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Method for continuously and controllably preparing small-size pyrithione granules

A technology of pyrithione salt and pyrithione, which is applied in chemical instruments and methods, chemical/physical/physical chemical processes, organic chemistry, etc., to achieve the effects of simple production process and device, good permeability and small particle size

Inactive Publication Date: 2013-08-14
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved by the present invention is: in the process of preparing small-diameter pyrithione salt particles, in order to simplify the preparation process and avoid the use of dispersants and tedious follow-up particle grinding, crushing and other processing processes, it is proposed to A Rapid, Continuous and Controlled Preparation of Small Pyridinethione Salt Particles by Direct Precipitation in a Microchannel Reactor

Method used

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  • Method for continuously and controllably preparing small-size pyrithione granules
  • Method for continuously and controllably preparing small-size pyrithione granules
  • Method for continuously and controllably preparing small-size pyrithione granules

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0030] Using 0.2mol / L zinc nitrate solution, under the condition that the flow rates of zinc nitrate and sodium pyrithione solution are both 15mL / min, the two are respectively injected into a micro-mixer with an inner diameter of 500 μm and a mixing channel length of 2cm. Preparation of Zinc Pyrithione by Mixed Reaction. Control the reaction temperature to be 80°C, and the molar ratio of raw materials R=2 (R≡n(sodium pyrithione) / n(Zn 2+ )), the corresponding concentration of pyrithione sodium solution is 0.4mol / L. The obtained samples were centrifuged and washed 2-3 times with deionized water, and dried overnight in an oven at 80°C. The sample is denoted as A1. From the scanning electron micrograph of the sample, it was found that the obtained sample was an irregular block (such as Figure 4 ). The average particle size of the sample is 0.48 μm and the particle size distribution is 0.27-0.79 μm according to the electron microscope photos.

example 2-4

[0032]The experiment was carried out in the same manner as Example 1, but the reaction temperature was changed. The reaction temperatures are 20°C, 40°C, and 60°C, respectively, and the zinc pyrithione obtained sequentially is A2, A3, and A4. According to the scanning electron microscope photos of the product, the average particle size and particle size distribution of A2 are 0.90 μm and 0.25-1.99 μm, the average particle size and particle size distribution of A3 are 0.60 μm and 0.22-1.2, and the average particle size distribution of A4 The diameter and particle size distribution are 0.52 μm and 0.2-1.00 μm, respectively. It can be seen that with the increase of reaction temperature, the average particle size of the product decreases and the distribution narrows.

example 5-6

[0034] Experiments were carried out in the same manner as in Example 1, but the raw material molar ratio R was changed. Keep the concentration of zinc nitrate solution at 0.2mol / L, change the R value to 1 and 4 respectively, and the zinc pyrithione obtained in turn is A5, A6. According to the scanning electron microscope photos of the product, the average particle size and particle size distribution of A5 are 0.55 μm and 0.29-0.85 μm, respectively, and the average particle size and particle size distribution of A6 are 0.53 μm and 0.23-0.75 μm, respectively. It can be seen that the R value has little effect on the particle size of the product.

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Abstract

The invention relates to a method for continuously and controllably preparing small-size pyrithione granules. According to the method, pyrithione or a water soluble salt of pyrithione and a polyvalent metal salt solution are respectively fed by respective feeding pumps into a microreactor connected with the pumps and the molar ratio of pyrithione or the water soluble salt of pyrithione to the polyvalent metal salt solution in the microreactor is (0.1-10):1; pyrithione or a water soluble salt of pyrithione and the polyvalent metal salt solution are mixed to carry out chemical precipitation reaction in a mixing channel of the micoreactor at the reaction temperature of 0-100 DEG C, so as to obtain a polyvalent metal salt mixed solution of pyrithione; the mixed solution is separated, washed and dried to finally obtain the polyvalent metal salt granules of pyrithione of which the granule size is controllable and granule size distribution is narrow. The method has the advantages of operation continuity, simple and convenient process and freely changed reaction conditions and the like.

Description

technical field [0001] The invention relates to a method for preparing pyrithione salt with small particle size (average particle size<1 μm), in particular to a method for rapidly, continuously and controllably preparing small particle size pyrithione salt particles through a microchannel reactor. Background technique [0002] Pyridinethione salts have good antibacterial properties, and polyvalent metal salts of pyrithione (such as magnesium, aluminum, zinc, tin, cadmium, zirconium, copper, etc.) can maintain Longer antibacterial activity, and is widely used in coatings, adhesives, antimicrobial agents and shampoos. Among them, zinc pyrithione and copper pyrithione are the most widely used. Use pyrithione (need to add alkali solution, such as sodium / potassium hydroxide or ammonia solution to react to form soluble pyrithione sodium salt, potassium salt or ammonium salt) or soluble pyrithione salt as starting material, and soluble metal compound The reaction to prepare po...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J19/00C07D213/89
Inventor 张利雄吴慧沈如伟王重庆
Owner NANJING UNIV OF TECH
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