CN107787963A - A kind of preparation method of anti-caking AVM toluene ointment - Google Patents
A kind of preparation method of anti-caking AVM toluene ointment Download PDFInfo
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- CN107787963A CN107787963A CN201710529962.XA CN201710529962A CN107787963A CN 107787963 A CN107787963 A CN 107787963A CN 201710529962 A CN201710529962 A CN 201710529962A CN 107787963 A CN107787963 A CN 107787963A
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- avm
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/02—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing liquids as carriers, diluents or solvents
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/34—Shaped forms, e.g. sheets, not provided for in any other sub-group of this main group
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/90—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having two or more relevant hetero rings, condensed among themselves or with a common carbocyclic ring system
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- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Dentistry (AREA)
- Plant Pathology (AREA)
- Engineering & Computer Science (AREA)
- Pest Control & Pesticides (AREA)
- Agronomy & Crop Science (AREA)
- Wood Science & Technology (AREA)
- Zoology (AREA)
- Environmental Sciences (AREA)
- Toxicology (AREA)
- Medicinal Preparation (AREA)
Abstract
The present invention relates to a kind of preparation method of anti-caking AVM toluene ointment, this method uses can prevent from luming to a certain amount of polar solvent of ointment addition, but the addition of polar solvent can excessively influence the emulsifying effectiveness of AVM, the preparation method of the present invention both prevented avermectin B2a from being separated out in ointment, so as to solve AVM toluene ointment caking problem, while it in turn ensure that the emulsifying effectiveness of AVM is unaffected.
Description
Technical field
The present invention relates to a kind of preparation method of anti-caking AVM toluene ointment, belongs to biological pesticide technology of preparing neck
Domain.
Background technology
Abamectin emulsifiable concentrate is a kind of common pesticidal preparations, is widely used in agricultural, as insecticide, for preventing and treating ten
The small food heart of Zi Hua sections diamondback moth, pear tree pear sucker, cotton red spider, phyllocnistis citrella stainton blister mite, cotton boll worm, apple tree peach
Worm and Tetranychus urticae, cabbage caterpillar etc..Abamectin emulsifiable concentrate is typically relatively stable, and 2 years contents of storage at normal temperature are qualified, emulsifiability
Well.And abamectin ointment is to prepare the indispensable composition of missible oil, still, agricultural chemicals enterprise production abamectin ointment, hold
Easily lump, g., jelly-like is presented, serious can not even be filled in bucket；Or after barrelling, during storage, bucket bottom by
Gradually there is one layer of caking, in addition it is rotten turn into g., jelly-like, can not be poured out from bucket, cause downstream product of returning goods or have a strong impact on,
Particularly the relatively low north of winter temperature, this denaturalization phenomenon are more serious.Although novel form sec-Butyl Acetate ointment can solve
The problem of certainly luming, but sec-Butyl Acetate ointment cost is higher, and new emulsifier research and development time length, along with pesticide producing, producer makes
With the emulsifying agent relative maturity of benzene class ointment, the acceptance of the secondary butyl ester ointment of Dichlorodiphenyl Acetate is low, so benzene kind solvent in the market
Ointment occupation rate of market it is still higher.
Therefore, the agglomeration problems for solving AVM toluene ointment are urgently to be resolved hurrily in face of numerous pharmacy corporations as putting
Outstanding problem.
The content of the invention
In view of the shortcomings of the prior art, the present invention provides a kind of preparation method of anti-caking AVM toluene ointment.
Term explanation：
AVM primary crystallization mother liquor：It is to be completed by prior art using the wholesale ferment of A Foman streptomycetes, fermentation period
For 260~270 hours abamectin fermented liquid obtained, by squeezing, drying, extracting, concentrating the processes such as decrease temperature crystalline, through from
The centrifuge mother liquor obtained after the heart, 13000~14000u/ml of mother liquor potency.
Dehydration：Dehydration of the present invention refers to the free moisture removed in raw material, makes the mass content ＜ 1% of moisture.
Technical scheme is as follows：
A kind of preparation method of anti-caking AVM toluene ointment, including step are as follows：
(1) AVM centrifuge mother liquor is concentrated into no methanol solvate, by AVM centrifuge mother liquor：The body of esters solvent
Product is than being 1：2~3 ratio is extracted AVM centrifuge mother liquor addition esters solvent, and AVM centrifuge mother liquor is complete
It is dissolved in esters solvent, obtains extraction feed liquid；
(2) hot water is added into extraction feed liquid and carries out washing desugar, repetition is washed to water layer printing opacity >=30%, obtains desugar material
Liquid；
(3) desugar feed liquid is dehydrated and is filtered to remove solid impurity, obtain removal of impurities feed liquid；
(4) removal of impurities feed liquid is cooled to 20 DEG C, is then at the uniform velocity cooled using refrigerant, be cooled to 0-5 DEG C, must crystallized
Liquid；
(5) by crystal solution centrifugal treating, AVM secondary mother liquid is obtained, AVM secondary mother liquid is concentrated into
Without esters solvent；
(6) by AVM secondary mother liquid in the AVM secondary mother liquid obtained to step (5)：The volume ratio of toluene is
1：2~3 ratio adds toluene and extracted, and AVM secondary mother liquid is dissolved completely in toluene, obtains toluene extraction feed liquid；
(7) after toluene extraction feed liquid being concentrated into ointment shape, the intensive polar solvent of ointment volume 2%~3% is added, is produced
The AVM toluene ointment of anti-caking.
According to currently preferred, in step (1), AVM centrifuge mother liquor：The volume ratio of esters solvent is 1：2.5.
According to currently preferred, in step (1), extraction temperature is 65~70 DEG C, is carried out under agitation.
According to currently preferred, in step (1), esters solvent is butyl acetate, isopropyl acetate or ethyl acetate.
According to currently preferred, in step (2), the addition volume of hot water is the 1/2~1/4 of extraction material liquid volume.
According to currently preferred, in step (2), the temperature of hot water is 85~90 DEG C, it is preferred that the temperature of hot water is 86
~88 DEG C, washing times are 3-5 times.
According to currently preferred, in step (3), it is dehydrated to be 0.06~0.07Mpa in vacuum, temperature is 80~85
Carried out under the conditions of DEG C.
According to currently preferred, the step (4), being cooled to 0-5 DEG C is dropped with 2-3 DEG C/h of rate of temperature fall
Temperature, whole temperature fall time control is in 5-10 hours.
According to currently preferred, the step (5), concentration is in 0.06~0.07MPa vacuums, 80~85 DEG C of conditions
Lower progress.
According to currently preferred, the step (6), AVM secondary mother liquid：The volume ratio of toluene is 1：2.5.
According to currently preferred, the step (7), concentration is in 0.06~0.07Mpa vacuums, 70~80 DEG C of conditions
Lower progress.
According to currently preferred, the step (7), intensive polar solvent is methanol, ethanol or dimethylformamide (DMF)
Middle one of which or any two or more mixing.
According to currently preferred, the step (7), the addition volume of intensive polar solvent is the 2% of ointment volume.
Step (2) of the present invention with purified water carry out wash desugar main purpose be will extract feed liquid in glycoprotein it is thorough
Removing.
Step (7) of the present invention is from the polar solvent strong to avermectin B2a dissolubility as AVM toluene ointment
Adjuvant.
The raw material AVM centrifuge mother liquor of the present invention can be bought by market, can also be prepared by prior art.
The method have the advantages that：
1st, found during the inventive method is realized, detection and analysis discovery is carried out to toluene ointment, cause caking existing
As the reason for be due to that B2a contents are higher in ointment, with the reduction of storage temperature, avermectin B2a is molten in nonpolar toluene
Agent easily reaches saturation precipitation and causes caking, jelly phenomenon, and preparation method of the invention takes esters solvent extraction by crude oil cream
B2a contents are down to less than 10% from 25-30% or so, greatly reduce the phenomenon of ointment caking.
2nd, preparation method of the invention uses can prevent from luming to a certain amount of polar solvent of ointment addition, but polarity is molten
The addition of agent can excessively influence the emulsifying effectiveness of AVM, and preparation method of the invention had both prevented avermectin B2a in oil
Separated out in cream, so as to solve AVM toluene ointment caking problem, while in turn ensure that the emulsifying effectiveness of AVM not by
Influence.
3rd, preparation method equipment of the invention is simple and easy, and the adjuvant dosage added is small, and not to product in itself
And the inherent quality of downstream product impacts, there is obvious economic benefit and promotional value.
4th, under subzero 20 DEG C of low temperature, nodeless mesh separates out AVM toluene ointment made from the inventive method, remains to protect
Such as normal temperature state, bucket bottom is held not freeze without caking, be more applicable for north of china in winter storage.
Raw materials used and equipment of the invention is prior art.
Advantages of the present invention is as follows：
Brief description of the drawings：
Fig. 1 is by B2a content chromatograms in present invention process extraction ointment；Retention time 4.645 is B2a peaks retention time
9.158 it is B1a peaks
Fig. 2 does not carry out the abamectin ointment chromatograms of B2a extractions；Retention time 4.661 is B2a peaks retention time
9.149 it is B1a peaks
Embodiment
Below by specific embodiment, the present invention will be further described, but not limited to this.
It is conventional existing equipment to implement device therefor.
The raw material used in embodiment, commercially available prod.
Embodiment 1
A kind of preparation method of the AVM toluene ointment of anti-caking, this method comprise the following steps：
(1) the AVM centrifuge mother liquor that potency is 15000u/ml is successively returned in alcohol evaporator and crystallizing tank in economic benefits and social benefits
No methanol solvate is concentrated in vacuo to, AVM centrifuge mother liquor is pressed with esters solvent：The volume ratio of toluene is 1：2 are extracted
Take, stir, and be warming up to 70 DEG C, after feed liquid is completely dissolved, obtain extraction feed liquid；
(2) purified water that the extraction amount of material liquid volume 1/2 is added into extraction feed liquid carries out washing desugar, adds purified water
Afterwards, stir 30 minutes, static 1 small layered, separate water layer, repeat washing 4 times, measure the 3rd, the 4th time water layer printing opacity difference
For 26%, 35%, desugar feed liquid is obtained；Described purifying coolant-temperature gage is 85 DEG C；
(3) be 0.06~0.07Mpa in vacuum in crystallizing tank by desugar feed liquid, temperature be dehydrated under the conditions of 85 DEG C to
Crystallizing tank visor obtains removal of impurities feed liquid without solid impurity is filtered to remove with plate and frame filter press after the globule；
(4) removal of impurities feed liquid is cooled to 20 DEG C at full speed, then at the uniform velocity cooled using refrigerant, control 3 DEG C/h, drop
Warm to 2 DEG C, about 6 hours whole used times；
(5) by the removal of impurities feed liquid after cooling by centrifuge obtain AVM secondary mother liquid vacuum be 0.06~
0.07MPa, temperature are carried out under the conditions of 85 DEG C, are concentrated into no esters solvent solvent；
(6) AVM concentrated mother liquor is pressed into AVM concentrated mother liquor with toluene：The volume ratio of toluene is 1：2 are extracted
Take to AVM centrifuge mother liquor and be dissolved completely in toluene；
(7) it is 0.06~0.07MPa in vacuum by mother liquor, after temperature is concentrated into ointment shape under the conditions of 75 DEG C, adds
The methanol of ointment volume 2% produces AVM toluene ointment as adjuvant.
Embodiment 2：
The preparation method of the AVM toluene ointment of a kind of anti-caking, with embodiment 1, the difference is that adding in step (2)
Enter the AVM centrifuge mother liquor that potency is 20000u/ml.
Comparative example 1：
A kind of preparation method of the AVM toluene ointment of anti-caking, with embodiment 1, the difference is that：In step (7) not
Add intensive polar solvent.
Comparative example 2：
A kind of preparation method of the AVM toluene ointment of anti-caking, with embodiment 1, the difference is that：Without step
(4), (5), (6), the direct crystal solution of processing step (3) in step (7).
Comparative example 3：
The preparation method of the AVM toluene ointment of a kind of anti-caking, with embodiment 1, the difference is that not carrying out step
(4), (5), (6), the directly crystal solution of processing step (3), and intensive polar solvent is not added with step (7) in step (7).
Comparative example 4：
A kind of preparation method of the AVM toluene ointment of anti-caking, with embodiment 2, the difference is that：In step (7) not
Add intensive polar solvent.
Comparative example 5：
A kind of preparation method of the AVM toluene ointment of anti-caking, with embodiment 2, the difference is that：Without step
(4), (5), (6), the direct crystal solution of processing step (3) in step (7).
Comparative example 6：
A kind of preparation method of the AVM toluene ointment of anti-caking, with embodiment 2, the difference is that：Step is not carried out
(4), (5), (6), the directly crystal solution of processing step (3), and intensive polar solvent is not added with step (7) in step (7).
Experimental example：
The abamectin ointment that embodiment 1-2 and comparative example 1-6 are obtained carries out B1a contents, the measure of B2a contents, and
With being stored 30 days under the conditions of -20 DEG C, cold storage-stable is tested, B1a contents, B2a content balances and cold storage-stable are seen below
Table 1：
Table 1
Claims (10)
1. a kind of preparation method of anti-caking AVM toluene ointment, including step are as follows：
(1) AVM centrifuge mother liquor is concentrated into no methanol solvate, by AVM centrifuge mother liquor：The volume ratio of esters solvent
For 1：2~3 ratio is extracted AVM centrifuge mother liquor addition esters solvent, and AVM centrifuge mother liquor is completely dissolved
In esters solvent, extraction feed liquid is obtained；
(2) hot water is added into extraction feed liquid and carries out washing desugar, repetition is washed to water layer printing opacity >=30%, obtains desugar feed liquid；
(3) desugar feed liquid is dehydrated and is filtered to remove solid impurity, obtain removal of impurities feed liquid；
(4) removal of impurities feed liquid is cooled to 20 DEG C, is then at the uniform velocity cooled using refrigerant, be cooled to 0-5 DEG C, obtain crystal solution；
(5) by crystal solution centrifugal treating, AVM secondary mother liquid is obtained, AVM secondary mother liquid is concentrated into no ester
Class solvent；
(6) by AVM secondary mother liquid in the AVM secondary mother liquid obtained to step (5)：The volume ratio of toluene is 1：2
~3 ratio adds toluene and extracted, and AVM secondary mother liquid is dissolved completely in toluene, obtains toluene extraction feed liquid；
(7) after toluene extraction feed liquid being concentrated into ointment shape, the intensive polar solvent of ointment volume 2%~3% is added, produces anti-caking
The AVM toluene ointment of block.
2. the preparation method of anti-caking AVM toluene ointment according to claim 1, it is characterised in that step (1)
In, AVM centrifuge mother liquor：The volume ratio of esters solvent is 1：2.5.
3. the preparation method of anti-caking AVM toluene ointment according to claim 1, it is characterised in that step (1)
In, extraction temperature is 65~70 DEG C, is carried out under agitation.
4. the preparation method of anti-caking AVM toluene ointment according to claim 1, it is characterised in that step (1)
In, esters solvent is butyl acetate, isopropyl acetate or ethyl acetate.
5. the preparation method of anti-caking AVM toluene ointment according to claim 1, it is characterised in that step (2)
In, the addition volume of hot water is the 1/2~1/4 of extraction material liquid volume.
6. the preparation method of anti-caking AVM toluene ointment according to claim 1, it is characterised in that step (2)
In, the temperature of hot water is 85~90 DEG C, it is preferred that the temperature of hot water is 86~88 DEG C, and washing times are 3-5 times.
7. the preparation method of anti-caking AVM toluene ointment according to claim 1, it is characterised in that step (3)
In, it is dehydrated to be 0.06~0.07Mpa in vacuum, temperature is carried out under the conditions of being 80~85 DEG C.
8. the preparation method of anti-caking AVM toluene ointment according to claim 1, it is characterised in that the step
(4), being cooled to 0-5 DEG C is cooled with 2-3 DEG C/h of rate of temperature fall, and whole temperature fall time control is in 5-10 hours.
9. the preparation method of anti-caking AVM toluene ointment according to claim 1, it is characterised in that the step
(6), AVM secondary mother liquid：The volume ratio of toluene is 1：2.5.
10. the preparation method of anti-caking AVM toluene ointment according to claim 1, it is characterised in that the step
Suddenly (7), concentration are carried out under the conditions of 0.06~0.07Mpa vacuums, 70~80 DEG C, intensive polar solvent be methanol, ethanol or
One of which or any two or more mixing in dimethylformamide (DMF), the addition volume of intensive polar solvent is ointment volume
2%.
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| CN201710529962.XA CN107787963A (en) | 2017-07-03 | 2017-07-03 | A kind of preparation method of anti-caking AVM toluene ointment |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109832585A (en) * | 2019-02-15 | 2019-06-04 | 国投中鲁果汁股份有限公司 | Yacon thin slice and the polynary joint processing system of full powder |
| CN110105415A (en) * | 2019-04-15 | 2019-08-09 | 江苏物网慧农科技集团有限公司 | A kind of method that avermectin B2a fine powder and ointment can be prepared simultaneously |
| CN110240622A (en) * | 2019-06-05 | 2019-09-17 | 江苏物网慧农科技集团有限公司 | It is a kind of produce during avermectin without benzene desugar technique |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109832585A (en) * | 2019-02-15 | 2019-06-04 | 国投中鲁果汁股份有限公司 | Yacon thin slice and the polynary joint processing system of full powder |
| CN110105415A (en) * | 2019-04-15 | 2019-08-09 | 江苏物网慧农科技集团有限公司 | A kind of method that avermectin B2a fine powder and ointment can be prepared simultaneously |
| CN110240622A (en) * | 2019-06-05 | 2019-09-17 | 江苏物网慧农科技集团有限公司 | It is a kind of produce during avermectin without benzene desugar technique |
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