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Preparation method of phthalocyanine cobalt sulfonamide desulfurization catalyst

A technology of cobalt phthalocyanine sulfonamide and desulfurization catalyst, which is applied in the field of preparation of new desulfurization catalyst-cobalt phthalocyanine sulfonamide, can solve the problems of phthalic anhydride affecting the yield and product quality, and achieve long catalytic cycle, high-efficiency desulfurization activity, The effect of process simplification

Inactive Publication Date: 2011-11-30
SHANDONG ANALYSIS & TEST CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The used raw material of this technique is cheap, but also has following shortcoming: one, the sublimation of phthalic anhydride influences productive rate
In addition, since calcium sulfate is slightly soluble in water, the product contains calcium sulfate and affects product quality.

Method used

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  • Preparation method of phthalocyanine cobalt sulfonamide desulfurization catalyst

Examples

Experimental program
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Effect test

Embodiment 1

[0021] Take 300g of phthalic anhydride and 600g of chlorosulfonic acid, reflux and sulfonate at 180°C for 8 hours, recover excess chlorosulfonic acid under reduced pressure, add the residue to 1000g of ice water, and filter to obtain the intermediate product, phthalic anhydride sulfonate Acid chloride, yield 67.5%. The recovered chlorosulfonic acid can be used mechanically again.

[0022] Then take 246g of phthalic anhydride sulfonyl chloride, 36g of pyromellitic anhydride, 300g of urea, 43.3g of anhydrous cobalt chloride, 6.5g of ammonium molybdate, and undergo condensation reaction at 190-220°C for 4 hours to generate cobalt phthalocyanine Sulfonamide, the product is dark blue solid.

Embodiment 2

[0024] Take 300g of phthalic anhydride and 400g of chlorosulfonic acid, reflux and sulfonate them at 180°C to 200°C for 8 hours, then add 300g of thionyl chloride and continue reflux for 3 hours, and recover excess thionyl chloride and chlorine under reduced pressure. Sulfonic acid, the residue was added to 1000g ice water, and the intermediate product phthalic anhydride sulfonyl chloride was obtained by filtration. Yield 87.6%. The recovered thionyl chloride and chlorosulfonic acid can be used again after simple fractionation and separation.

[0025] Take 246g of the intermediate product phthalic anhydride sulfonyl chloride, 36g of pyromellitic anhydride, 300g of urea, 43.3g of anhydrous cobalt chloride, 6.5g of ammonium molybdate, and undergo condensation reaction at 190-220°C for 4 hours to generate cobalt phthalocyanine sulfonate Amide, the product is dark blue solid.

Embodiment 3

[0027] Take 300g of phthalic anhydride, recover 600g of chlorosulfonic acid, reflux and sulfonate at 180°C for 8 hours, recover excess chlorosulfonic acid under reduced pressure, add the residue to 1000g of ice water, and filter to obtain the intermediate product of phthalic anhydride Sulfonyl chloride, yield 58.3%. The recovered chlorosulfonic acid can be used mechanically again.

[0028] Then take 246g of phthalic anhydride sulfonyl chloride, 36g of pyromellitic anhydride, 300g of urea, 43.3g of anhydrous cobalt chloride, 6.5g of ammonium molybdate, and undergo condensation reaction at 190-220°C for 4 hours to generate cobalt phthalocyanine Sulfonamide, the product is dark blue solid.

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Abstract

The invention relates to a method for preparing a cobalt phthalocyanine sulfonamide desulfurization catalyst, comprising the steps of: adding chlorosulfonic acid or chlorosulfonic acid into thionyl chloride and carrying out sulfonation through taking phthalic anhydride as a raw material so as to obtain phthalic anhydride sulfonyl chloride; and subjecting the obtained product and pyromellitic formic anhydride, urea, anhydrous cobalt chloride and ammonium molybdate to condensation reaction so as to obtain dinuclear cobalt phthalocyanine sulfonamide. By means of the preparation method provided by the invention, the problems of phthalic anhydride sublimation, sulfuric acid neutralization and separation and the like caused in conventional productive processes of sulfonated cobalt phthalocyanine are avoided and the preparation method has the characteristics of mild production condition, simple production process, recoverability of excessive raw materials and the like. The obtained cobalt phthalocyanine sulfonamide desulfurization catalyst can be applied to catalytic oxidation removing processes of organic sulfur and inorganic sulfur and has the characteristics of high activity, high selectivity, easiness in regeneration and the like.

Description

technical field [0001] The invention relates to a preparation method of a novel desulfurization catalyst-cobalt phthalocyanine sulfonamide, belonging to the technical field of synthesis of phthalocyanine catalysts. Background technique [0002] The desulfurization treatment in petrochemical and coal chemical production, especially the desulfurization of coke oven gas and petroleum gas, has widely used the catalytic oxidation method in the wet method, among which the PDS method using sulfonated cobalt phthalocyanine as the catalyst is the most concerned. The PDS method is a new type of desulfurization process developed in recent years, which has a good removal effect on most organic and inorganic sulfur. The phthalocyanine cobalt series catalyst used in the PDS method is a new type of high-efficiency catalyst. It has been widely used in the desulfurization and deodorization of low- and high-sulfur gases and low-viscosity liquids. It has obvious effects on hydrogenated gasolin...

Claims

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Application Information

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IPC IPC(8): B01J31/22C07D487/22
Inventor 高乾善纪文华
Owner SHANDONG ANALYSIS & TEST CENT
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