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Method for directly synthesizing nanometer zinc pyrithionewith small particle size

A technology of zinc pyrithione and pyrithione, which is applied in the continuous and controllable preparation of zinc pyrithione with nanometer small particle size, direct synthesis and preparation of zinc pyrithione with small particle size nanometer, fast field, and can solve the problem of increasing subsequent grinding and crushing Problems such as post-processing, unstable particle size and distribution of zinc pyrithione, long feeding time and reaction time, etc., to overcome equipment loss and safety problems, low equipment requirements, and narrow particle size distribution

Inactive Publication Date: 2017-09-08
JIANGSU ZHONGBANG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Zinc pyrithione particles obtained by this method are irregular, have a wide particle size distribution and poor repeatability, and at the same time add cumbersome post-processing processes such as grinding and crushing
U.S. Patent 6,017,936 provides a method for one-time preparation of small particle zinc pyrithione in a high-pressure turbulent flow reactor, but still needs to add an organic dispersant medium in the reaction solution, and simultaneously maintain high pressure and turbulent flow in the reactor. The temperature is controlled at 0-23°C. The reaction conditions of this method are relatively harsh, and the feeding time and reaction time are relatively long.
And Zhang Lixiong (patent No. 103242228A) etc. have invented a kind of method that can continuously synthesize the zinc pyrithione of small particle diameter in microreactor, the zinc pyrithione particle that this method obtains is less, and average particle diameter is 0.2 ~1μm, the particle size distribution is narrow, but due to the small processing capacity and high requirements on equipment, it is difficult to realize industrial production
[0005] In summary, although there are literatures and patents currently reporting methods for synthesizing zinc pyrithione with small particle sizes, some synthesis methods are cumbersome to operate, complex in process, and the particle size and distribution of the prepared zinc pyrithione are unstable; Some conditions are harsh and it is difficult to realize industrial production

Method used

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  • Method for directly synthesizing nanometer zinc pyrithionewith small particle size

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Prepare a zinc nitrate solution with a mass fraction of 20%, turn on the feed pump and the rotating packed bed, the rotating speed of the rotating packed bed is 2000r / min, turn on the water pump, and adjust the circulating water temperature to 80°C. When the temperature of the zinc nitrate reaches 50° C., the feed pump for delivering pyrithione or pyrithione salt solution is started, wherein the prepared pyrithione or pyrithione salt solution has a mass fraction of 20%. Control the liquid flow rate of zinc nitrate to be 200L / h, and the flow rate of pyrithione or pyrithione saline solution to be 200L / h. After the reaction, the zinc pyrithione dispersion was obtained, centrifuged, washed, and then dried to obtain the zinc pyrithione sample A-1. According to the results of the scanning electron microscope, the average particle size was 120nm, and the particle size distribution was 20-300nm.

Embodiment 2-4

[0030] Adopt the method identical with example 1 to carry out experiment, but change the rotating speed of rotating packed bed, be respectively 800r / min, 1200r / min and 1600r / min, obtain zinc pyrithione sample A-2, A-3 and A-4 successively ; The average particle size of A-2 is 900nm, and the particle size distribution is 650nm to 1300nm; the average particle size of A-3 is 530nm, and the particle size distribution is 360nm to 980nm; the average particle size of A-4 is The diameter is 260nm, and the particle size distribution is between 110nm and 580nm. It can be seen that with the increase of the rotating speed of the rotating packed bed, the average particle size decreases and the particle size distribution narrows.

Embodiment 5-7

[0032]Adopt the method identical with example 1 to carry out test, change reaction temperature to be respectively 20 ℃, 40 ℃ and 60 ℃, obtain the average particle diameter successively and be respectively the zinc pyrithione of 300, 230 and 150nm, its particle size distribution is respectively 100~ Between 500nm, 50-450nm and 30-380nm.

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Abstract

The invention discloses a method for directly synthesizing nanometer zinc pyrithionewith small particle size. The method comprises the following basic steps: preparing pyrithione or omadine and a water-solublemetallic zinc compound into aqueous solutionseparately, feeding the preparedpyrithione or omadine and the water-solublemetallic zinc compound into a high gravity reactor through respective liquid inlet tubes, controlling the rotate speed of the high gravity reactor to be 500 to 2100rpm, performing reaction at 0 to 100 DEG C to obtain suspensionmixed liquor, and performing centrifugation, washing and drying on the suspensionmixed liquor, so as to obtain the nanometer zinc pyrithionewith small particle size. The method for directly synthesizing nanometer zinc pyrithionewith small particle sizeavoids the adoption of a dispersing agent and tediousaftertreatment processes, such as subsequent particle grinding and crushing, meanwhile ensures that synthesized zinc pyrithioneparticles are small and the particle size distribution is narrow, and can realize industrial production.

Description

technical field [0001] The present invention relates to the technical field of chemical engineering, in particular to a method for directly synthesizing and preparing zinc pyrithione with nanometer small particle size, in particular to a method for rapidly, continuously and controllably preparing zinc pyrithione with small particle size nanometer by using a supergravity reactor . Background technique [0002] Zinc pyrithione (ZPT), also known as pyridine urn zinc, pyrithione zinc or omatine zinc, 1-nitrogen oxide-2-mercaptopyridine zinc salt, is an excellent anti-scaling agent and anti-greasing agent , has strong lethality to fungi and bacteria, has broad-spectrum, low toxicity, environmental protection and other characteristics, is widely used in shampoo products and coatings and other fields, and has broad market prospects. Especially when used in shampoo, it has good anti-dandruff and anti-itch effect. [0003] There are many research reports on the synthesis process of...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/89B01J19/18B01J4/00
CPCB01J4/001B01J19/006B01J19/18C07D213/89
Inventor 王平丁永山桂清薛谊徐强吴四清李维思
Owner JIANGSU ZHONGBANG PHARMA
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