Zinc thiazole preparation method used for reducing impurity content of zinc thiazole

A technology of thiazole zinc and thiadiazole, which is applied in the field of preparation of thiazole zinc to reduce the impurity content in thiazole zinc, can solve problems such as difficulty in industrial implementation, difficulty in meeting production requirements, complexity, etc.

Active Publication Date: 2019-07-09
JIANGSU XINNONG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method is very complicated and difficult to implement in industry. Although it solves the

Method used

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  • Zinc thiazole preparation method used for reducing impurity content of zinc thiazole
  • Zinc thiazole preparation method used for reducing impurity content of zinc thiazole
  • Zinc thiazole preparation method used for reducing impurity content of zinc thiazole

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Embodiment 1: prepare thiazole zinc by high pH value thiadiazole sodium solution

[0038] The thiadiazole salt solution is prepared by using different initial concentrations of sodium hydroxide solution. The specific method is to dissolve sodium hydroxide in water and add water to 100ml, then add a certain amount of solid thiadiazole, and heat to 80°C for 30 minutes to obtain thiadiazole salt solution. Diazol sodium solution.

[0039] The pH value of the final solution of the thiadiazole sodium solution is controlled by adjusting the addition amount of thiadiazole, and the pH value is adjusted at 12-15.

[0040] Specifically, the different sodium hydroxide concentrations and the pH value of the final thiadiazole sodium solution are as shown in Table 1.

[0041] The preparation of table 1 high concentration thiadiazole sodium solution

[0042]

[0043]

[0044] Apply above-mentioned thiadiazole sodium solution to prepare thiazole zinc, zinc salt adopts zinc sulfa...

Embodiment 2

[0051] Embodiment 2: low pH thiadiazole sodium solution prepares thiazole zinc

[0052] Prepare thiazole zinc in the same way as in Example 1. When adjusting the pH value of the thiadiazole sodium solution, the pH value of the final solution of the thiadiazole salt solution is controlled between 8-13 by adjusting the amount of thiadiazole added.

[0053] Specifically, the pH values ​​of different sodium hydroxide concentrations and the final thiadiazole sodium solution are shown in Table 3 below.

[0054] The preparation of table 3 high concentration thiadiazole sodium solution

[0055] serial number Sodium hydroxide concentration (g / L) Thiadiazole Sodium Solution pH L01 60 8.02 L02 70 8.14 L03 80 8.54 L04 90 9.32 L05 100 10.35 L06 110 11.43 L07 120 12.54

[0056] Apply above-mentioned thiadiazole sodium solution to prepare thiazole zinc, zinc salt adopts zinc sulfate, the molar concentration of thiadiazole sodium sol...

Embodiment 3

[0061] Embodiment 3: other condition control in preparing thiazole zinc

[0062] In the preparation process of embodiment 1 and embodiment 2, thiadiazole sodium solution is replaced by other thiadiazole alkaline solutions, zinc sulfate solution is replaced by other zinc salt solutions, by controlling the pH of thiadiazole salt solution value and the pH value in the reaction system to detect the content of impurity zinc hydroxide and impurity thiadiazole in the zinc thiazole product, the relationship between its pH value and impurity content and the relationship with the yield are the same as in Example 1 and 2 results trend.

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Abstract

The invention relates to a zinc thiazole preparation method used for reducing impurity content of zinc thiazole. The zinc thiazole preparation method used for reducing impurity content of zinc thiazole comprises following steps: A, an alkali solution is adopted to dissolve thiadiazole to form a thiadiazole salt solution; and B, the thiadiazole salt solution and a zinc salt solution are subjected to mixing reaction to obtain zinc thiazole; wherein in the step A, the pH value of the thiadiazole salt solution is 9 to 14, and in the step B, the pH value of the thiadiazole salt solution and the zinc salt solution mixed reaction solution system is 8 to 13. The zinc thiazole preparation method is adopted in study of factors in zinc thiazole preparation process influencing generation of impurity zinc hydroxide and impurity thiadiazole, and raw material solution pH value and reaction process pH value are adjusted to solve the problems in the prior art.

Description

technical field [0001] The invention belongs to the field of fine chemicals, and in particular relates to a preparation method of zinc thiazole for reducing the impurity content in zinc thiazole. Background technique [0002] In the present invention, thiazole zinc is two (2-amino-5-mercapto-1,3,4-thiadiazole) zinc, and its chemical formula is: [0003] [0004] In the present invention, the raw material used for the preparation of thiazole zinc is 2-amino-5-mercapto-1,3,4-thiadiazole (hereinafter referred to as "thiadiazole"), and the CAS number of thiadiazole is 2349-67-9 , its structural formula is as follows: [0005] [0006] Patent CN1152869C discloses thiadiazole metal complexes and their preparation methods and uses. The preparation method of the disclosed thiazole zinc is as follows: first place 60ml of water in a 100ml beaker, add 18g of sodium hydroxide, stir to dissolve, and then add Stir 54g of the above-mentioned thiadiazole to obtain completely dissolv...

Claims

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Application Information

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IPC IPC(8): C07D285/135
CPCC07D285/135
Inventor 杨宏武应毅戴金贵徐群辉
Owner JIANGSU XINNONG CHEM
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