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A kind of preparation method of high-content kasugamycin aqueous agent

A technology of high content of kasugamycin, which is applied in the field of pesticides, can solve the problems that the content of kasugamycin is difficult to increase, it is difficult to completely remove ammonium salt, and affect the content of the product, so as to achieve stable properties, complete removal of impurities, and low salt content. low effect

Active Publication Date: 2019-04-02
陕西绿盾生物药业创新中心有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are three main deficiencies in the report. One is the use of saturated ammonium chloride desorption, resulting in a large amount of ammonium salt remaining in the desorption solution, and finally using nanofiltration to remove ammonium. The nanofiltration membrane has a high load and is difficult to completely remove ammonium. salt, and finally a large amount of ammonium salt remains in solution and enters the product
Second, due to the high content of residual salt ammonium chloride, it is difficult to increase the content of kasugamycin in the product, which can only be between 0.5-4%.
Third, nanofiltration can only remove monovalent ions, and divalent ions such as calcium and magnesium brought into the fermentation broth can only remain in the product, forming impurities and affecting the further increase of product content

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] (1) Weigh 2500Kg of 1.50% fermented liquid, adjust the pH to 3.5 with oxalic acid, and filter by ultrafiltration. A total of 3800Kg of the filtrate is filtered out, and the detected content of the mixed liquid is 0.94%.

[0030] (2) Pass 3800Kg of filtrate through 734 sodium resin at a speed of 20m / h to remove impurities.

[0031] (3) Elute with 0.15mol / L NaOH at a speed of 18m / h to obtain 996Kg of a kasugamycin solution with a content of 3.42%, pH=7.4.

[0032] (4) Use 0.15mol hydrochloric acid to adjust the pH to 3.5, use nanofiltration with a pore size of 1 nm, and a molecular weight cut-off of 150-300 to concentrate. When concentrated to 502Kg, the flow rate is reduced to 40% of the initial flow rate, and a conductivity of 9.1 µS / cm is added. 494Kg of pure water continued to be concentrated, and this was repeated three times. After testing, the content was 8.53%, the solid content was 10.59%, and the NaCl content was 0.047%. Stop the machine to obtain a concentrated...

Embodiment 2

[0035] (1) Weigh 2500Kg of 1.03% fermented liquid, adjust the pH to 3.5 with oxalic acid, and filter by ultrafiltration. A total of 3805Kg of the filtrate is filtered out, and the detected content of the mixed liquid is 0.65%.

[0036] (2) Pass 3805Kg of filtrate through 734 sodium resin at a speed of 20m / h to remove impurities.

[0037] (3) Elute with 0.15mol / L NaOH at a speed of 18m / h to obtain 700Kg of a kasugamycin solution with a content of 3.36%, pH=7.4.

[0038] (3) Use 0.15mol hydrochloric acid to adjust the pH to 3.5, use a nanofiltration membrane with a pore size of 1 nm, and a molecular weight cut-off of 150-300 to concentrate. When concentrated to 502Kg, the flow rate is reduced to 40% of the initial flow rate, and the conductivity is less than 9.8µS 494Kg / cm of pure water continued to concentrate, and this was repeated three times. After testing, the content was 8.50%, the solid content was 10.55%, and the NaCl content was 0.047%. Shut down to obtain a concentrate...

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Abstract

The invention relates to a preparation method of a high-content kasugamycin aqueous solution. By the method, high-concentration kasugamycin aqueous solution with the content being 5 to 8 percent can be prepared, the salt concentration of a product is extremely low, the use effect is good, use convenience is achieved, the use requirement of plane prevention with high requirement on concentration can be met, and the storage and transportation cost is low.

Description

technical field [0001] The invention belongs to the field of pesticides, and in particular relates to a preparation method of a high-content kasugamycin aqueous solution. Background technique [0002] Kasugamycin is an aminoglycoside microbial-derived biofungicide pesticide. The product generally exists in the form of kasugamycin monohydrate hydrochloride hydrate. It is mainly used to control rice blast, tomato gray mold, citrus canker and other fungi and Bacterial diseases. Due to the better control effect, kasugamycin is more and more widely used. [0003] As we all know, water agent is the best dosage form of kasugamycin, which has the characteristics of environmental protection, high efficiency and safety. However, the content of kasugamycin aqueous preparations currently registered in the market is generally low, between 2% and 4%. The transportation cost is high, the use is inconvenient, and it cannot meet the booming needs of aerial defense and other aspects; many p...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): A01N43/16A01N25/02A01P1/00A01P3/00C07H15/207C07H1/08
CPCA01N25/02A01N43/16C07H1/08C07H15/207
Inventor 王震
Owner 陕西绿盾生物药业创新中心有限公司