CN104650167B - A kind of preparation method of avermectin B2a - Google Patents
A kind of preparation method of avermectin B2a Download PDFInfo
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- CN104650167B CN104650167B CN201510104018.0A CN201510104018A CN104650167B CN 104650167 B CN104650167 B CN 104650167B CN 201510104018 A CN201510104018 A CN 201510104018A CN 104650167 B CN104650167 B CN 104650167B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H17/00—Compounds containing heterocyclic radicals directly attached to hetero atoms of saccharide radicals
- C07H17/04—Heterocyclic radicals containing only oxygen as ring hetero atoms
- C07H17/08—Hetero rings containing eight or more ring members, e.g. erythromycins
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
Abstract
The present invention relates to a kind of high-purity Abamectin B2a preparation method, including step to be concentrated into no cut by Avermectin B1a crystalline mother solution under vacuum condition, obtains the thick material of ointment；Add extractant to be extracted, obtain extract, then using saturated common salt water washing extract 2~3 times, n-butyl acetate solution is obtained after removing aqueous phase；N-butyl acetate solution decrease temperature crystalline, the growing the grain that will be obtained, filter, obtain avermectin B2a coarse crystallization；Recrystallize and filter in avermectin B2a coarse crystallization, dry, obtain high-purity Abamectin B2a fine powders.The present invention replaces toxic solvent aromatic hydrocarbon to produce avermectin B2a fine work with environment-friendly type innoxious solvent n-butyl acetate, it is small to live damaging property of employee's body during production operation, and pollution on the environment is also relatively small, in addition, using n-butyl acetate as B2a as recrystallisation solvent, gained avermectin B2a fine powder purity is more than 95%.
Description
Technical field：
The present invention relates to a kind of preparation method of biological pesticide, more particularly to one kind are high using the extraction of environment-friendly type recrystallisation solvent
The preparation method of purity avermectin B2a, belong to preparation technique of pesticide field.
Background technology：
AVM is in ten similar hexa-atomic big rings of the one group of structure obtained by tunning separation and Extraction in streptomycete
Esters antibiotic, 8 homologues form similar in one group of structure, and B1 and B2 are two big components in the homologue.Avermectin
Plain B classes component is to nematode, insect, and mite class has a high Biocidal activity, but killing ability B1a to different targets and
B2a has significant difference again.Avermectin B2a has good effect to root-knot nematode, according to Putter etc. 1981, in Ah
Tie up in 8 components of rhzomorph, B1a and B2a are maximally effective agricultural actives, wherein B2a to plant root-knot nematode activity highest,
Its lasting period in soil is up to 2 months.The experiments such as Vecent prove, the avermectin B2a original that the lasting period is grown in soil
Because being that it is metabolized as avermectin B2a -2,3- ketone by edaphon, the material compares Avermectin to the activity of root-knot nematode
Plain B2a is higher.
Chinese patent literature CN102977168A discloses a kind of extraction preparation method of avermectin B2a, and it is first
Avermectin B1a crystalline mother solution is concentrated into ointment shape, then adds extractant toluene into ointment and is extracted, addition helps in right amount
Filtering agent is cooled to 10-0 DEG C of progress B2a coarse crystallization after stirring, B2a crystal crude product then is carried out into weight with 5~7 times of toluene
Crystallization, filter, dry, obtain the avermectin B2a crystal fine work that purity is more than 90%.Although this method provides a kind of production
Advantage of lower cost, and it is easy to the extraction preparation method of industrialized production avermectin B2a, but this method uses carcinogen first
Benzene is used as crystallization and recrystallization solvent, larger to live damaging property of employee's body during production operation, and to environment
It can pollute.In addition, the technique is relatively low by twice of B2a crystal purity being recrystallized to give, purity is only 90%.
Chinese patent literature CN103333214A discloses a kind of preparation method of avermectin B2a fine powder, using 0.25-
0.6% tetrabutyl phosphonium bromide aqueous ammonium washs to sec-butyl acetate extract so that AVM purity improve to
More than 93%, in that patent, although improving the purity of AVM to a certain extent, the technique uses carcinogen
Aromatic hydrocarbon first uses second as crystallization and recrystallization solvent, property dangerous to live member during production operation in technique
The secondary butyl ester extraction of acid, is crystallized, technique is complex, raw with aromatic hydrocarbon again after sec-butyl acetate is evaporated in vacuo out after washing
It is higher to produce cost.
The content of the invention：
In view of the shortcomings of the prior art, the present invention provides a kind of using environment-friendly type recrystallisation solvent extraction high-purity Abamectin
B2a preparation method.
Technical scheme is as follows：
A kind of high-purity Abamectin B2a preparation method, including step are as follows：
(1) Avermectin B1a crystalline mother solution is concentrated into no cut under vacuum condition, obtains the thick material of ointment；
(2) extractant is added into the thick material of ointment obtained by step (1) to be extracted, obtain extract, then using full
With brine It extract 2~3 times, n-butyl acetate solution is obtained after removing aqueous phase；Described extractant is the positive fourth of acetic acid
Ester, addition and the thick material mass ratio of ointment of n-butyl acetate are (1~3)：1；
(3) obtained n-butyl acetate solution is cooled to 0~5 DEG C, after separating out a large amount of crystal, growing the grain, filter, obtain Ah
Tie up rhzomorph B2a coarse crystallization；
(4) n-butyl acetate is added into avermectin B2a coarse crystallization to be recrystallized, recrystallize the use of n-butyl acetate
The mass ratio of amount and coarse crystallization is (1~3)：1, filter, dry, obtain high-purity Abamectin B2a fine powders.
Currently preferred, Avermectin B1a crystalline mother solution is Crystallization Separation Avermectin in Avermectin B1a production process
Remaining liquid after plain B1a, Avermectin B1a production process comprise the following steps：
A, dry mycelium is made after press filtration, drying in abamectin fermented liquid；B, dry mycelium and methanol are according to mass ratio
For 1:8~9 ratio adds methanol and is extracted, filtered, and obtains leaching liquor；C, leaching liquor is concentrated into paste, after washing, filled into
The methanol that 0.6~0.8 times of ointment quality carries out rising temperature for dissolving, after being cooled to normal temperature, through filtering, dries, obtained solid is
Avermectin B1a fine powder, filtrate are Avermectin B1a crystalline mother solution, Avermectin B1a in Avermectin B1a crystalline mother solution
It is respectively 25%~30% and 55%~60% with avermectin B2a purity.
Currently preferred, the concentration of Avermectin B1a crystalline mother solution is that Avermectin B1a is crystallized into mother in step (1)
Liquid is warming up to 60~80 DEG C, keeps the temperature to distill out portion's cut big absolutely, until obtain oily plaster material, vacuum during concentration
For 0.05~0.07Mpa.
Currently preferred, the extraction in step (2) is that extractant n-butyl acetate is added into the thick material of ointment, is warming up to
60~70 DEG C, stirring is completely dissolved to the thick material of ointment for 0.5~1 hour, addition and the thick material mass ratio of ointment of n-butyl acetate
For (2~2.5)：1.
Currently preferred, the washing in step (2) is adds the saturated aqueous common salt of extract quality 20~30%, 80
~90 DEG C are stirred 1~2 hour, are then stood 10~15 minutes and are layered, remove aqueous phase, obtain n-butyl acetate solution.
Currently preferred, the cooling in step (3) is carried out in two steps, first with water-bath by the fast prompt drop of n-butyl acetate solution
Then temperature adjusts mixing speed and is cooled to 0 to 10~20r/min, and with 2~3 DEG C per hour of rate of temperature fall to 15~20 DEG C
~5 DEG C.
Currently preferred, the growing the grain in step (3) carries out growing the grain to be incubated 1~2 hour at 0~5 DEG C.
Currently preferred, recrystallization adds to add n-butyl acetate into avermectin B2a coarse crystallization in step (4)
Enter activated carbon, stirring is warming up to 80~90 DEG C, after avermectin B2a coarse crystallization is completely dissolved, is incubated 0.5~1h, is taken out
Filter, recovery filtrate to crystallizing tank, is crystallized, growing the grain according to the cooling method of step (3), is then filtered, and is dried, is obtained AVM hereinafter
Rhzomorph B2a fine powders.
It is currently preferred, when being recrystallized in step (4), addition and the avermectin B2a coarse crystallization of n-butyl acetate
Mass ratio be (2~2.5)：1, the dosage of activated carbon is the 0.5%~1% of avermectin B2a coarse crystallization quality.
A currently preferred technical scheme, a kind of high-purity Abamectin B2a preparation method, including step is such as
Under：
(1) by the Avermectin B1a crystalline mother solution after Crystallization Separation Avermectin B1a in Avermectin B1a production process
60~80 DEG C are warming up to, keeps distilling out under the conditions of the Temperature Vacuum portion's cut big absolutely, until obtain the thick material of ointment, during concentration
Vacuum is 0.05~0.07Mpa
(2) extractant n-butyl acetate is added into the thick material of ointment, is warming up to 60~70 DEG C, stirs 0.5~1 hour to oil
The thick material of cream is completely dissolved, and addition and the thick material mass ratio of ointment of n-butyl acetate are (2~2.5)：1, extract is obtained, adds extraction
The saturated aqueous common salt of liquid quality 20~30% is taken, is stirred at 80~90 DEG C 1~2 hour, is then stood 10~15 minutes and divided
Layer, removes aqueous phase, after repeated washing 2~3 times n-butyl acetate solution；
(3) first with water-bath by n-butyl acetate solution fast cooling to 15~20 DEG C, then adjust mixing speed to 10~
20r/min, and cooled with 2~3 DEG C per hour of rate of temperature fall, it is cooled to 0~5 DEG C of insulation and carries out growing the grain in 1~2 hour,
Suction filtration obtains avermectin B2a coarse crystallization；
(4) n-butyl acetate is added into avermectin B2a coarse crystallization, adds activated carbon, stirring is warming up to 80~90 DEG C,
After avermectin B2a coarse crystallization is completely dissolved, 0.5~1h is incubated, is filtered, recovery filtrate is to crystallizing tank, according to step
(3) cooling method is crystallized, growing the grain, is then filtered, and is dried, is obtained avermectin B2a fine powder, the addition of n-butyl acetate
The mass ratio of amount and coarse crystallization is 2：1~2.5：1；Activated carbon dosage is the 0.5%~1% of coarse crystallization mass fraction.
Beneficial effects of the present invention：
1st, it is small to live damaging property of employee's body during production operation, and pollution on the environment is also relatively
It is small.Because the preparation method of the present invention uses environment-friendly type solvent n-butyl acetate to be adopted as recrystallisation solvent relative to tradition
It is small with aromatic hydrocarbon solvent toxic.
2nd, the higher avermectin B2a crystalline product of purity can be obtained.Because n-butyl acetate is in cryogenic conditions
Under, B1a solubility is remained unchanged higher, so it can be realized preferably to B2a in primary crystallization mother liquor and B1a under cryogenic
Fractionation, B2a crystallization in B1a contents it is relatively low；In addition, aromatic hydrocarbon solvent is when for crystallization to B2a, due to its outburst
Property crystallization, separated out B2a crystallization parcel impurity it is more, cause purity low, and use n-butyl acetate it is molten as B2a crystallization
During agent, because its crystallization temperature is wider, using gradient slow cooling, the quantity that crystal seed can be controlled to generate, obtain larger more equal
Even crystal so that B2a crystallization purities are of a relatively high, and crystal formation is relatively preferable.
3rd, the production time is saved, reduces production cost.The crystallization processes treating capacity of this avermectin B2a is toluene crystallization
2~3 times, the crystallisation times that reach needed for certain fine work purity are few, and comprehensive yield is high, has saved production time and cost,
It is that a kind of more traditional B2a preparation methods are cheap, efficient method.
Brief description of the drawings
Fig. 1 is the liquid chromatogram of high-purity Abamectin B2a components made from embodiment 1 (n-butyl acetate is solvent)
Fig. 2 is the liquid chromatogram of avermectin B2a component made from comparative example 1 (toluene is solvent)
Embodiment：
Below by specific embodiment, the present invention will be further described, but not limited to this.
Equipment used in embodiment is conventional existing equipment.
Avermectin B1a crystalline mother solution is Crystallization Separation Avermectin B1a in Avermectin B1a production process in embodiment
Remaining liquid afterwards, Avermectin B1a production process comprise the following steps：
A, dry mycelium is made after press filtration, drying in abamectin fermented liquid；B, dry mycelium and methanol are according to mass ratio
For 1:8 ratio adds methanol and is extracted, filtered, and obtains leaching liquor；C, leaching liquor is concentrated into paste, after washing, fills into oil
The methanol that 0.7 times of cream quality carries out rising temperature for dissolving, after being cooled to normal temperature, through filtering, dries, obtained solid is AVM
B1a fine powders, filtrate are Avermectin B1a crystalline mother solution, and avermectin B2a purity is in Avermectin B1a crystalline mother solution
56.5%.
Embodiment 1：
A kind of high-purity Abamectin B2a preparation method, including step are as follows：
1st, the Avermectin B1a crystallization after Crystallization Separation Avermectin B1a in 1500ml Avermectin B1a production processes is taken
Mother liquor is warming up to 70 DEG C, keeps distilling out portion's cut big absolutely under the conditions of the Temperature Vacuum, until obtaining the thick material of ointment, vacuum condition
Vacuum be 0.06Mpa；
2nd, the thick material 450g of ointment for taking step 1 to obtain, 1125ml n-butyl acetates are added, is warming up to 70 DEG C, stirring 0.5 is small
It is completely dissolved up to the thick material of ointment, obtains extract, add 350ml saturated aqueous common salts, is stirred 2 hours at 80 DEG C, then stand 15
Minute be layered, remove aqueous phase, after repeated washing 2 times n-butyl acetate solution；
3rd, first with water-bath by n-butyl acetate solution fast cooling to 20 DEG C, then adjust mixing speed to 10~20r/
Min, and cooled with 2 DEG C per hour of rate of temperature fall, it is cooled to 0 DEG C of insulation and carries out within 2 hours growing the grain, suction filtration obtains Avermectin
Plain B2a coarse crystallization 195g；
4th, 290ml n-butyl acetates are added into avermectin B2a coarse crystallization again, add 1.0g activated carbons, stirring heating
To 80 DEG C, after avermectin B2a coarse crystallization is completely dissolved, 0.5h is incubated, is filtered, recovery filtrate is first used to crystallizing tank
N-butyl acetate solution fast cooling to 20 DEG C, is then adjusted mixing speed to 10~20r/min by water-bath, and with per hour 2
DEG C rate of temperature fall cooled, be cooled to 0 DEG C of insulation crystallized within 2 hours, growing the grain, then filter, dry, obtain Avermectin
Plain B2a fine powders, survey its B2a and survey dried avermectin B2a fine powder liquid chromatogram, as a result as shown in figure 1, purity is
95.44%.
Embodiment 2：
A kind of high-purity Abamectin B2a preparation method, including step are as follows：
1st, the Avermectin B1a crystallization after Crystallization Separation Avermectin B1a in 1500ml Avermectin B1a production processes is taken
Mother liquor is warming up to 80 DEG C, keeps the temperature to distill 2h under vacuum is 0.065Mpa vacuum condition, distills out portion big absolutely and evaporates
Point, until the thick material of ointment is obtained,
2nd, the thick material 440g of ointment for taking step 1 to obtain, 1100ml n-butyl acetates are added, is warming up to 60 DEG C, stirred 1 hour
It is completely dissolved to the thick material of ointment, obtains extract, add 430ml saturated aqueous common salts, is stirred at 85 DEG C 1 hour, then stand 15 points
Clock is layered, and removes aqueous phase, after repeated washing 2 times n-butyl acetate solution；
3rd, first with water-bath by n-butyl acetate solution fast cooling to 20 DEG C, then adjust mixing speed to 10r/min, and
Rate of temperature fall with 3 DEG C per hour is cooled, and is cooled to 0 DEG C of insulation and is carried out within 2 hours growing the grain, suction filtration obtains avermectin B2a
Coarse crystallization 183g；
4th, 458ml n-butyl acetates are added into avermectin B2a coarse crystallization again, add 1.0g activated carbons, stirring heating
To 80 DEG C, after avermectin B2a coarse crystallization is completely dissolved, 0.5h is incubated, is filtered, recovery filtrate is first used to crystallizing tank
N-butyl acetate solution fast cooling to 20 DEG C, is then adjusted mixing speed to 10r/min by water-bath, and with 3 DEG C per hour
Rate of temperature fall is cooled, be cooled to 0 DEG C of insulation crystallized within 2 hours, growing the grain, then filter, dry, obtain AVM
B2a fine powder 147g, its B2a purity is surveyed as 95.67%.
Comparative example 1
A kind of preparation method of avermectin B2a, comprises the following steps：
A. 1500ml Avermectin B1as crystalline mother solution (B2a purity is referred to as 56.65%), it is small that 70 DEG C of vacuum distillations 2 are warming up to
When, solution is condensed into paste.
B. it be 450g to deserve to be called and state gained lotion weight, addition 900ml toluene, is warming up to 60 DEG C of stirring and dissolvings 30 minutes, so
350ml saturated aqueous common salts are added afterwards, are stirred at 80 DEG C 1 hour, a point water is carried out after then standing 15 minutes, and repetition is above-mentioned to wash 2 again
Secondary, layering.
C. water-bath fast cooling is utilized then to delay to 20 DEG C using ethylene glycol chilled water the toluene solution obtained after layering
Slowly 0 DEG C is cooled to, stirred crystallization 2 hours, obtains a crude product 179g.
D. the toluene for adding 7 times of crude product weight is recrystallized twice, and suction filtration obtains fine work 125g, is dried, is obtained Ah
Rhzomorph B2a fine powders are tieed up, it is 90.80% to survey its B2a purity, surveys dried avermectin B2a fine powder liquid chromatogram, as a result such as
Shown in Fig. 2.
Experimental example
Using area normalization method testing example 1 and the purity of the avermectin B2a fine powder of comparative example 1,
Powder detection method：High-efficient liquid phase chromatogram area normalization method
Instrument：High performance liquid chromatograph
Chromatographic condition：Mobile phase (methanol：Water=85:15)
Detection and wavelength：UV, 245nm
Chromatographic column (C18,4.6mm*250mm)
Flow velocity：1ml/min
Sample size：20ul
Testing procedure：0.025~0.030g of fine powder is weighed in 100ml volumetric flasks, is dissolved with methanol, constant volume.Draw molten
Liquid 20ml injection high performance chromatographs are solved, by above chromatographic condition, detection time 15min, B2a appearance time are left for 5min
The right side, B2a purity is calculated according to area normalization method.The purity of the avermectin B2a fine powder of the embodiment 1 measured is shown in Table 1,
The purity of the avermectin B2a fine powder of the comparative example 1 measured is shown in Table 2, and be can be seen that by table 1, table 2 with reference to Fig. 1, Fig. 2
Avermectin B2a fine powder purity made from the method for the present invention is used as 95.44%, and comparative example 1 uses toluene as solvent system
The avermectin B2a fine powder purity obtained only reaches 90%.
Table 1
Analysis result table
Table 2
Analysis result table
Claims (6)
1. a kind of preparation method of avermectin B2a, including step are as follows：
(1) Avermectin B1a crystalline mother solution is concentrated into no cut under vacuum condition, obtains the thick material of ointment；
(2) extractant n-butyl acetate is added into the thick material of ointment obtained by step (1) to be extracted, be warming up to 60~70 DEG C,
Stirring is completely dissolved for 0.5~1 hour to the thick material of ointment, and addition and the thick material mass ratio of ointment of n-butyl acetate are 2~2.5：
1；Extract is obtained, then adds the saturated aqueous common salt of extract quality 20~30%, stirs 1~2 hour at 80~90 DEG C, so
Stand 10~15 minutes afterwards to be layered, remove aqueous phase, washing extract 2~3 times, obtain n-butyl acetate solution
(3) by obtained n-butyl acetate solution first with water-bath by n-butyl acetate solution fast cooling to 15~20 DEG C, then
Regulation mixing speed is cooled to 0~5 DEG C to 10~20r/min, and with 2~3 DEG C per hour of rate of temperature fall, separates out a large amount of crystal
Afterwards, 1~2 hour is incubated at 0~5 DEG C and carries out growing the grain, filters, obtains avermectin B2a coarse crystallization；
(4) n-butyl acetate is added into avermectin B2a coarse crystallization to be recrystallized, recrystallize the dosage of n-butyl acetate with
The mass ratio of coarse crystallization is 1~3：1, filter, dry, obtain avermectin B2a fine powder.
2. the preparation method of avermectin B2a according to claim 1, it is characterised in that Avermectin B1a crystalline mother solution
For remaining liquid after Crystallization Separation Avermectin B1a in Avermectin B1a production process, Avermectin B1a production process bag
Include following steps：
A, dry mycelium is made after press filtration, drying in abamectin fermented liquid；
B, dry mycelium is 1 according to mass ratio with methanol:8~9 ratio adds methanol and is extracted, filtered, and obtains leaching liquor；
C, leaching liquor is concentrated into paste, after washing, the methanol for filling into 0.6~0.8 times of ointment quality carries out rising temperature for dissolving, cooling
To normal temperature, through filtering, dry, obtained solid is Avermectin B1a fine powder, and filtrate is that Avermectin B1a crystallization is female
Liquid, in Avermectin B1a crystalline mother solution Avermectin B1a and avermectin B2a purity be respectively 25%~30% and 55%~
60%.
3. the preparation method of avermectin B2a according to claim 1, it is characterised in that AVM in step (1)
The concentration of B1a crystalline mother solutions is that Avermectin B1a crystalline mother solution is warming up into 60~80 DEG C, keeps the temperature to distill out exhausted big portion
Cut, until obtain oily plaster material, vacuum during concentration is 0.05~0.07Mpa.
4. the preparation method of avermectin B2a according to claim 1, it is characterised in that in step (4) recrystallization be to
N-butyl acetate is added in avermectin B2a coarse crystallization, adds activated carbon, stirring is warming up to 80~90 DEG C, treats avermectin B2a
After coarse crystallization is completely dissolved, 0.5~1h is incubated, is filtered, recovery filtrate is to crystallizing tank, according to the cooling method of step (3)
Crystallized, growing the grain, then filtered, dried, obtain avermectin B2a fine powder.
5. the preparation method of avermectin B2a according to claim 4, it is characterised in that when being recrystallized in step (4),
The addition of n-butyl acetate is 2~2.5 with the mass ratio of avermectin B2a coarse crystallization：1, the dosage of activated carbon is Avermectin
The 0.5%~1% of plain B2a coarse crystallization quality.
6. a kind of preparation method of avermectin B2a, including step are as follows：
(1) the Avermectin B1a crystalline mother solution after Crystallization Separation Avermectin B1a in Avermectin B1a production process is heated up
To 60~80 DEG C, keep distilling out under the conditions of the Temperature Vacuum portion's cut big absolutely, until obtain the thick material of ointment, vacuum during concentration
Spend for 0.05~0.07Mpa；
(2) extractant n-butyl acetate is added into the thick material of ointment, is warming up to 60~70 DEG C, stirring 0.5~1 hour is thick to ointment
Material is completely dissolved, and addition and the thick material mass ratio of ointment of n-butyl acetate are 2~2.5：1, extract is obtained, adds extract matter
The saturated aqueous common salt of amount 20~30%, stirred at 80~90 DEG C 1~2 hour, then stand 10~15 minutes and be layered, removed
Aqueous phase, after repeated washing 2~3 times n-butyl acetate solution；
(3) first with water-bath by n-butyl acetate solution fast cooling to 15~20 DEG C, then adjust mixing speed to 10~20r/
Min, and cooled with 2~3 DEG C per hour of rate of temperature fall, it is cooled to 0~5 DEG C of insulation and carries out growing the grain in 1~2 hour, filters
Obtain avermectin B2a coarse crystallization；
(4) add n-butyl acetate into avermectin B2a coarse crystallization, add activated carbon, stirring is warming up to 80~90 DEG C, treat Ah
After dimension rhzomorph B2a coarse crystallization is completely dissolved, 0.5~1h is incubated, is filtered, recovery filtrate is to crystallizing tank, according to step (3)
Cooling method is crystallized, growing the grain, is then filtered, and is dried, is obtained avermectin B2a fine powder, the addition of n-butyl acetate with
The mass ratio of coarse crystallization is 2：1~2.5：1；Activated carbon dosage is the 0.5%~1% of coarse crystallization mass fraction.
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| 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 |
| CN111387179B (en) * | 2020-04-29 | 2021-11-12 | 河北威远生物化工有限公司 | Avermectin B2a solvation solid and preparation method thereof |
| CN111606960A (en) * | 2020-05-15 | 2020-09-01 | 河北威远生物化工有限公司 | Avermectin B2a solvated crystal |
| CN112707939B (en) * | 2020-12-25 | 2022-06-24 | 河北威远生物化工有限公司 | Purification method of 4' -(s) -emamectin benzoate B2a |
| CN114044798B (en) * | 2021-10-28 | 2024-04-12 | 华北制药集团爱诺有限公司 | Extraction and purification method of abamectin B2a |
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| US5077398A (en) * | 1986-11-18 | 1991-12-31 | Merck & Co., Inc. | Process for isolation of avermectin B1 components with improved purity and subsequent isolaton of B2 components |
| CN102217591A (en) * | 2011-04-26 | 2011-10-19 | 张福志 | Environmentally-friendly abamectin ointment production process |
| CN103483405B (en) * | 2012-06-13 | 2015-12-09 | 王玉万 | The method of stepwise solvent extraction Avermectin B1a and B2a from mycelium |
| CN103030676B (en) * | 2012-11-19 | 2015-07-22 | 河北威远生化农药有限公司 | Process for extracting component B1 and component B2 of abamectin step by step by using crystallization process |
| CN103333214B (en) * | 2013-07-03 | 2015-08-12 | 大庆志飞生物化工有限公司 | A kind of Avrmectin B 2athe preparation method of fine powder |
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