add 1000g of styrene-based macroporous weakly acidic cation exchange resin, 200g of the composition prepared in step 1, 50g of iron tetrafluoroborate, 1150g of N,N-dimethylformamide into the reaction kettle, heat up to 87°C, and keep it warm for 13h , after the completion, the product is taken out, washed with water, and dried to obtain a catalytic material for synthesizing tetraphenylporphyrin.

Embodiment 2

[0021] Step 1. Preparation of the composition

[0022] In the reaction kettle, add 1000g of N,N-dimethylformamide, 30g of p-phenylazoamine-4-sulfonic acid, 5g of 3,3'-dicarboxydiphenyl disulfide, 1-propylsulfonic acid -0.01 g of 3-methylimidazolium trifluoromethanesulfonate, and 0.01 g of (S)-2-(diphenyl(trimethylsilyloxy)methyl)pyrrolidine, and mix well at room temperature.

[0023] Step 2. Preparation of Catalyst

[0024] Add 1000g of styrene-based macroporous weakly acidic cation exchange resin, 100g of the composition prepared in step 1, 20g of iron tetrafluoroborate, 800g of N,N-dimethylformamide into the reaction kettle, heat up to 80°C, and keep it warm for 6h , after the completion, the product is taken out, washed with water, and dried to obtain a catalytic material for synthesizing tetraphenylporphyrin.

Embodiment 3

[0026] Step 1. Preparation of the composition

[0027] In the reaction kettle, add 1000g of N,N-dimethylformamide, 90g of p-phenylazoamine-4-sulfonic acid, 50g of 3,3'-dicarboxydiphenyl disulfide, 1-propylsulfonic acid -0.1 g of 3-methylimidazolium trifluoromethanesulfonate, and 0.1 g of (S)-2-(diphenyl(trimethylsilyloxy)methyl)pyrrolidine, and mix well at room temperature.

[0028] Step 2. Preparation of Catalyst

[0029] Add 1000g of styrene-based macroporous weakly acidic cation exchange resin, 300g of the composition prepared in step 1, 80g of ferric tetrafluoroborate, 1500g of N,N-dimethylformamide into the reaction kettle, raise the temperature to 95°C, and keep it warm for 20h , after the completion, the product is taken out, washed with water, and dried to obtain a catalytic material for synthesizing tetraphenylporphyrin.

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Abstract

The invention provides a method for preparing a catalysis material for synthesizing tetraphenylporphyrin. The method comprises the following steps: putting a styrene series macroporous weakly acidic cation exchange resin in parts by weight into a reaction kettle, heating the composition obtained in the step 1, ferrocenium tetrafluoroborate and N,N-dimethyl formamide, taking out a product after heating is completed, washing with water, and drying, thereby obtaining the catalysis material for synthesizing tetraphenylporphyrin. The catalysis material generated by using the method has the advantages that the pH value of a tetraphenylporphyrin production system is uniform and controllable, and the tetraphenylporphyrin is not liable to crush, is easy to separate and is not easily mixed with impurities.

Description

technical field [0001] The invention relates to a preparation method of a catalyst, in particular to a preparation method of a catalytic material for synthesizing tetraphenylporphyrin. Background technique [0002] Porphyrin compounds have a certain degree of aromaticity, good stability, wide spectral response, and strong ability to complex metal ions because of their parent porphin, which is mainly rigid and has a flexible macrocyclic conjugated junction. Dark crystal with high melting point. Due to the special structure and properties of porphyrin compounds, they have a wide range of uses. For example, natural porphyrin compounds have special physiological activities, and many functions in the life process are related to metalloporphyrins. Therefore, it has become an important research topic to artificially synthesize porphyrins of various structures to simulate various properties of natural porphyrin compounds. . In addition, it has very broad application prospects in ...

Claims

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Application Information

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IPC IPC(8): B01J31/30C07D487/22
CPCB01J31/30C07D487/22
Inventor 王大可谷灿波
Owner 孝感市锐思新材科技有限公司
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