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Synthesis method of copper pyrithione

A technology of copper pyrithione and synthesis method, applied in chemical instruments and methods, chemical recovery, molecular sieve catalysts and other directions, can solve problems such as punching materials, and achieve the effects of simple process operation, reduction of production cost, reduction of waste water volume and COD

Active Publication Date: 2012-10-03
NANTONG ACETIC ACID CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For subsequent reactions, the excess hydrogen peroxide must be destroyed, otherwise it is easy to cause dangers such as punching

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0045] The preparation synthesis steps of described catalyst are as follows:

[0046] Dissolve cetyltrimethylammonium bromide and sodium silicate in hot water to obtain a clear solution, adjust the pH value to 8~9, add the aqueous solution of chloride of metal A and the aqueous solution of B salt of metal B dropwise Into the above solution, then adjust the pH to 9.0~9.5, and finally add the aqueous solution of metal C carbonate dropwise, after stirring evenly, transfer the obtained mixed sol into an autoclave, and conduct a hydrothermal reaction at 120~180°C for 24~48h, Allow it to cool down to room temperature naturally, wash it with deionized water first, then with absolute ethanol, and dry at room temperature to obtain the original catalyst powder. The original powder is calcined in a muffle furnace at 550-600°C, and then cooled naturally to obtain the catalyst.

[0047] The specific examples of preparing the catalyst are as follows:

Embodiment 1

[0049] Dissolve 25g of trimethylhexadecylammonium bromide in 200ml of deionized water, keep stirring at 20~60°C for 30 minutes, add 50g of Na 2 SiO 3 , stir well, use dilute H 2 SO 4 The pH of the solution was adjusted to 8.5, and then 60 ml of an aqueous solution containing 7.5 g of titanium trichloride was added dropwise to the above solution under vigorous stirring, and then 220 ml of an aqueous solution of sodium stannate containing 30.0 g of sodium stannate trihydrate was added dropwise. Adjust the pH to 9.0~9.5 with ammonia water, and finally add 40ml of an aqueous solution containing sodium tungstate dihydrate 19.0. Stir the obtained mixed sol for 2 hours and then transfer it to a stainless steel autoclave for hydrothermal reaction at 120°C for 24 hours. After the reaction, cool to room temperature with water, filter the product, wash with deionized water and absolute ethanol three times, and dry at room temperature The raw catalyst powder is obtained. The original ...

Embodiment 2

[0051] Dissolve 25g of trimethylhexadecylammonium bromide in 200ml of deionized water, keep stirring at 20~60°C for 30 minutes, add 50g of Na 2 SiO 3 , stir well, use dilute H 2 SO 4 Adjust the pH of the solution to 8.5, then add dropwise 40ml of an aqueous solution containing 5g of titanium trichloride to the above solution under vigorous stirring, then add dropwise 150ml of an aqueous solution of sodium stannate containing 20.0g of sodium stannate trihydrate, and use ammonia water to Adjust the pH to 9.0~9.5, and finally add 25ml of an aqueous solution containing sodium tungstate dihydrate 12.7. Stir the obtained mixed sol for 2 hours, then transfer it to a stainless steel autoclave, and conduct a hydrothermal reaction at 150°C for 48 hours. After the reaction, cool to room temperature with water, filter the product, wash three times with deionized water and absolute ethanol, and dry at room temperature The raw catalyst powder is obtained. The original powder was calcine...

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Abstract

The invention relates to a synthesis method of copper pyrithione, which is characterized by comprising the following steps: (1) 2-chloropyridine oxidization: adding 2-chloropyridine and a catalyst into a container, and dropwisely adding hydrogen peroxide; (2) filtering the solution obtained in the step (1), carrying out vacuum drying on the filter cake, washing the filter cake, and carrying out vacuum drying on the filter cake again, wherein the obtained filter cake is the catalyst used in the step (1), and the filtrate is a 2-chloropyridine oxynitride solution; and (3) preparation of copper pyrithione. By using the synthesis method provided by the invention, the oxidization yield of 2-chloropyridine is enhanced from 80% to 98%, the total yield is enhanced from 75% to 93%, the product quality is enhanced from 95-96% to more than 98%, and the recycled catalyst can be used repeatedly; and thus, the raw material consumption is reduced, the production cost is lowered, the technological operation is simple, and the wastewater amount and COD (chemical oxygen demand) are obviously reduced.

Description

technical field [0001] The invention belongs to the field of chemical industry and relates to a preparation process, in particular to a method for synthesizing copper pyrithione. Background technique [0002] Copper pyrithione (CPT), alias: Omedin copper, molecular formula: C 10 h 8 N 2 o 2 S 2 Cu, molecular weight: 315.9, appearance is green powder solid, pH value: 6.0~8.0. [0003] Copper pyrithione is a high-efficiency, low-toxicity, mildew-proof and fungicide used in ship antifouling paints to prevent crustaceans, seaweeds and aquatic organisms from adhering to hull plates. It is also used in the production of daily chemical products, adhesives, paints, coatings, papermaking, medicine, leather and other industries. It is also widely used. [0004] The existing synthesis technology process of copper pyrithione mainly contains following 3 kinds: [0005] ①Using 2-aminopyridine as the starting material, 2-mercaptopyridine-N-oxide was synthesized through acetylation,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/89B01J29/03
CPCY02P20/584
Inventor 丁彩峰林民朱小刚刘芳吴慰祖舒兴田周新建薛建锋王健华朱双双
Owner NANTONG ACETIC ACID CHEM
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