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A kind of purification method of emamectin benzoate

A purification method, a technology of emamectin, applied in chemical instruments and methods, sugar derivatives, organic chemistry, etc., can solve the problems of excessive acetone content, low product purity, low recrystallization yield, etc., and reduce the recovery energy. Consumption, increase economic benefits, reduce the effect of solvent loss

Active Publication Date: 2018-11-27
NINGXIA TAIYICIN BIOTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The acetone recrystallization process is sensitive to temperature changes, and it is prone to precipitation during the fine filtration process of the solution and the crystallization speed is too fast, resulting in the phenomenon of crystal wrapping acetone, resulting in low recrystallization yield, low product purity, and excessive acetone content in the finished product quality
[0005] The process technology of using macroporous resin to purify emamectin benzoate has not been mentioned yet

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Take 500ml of emamectin extract (concentration 700mg / ml), heat up to 38±2°C, add 75ml of saturated sodium chloride solution in an amount of 15% (V / V), fully stir for 40 minutes, and let stand for 20 minutes , divide water, filter, obtain emamectin isopropyl acetate dehydration liquid 460ml (concentration 750mg / ml), add isopropyl acetate solvent 3000ml, dehydration liquid is diluted, obtain diluent 3450ml (concentration 100mg / ml) ,spare.

[0030] Put 3450ml of the above diluent (concentration 100mg / ml) into the macroporous resin LX1600 tank at a temperature of 20-25°C at a speed of 2.0BV / h until the feed liquid is completely fed.

[0031] After feeding the feed liquid, wash it with purified water until it is colorless, and elute it with dichloroethane at a rate of 1.5BV / h. Aminoabamectin dichloroethane eluent, liquid phase detection when the concentration of emamectin reaches about 200 μg / ml, stop elution, combined eluent total 1620ml (concentration 210mg / ml), yield 97....

Embodiment 2

[0037] Take 550ml of emamectin extract (concentration 700mg / ml), heat up to 38±2°C, add 93.5ml of saturated sodium chloride solution in an amount of 17% (V / V), stir for 30 minutes, and let stand for 15 minutes , divide water, filter, obtain emamectin isopropyl acetate dehydration liquid 500ml (concentration 770mg / ml), add isopropyl acetate solvent 3000ml, dehydration liquid is diluted, obtain diluent 3250ml (concentration 120mg / ml) ,spare.

[0038]Put 3250ml of the above diluent (concentration: 120mg / ml) into the macroporous resin LX1600 tank at a temperature of 20-25°C at a speed of 3.0BV / h until the feed liquid is completely fed.

[0039] After feed liquid enters, top wash with purified water to colorless, carry out elution with dichloroethane, elution speed is carried out with 2.0BV / h, after high-performance liquid checks emamectin peak appears, collect formazan Aminoabamectin dichloroethane eluent, liquid phase detection when the concentration of emamectin reaches about 2...

Embodiment 3

[0045] Get 600ml of emamectin extract (concentration 700mg / ml), heat up to 38±2°C, add 120ml of saturated sodium chloride solution in an amount of 20% (V / V), stir for 40 minutes, and let stand for 30 minutes. Divide water, filter, obtain emamectin isopropyl acetate dehydration liquid 540ml (concentration 765mg / ml), add isopropyl acetate solvent 3100ml, dehydration liquid is diluted, obtain diluent 3480ml (concentration 115mg / ml), spare.

[0046] Put 3480ml of the above diluent (concentration 115mg / ml) into the macroporous resin LX1600 tank at a temperature of 20-25°C at a speed of 4.0BV / h until the feed liquid is completely fed.

[0047] After feed liquid enters, top wash with purified water until colorless, carry out elution with dichloroethane, elution speed is carried out with 2.5BV / h, after high-performance liquid checks emamectin peak appears, collect formazan Aminoabamectin dichloroethane eluent, liquid phase detection when the concentration of emamectin reaches about 2...

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PUM

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Abstract

The invention relates to an emamectin benzoate purifying method which comprises the following steps: pretreating a methylamino abamectin extract; performing macroporous resin adsorption and dichloroethane analysis; performing reduced pressure distillation of the obtained analysis liquid to remove dichloroethane; adding an isopropyl acetate solution and dissolving; adding a sodium chloride saturated solution, and sufficiently stirring; standing, separating water and filtering with an ultrafiltration membrane to obtain methylamino abamectin refined liquid; and performing a salt forming reaction between the refined liquid and a benzoic acid solution. In the invention, the methylamino abamectin extract is purified by use of the macroporous resin, the purity of the product emamectin benzoate of the salt forming reaction between the methylamino abamectin and benzoic acid is not less than 90%, the yield of the salt forming reaction between the purified methylamino abamectin and benzoic acid is increased by 6%, and the output and economic benefits are increased; and moreover, acetone is not adopted for recrystallization, the solvent loss is reduced, and the solvent recycling energy consumption is lowered.

Description

technical field [0001] The invention belongs to the technical field of antibiotic extraction, in particular to a method for purifying emamectin benzoate. Background technique [0002] Emamectin benzoate is a derivative of abamectin, a biological fermentation product. The common name in English is emamectin benzoate, and the trade name is emamectin. It is a mixture of emamectin B1a and B1b, the molecular formula is C 49 h 75 NO 13 ·C 7 h 6 o 2 and C 48 h 73 NO 13 ·C 7 h 6 o 2 , compared with the parent (abamectin), its biological activity has increased by 1 to 3 orders of magnitude, and it has the characteristics of ultra-efficient, low toxicity, low residue, and pollution-free biological pesticides. It is widely used in the control of various pests on vegetables, fruit trees, cotton and other crops. At the same time, emamectin emamectin is also a highly efficient, broad-spectrum, safe poultry and livestock repellent, which can be widely used in the treatment of ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H17/08C07H1/06
CPCC07H1/06C07H17/08Y02P20/10
Inventor 裴立忠王勇平张鹏张江飞
Owner NINGXIA TAIYICIN BIOTECH CO LTD