CN109912671B - Method for extracting abamectin B2a by using abamectin crystallization mother liquor - Google Patents

Method for extracting abamectin B2a by using abamectin crystallization mother liquor Download PDF

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CN109912671B
CN109912671B CN201910291827.5A CN201910291827A CN109912671B CN 109912671 B CN109912671 B CN 109912671B CN 201910291827 A CN201910291827 A CN 201910291827A CN 109912671 B CN109912671 B CN 109912671B
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abamectin
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stirring
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CN109912671A (en
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任勇
张萍
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Ningxia Taiyixin Biotechnology Co ltd
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Ningxia Taiyicin Biotech Co ltd
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Abstract

The invention relates to a method for extracting abamectin B2a by using abamectin crystallization mother liquor, which comprises the following process steps: decompressing and concentrating the abamectin crystallization mother liquor, removing the solvent to obtain a solid, then adding triethylene glycol-methyl ether or triethylene glycol-ethyl ether, stirring and dissolving at 40-60 ℃, filtering to obtain an abamectin solution, decoloring, filtering, cooling and crystallizing, standing, filtering and drying to obtain the abamectin B2 a. The invention can lead the effective content of the avermectin B2a to reach 97-98 percent, lead the extraction yield to reach 96-98 percent, have simple whole extraction process and easily controlled process flow, adopt a single crystallization method, avoid repeated crystallization process, have lower production cost, further improve the utilization rate of the avermectin B2a and provide technical support for industrialization thereof.

Description

Method for extracting abamectin B2a by using abamectin crystallization mother liquor
Technical Field
The invention belongs to the technical field of antibiotic extraction, and particularly relates to a method for extracting abamectin B2a by using abamectin crystallization mother liquor.
Background
Avermectins, the English name Avermectins, is a sixteen-membered macrolide compound with insecticidal, acaricidal and nematicidal activities, which is firstly developed by Dacun Zhi and the like of North Rily university of Japan and Merck company of America, and is produced by fermenting Streptomyces avermitilis in Streptomyces griseus. The natural Avermectins contains 8 components, mainly 4 components are A1a, A2a, B1a and B2a, and the total content is more than or equal to 80 percent; the corresponding 4 homologues with smaller proportion are A1B, A2B, B1B and B2B, and the total content is less than or equal to 20 percent.
The abamectin B2 comprises two main components B2a and B2B, and the national standard GB19336-2007 original abamectin pesticide takes a mixture B2 of B2a + B2B as a target, and is not separated independently; moreover, the B2a occupies an absolutely large content, the effective content exceeds 90 percent, and the B2B is trace. The B2 has moderate toxicity as a whole, the toxicity is lower than that of B1, and the use is safer and more environment-friendly. The abamectin B2a can be used as an effective control drug for Meloidogyne incognita, has a strong killing effect on 2-instar larvae in Meloidogyne incognita infection state, and the killing effect is unrecoverable. In addition, the abamectin B2a can also effectively inhibit the hatching of meloidogyne incognita eggs.
At present, some documents for extracting abamectin B2a by using abamectin ointment are disclosed in China, wherein
The Chinese patent document with application number 201210548729 provides an extraction preparation method of abamectin B2a, which comprises the steps of preparing abamectin fermentation liquor into dry mycelia and leaching; concentrating the leaching solution, and adding an extracting agent such as toluene and the like for extraction; crystallizing the extract liquor I; concentrating the obtained mother liquor to obtain ointment; adding toluene into the ointment to obtain an extract liquid II; adding a filter aid into the extract liquor II, stirring, cooling, crystallizing, growing crystals, and filtering; adding toluene to dissolve the obtained filter cake, cooling the filtrate again, crystallizing, growing crystals, and filtering; obtaining a crude product of abamectin B2a crystal; recrystallizing the abamectin B2a crystal crude product to obtain an abamectin B2a crystal refined product. The technology comprises the following steps: 1. the toxic solvent-toluene is used as an extracting agent, which is easy to cause damage to the health of constructors and pollutes the environment; 2. the extraction purity of the abamectin B2a is low, and is only below 90%; 3. the secondary crystallization mode is adopted, so that the production period is longer and the production cost is higher.
Chinese patent document with application number 201510104018 provides a preparation method of high-purity abamectin B2a, which comprises the steps of concentrating abamectin B1a crystallization mother liquor under vacuum condition until no fraction is obtained, and obtaining ointment thick material; extracting with n-butyl acetate solution as an extractant to obtain an extract, washing the extract with saturated salt solution for 2-3 times, and removing a water phase to obtain n-butyl acetate solution; cooling and crystallizing the obtained n-butyl acetate solution, growing crystals, and performing suction filtration to obtain crude crystals of abamectin B2 a; recrystallizing, filtering and drying the abamectin B2a coarse crystals to obtain high-purity abamectin B2a fine powder. The technology uses an environment-friendly nontoxic solvent n-butyl acetate to replace a toxic solvent aromatic hydrocarbon to produce the fine avermectin B2a, has small harm to the bodies of field workers in the production operation process, and causes relatively small pollution to the environment, and in addition, the n-butyl acetate is used as the B2a as a crystallization solvent, and the purity of the obtained fine avermectin B2a powder is more than 95%. However, the technology still needs to adopt a secondary crystallization mode for extraction, the production period is long, and the production cost is high.
The Chinese patent document with application number 201310276902 provides a preparation method of abamectin B2a fine powder, which comprises the steps of firstly concentrating an abamectin B1a crystallization mother liquor into a paste, dissolving the obtained paste with sec-butyl acetate, then adding a tetrabutylammonium bromide aqueous solution for washing and layering, then concentrating the obtained sec-butyl acetate solution, then adding a crystallization solvent for dissolving, naturally cooling to room temperature for crystallization, filtering to obtain an abamectin B2a fine powder crude product, and finally recrystallizing the abamectin B2a fine powder crude product to obtain the abamectin B2a fine powder. This technique is washed with tetrabutyl ammonium bromide aqueous solution, and washing or saturated salt solution washing edulcoration effect of tradition are better, the solution is changeed the layering, have improved avermectin B2 a's purity to a certain extent, but adopt carcinogen aromatic hydrocarbon to use as crystallization and recrystallization solvent, and safety can not ensure, and the environmental pollution index increases, and twice crystallization mode leads to production cycle longer simultaneously, and manufacturing cost is higher relatively.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide the method for extracting the abamectin B2a by using the abamectin crystallization mother liquor, which has the advantages of effectively improving the purity of the abamectin B2a, along with environmental protection, safety, simple extraction process, short production period and effectively reduced production cost.
The technical scheme adopted for realizing the purpose is as follows:
a method for extracting abamectin B2a by using abamectin crystallization mother liquor is characterized by comprising the following process steps:
1) decompressing and concentrating the abamectin crystallization mother liquor, and removing the solvent to obtain a solid;
2) adding triethylene glycol-methyl ether or triethylene glycol-ethyl ether into the solid obtained in the process 1), stirring and dissolving at the temperature of 40-60 ℃, and filtering to obtain an abamectin solution;
3) adding silica gel decolorizing sand into the abamectin solution for decolorizing, fully stirring and filtering, adding purified water into the obtained filtrate, cooling and crystallizing, standing, filtering and drying to obtain abamectin B2 a.
In the process 1), the pressure of the reduced pressure concentration is controlled to be-0.1-0.01 MPa, and the concentration is carried out until no liquid flows out.
In the process 2), the dosage of the triethylene glycol-methyl ether or the triethylene glycol-ethyl ether is
WSolid object:LTriethylene glycol monomethyl ether or triethylene glycol diethyl ether=1kg:6-8L。
In the process 3), the dosage of the silica gel decolorizing sand is
WSolid object:WSilica gel decolorization sand=1kg:20-40g。
In the process 3), the cooling crystallization conditions are as follows: the temperature of the mixed solution is reduced from the initial temperature of 40-60 ℃ to-5-0 ℃, and the speed of temperature reduction is controlled at 2-3 ℃/h;
in the cooling process, the initial stirring speed is controlled at 50-60 r/min; reducing the temperature to 20-25 ℃, and controlling the stirring speed at 30-35 r/min; reducing the temperature to 5-10 ℃, and controlling the stirring speed at 15-20 r/min; reducing the temperature to 0 ℃, and controlling the stirring speed at 5-10 r/min;
and in the process of cooling, when the solution is slightly turbid, adding seed crystals, continuously stirring for 80-100min, and standing.
The seed crystal is abamectin B2a, and the addition amount is as follows:
Wsolid object︰W Abamectin B2a=1kg︰1-2g。
In the process 3), the decoloring and stirring time is 80-100 min.
The standing time is 180-200 min.
Triethylene glycol methyl ether and triethylene glycol ethyl ether belong to organic solvents with more than 3 functional groups, and the compounds generate stronger dissolving performance due to the interaction of multiple functional groups. The invention fully utilizes the dissolution characteristic of triethylene glycol-methyl ether or triethylene glycol-ethyl ether, in particular the physicochemical characteristic that the abamectin B2a is easily dissolved in the triethylene glycol-methyl ether or triethylene glycol-ethyl ether, adopts the triethylene glycol-methyl ether or triethylene glycol-ethyl ether as an extraction solvent, quickly dissolves the abamectin B2a in the abamectin solid without the solvent, and then carries out crystallization extraction, thereby extracting the abamectin B2a in the abamectin crystallization mother liquor to the maximum extent, and finally realizing the technical advantages of 96-98% of extraction yield and 97-98% of effective content of the abamectin B2 a; the whole extraction process is simple, the process flow is easy to control, a single crystallization method is adopted, the repeated crystallization process is avoided, and the production cost is low. Meanwhile, the triethylene glycol-methyl ether or triethylene glycol-ethyl ether is a multifunctional solvent, and relatively small pollution is caused to the environment.
In conclusion, the extraction process disclosed by the invention can effectively separate the abamectin B2a from the abamectin crystallization mother liquor, has high extraction yield and good extraction effect, further improves the utilization rate of the abamectin B2a, and provides technical support for industrialization.
Detailed Description
The invention is illustrated below by way of examples, which are to be understood as being illustrative and not limiting. The scope and core content of the invention are to be determined by the claims.
Sources of avermectin crystallization mother liquor in the following examples:
the avermectin fermentation liquor is made into dry mycelium after filter pressing and drying. And leaching and filtering the dry mycelium and methanol or ethanol according to the mass ratio of 1:8 to obtain a leaching solution. Concentrating the leaching solution under reduced pressure to paste, washing with water, adding methanol or ethanol, heating to dissolve, cooling to normal temperature, vacuum filtering, and drying to obtain solid, i.e. fine avermectin B1a powder, filtrate, i.e. avermectin crystal mother liquor, wherein the concentration of avermectin B2a in the avermectin crystal mother liquor is 30-40%.
The following triethylene glycol-methyl ether and triethylene glycol-ethyl ether are supplied by Jiangsu Tianyin chemical Co., Ltd.
The pressure of the reduced pressure concentration is controlled between-0.1 and 0.01 MPa.
Example 1
The detection result shows that the concentration content of the abamectin B2a in the abamectin crystallization mother liquor is 31.2L. Concentrating under reduced pressure until no liquid flows out (removing solvent) to obtain solid 3.2 kg; 19.2L of triethylene glycol-methyl ether is added into the solid, stirred and dissolved at the temperature of 40 ℃, and then filtered to obtain 19.2L of abamectin solution. Adding silica gel decolorizing sand 64g into avermectin solution, stirring for 80min, and filtering. Adding purified water into the filtered abamectin solution, cooling and crystallizing, and reducing the temperature of the mixed solution from the initial 40 ℃ to 0 ℃. The cooling speed is controlled at 2-3 ℃/h. In the cooling process, the initial stirring speed is controlled at 50 r/min; the temperature is reduced to 25 ℃, and the stirring speed is controlled at 35 r/min; the temperature is reduced to 10 ℃, and the stirring speed is controlled at 20 r/min; the temperature is reduced to 0 ℃, and the stirring speed is controlled at 10 r/min. In the process of cooling, when the solution is slightly turbid, adding seed crystal abamectin B2a 3.2.2 g, continuing stirring for 80min, standing for 180min, filtering and drying to obtain solid abamectin B2a 3 kg. The detection proves that the effective content of the abamectin B2a is 97.1%, and the extraction yield reaches 96.2%.
Example 2
The detection result shows that the concentration content of the abamectin B2a in the abamectin crystal mother liquor 10L is 33.1%. Concentrating under reduced pressure until no liquid flows out (removing solvent) to obtain solid 3.5 kg; adding 22.8L of triethylene glycol-diethyl ether into the solid, stirring and dissolving at 45 ℃, and filtering to obtain 22.8L of abamectin solution. And adding 88g of silica gel desanding sand into the abamectin solution, stirring for 85min, and filtering. Adding purified water into the filtered abamectin solution, cooling and crystallizing, and reducing the temperature of the mixed solution from the initial 45 ℃ to-1 ℃. The cooling speed is controlled at 2-3 ℃/h. In the cooling process, the initial stirring speed is controlled at 52 r/min; the temperature is reduced to 24 ℃, and the stirring speed is controlled at 34 r/min; the temperature is reduced to 9 ℃, and the stirring speed is controlled at 19 r/min; the temperature is reduced to-1 ℃, and the stirring speed is controlled at 9 r/min. In the process of cooling, when the solution is slightly turbid, adding seed crystal abamectin B2a 4.3.3 g, continuing stirring for 85min, standing for 185min, filtering and drying to obtain solid abamectin B2a 3.2.2 kg. The detection proves that the effective content of the abamectin B2a is 97.4%, and the extraction yield reaches 96.6%.
Example 3
The detection result shows that the concentration content of the abamectin B2a in the abamectin crystallization mother liquor is 35.6 percent. Concentrating under reduced pressure until no liquid flows out (removing solvent) to obtain solid 3.8 kg; adding 26.6L of triethylene glycol-methyl ether into the solid, stirring and dissolving at 50 ℃, and filtering to obtain 26.6L of abamectin solution. Adding 114g of silica gel desanding sand into the abamectin solution, stirring for 90min, and filtering. Adding purified water into the filtered abamectin solution, cooling and crystallizing, and reducing the temperature of the mixed solution from the initial 50 ℃ to-2 ℃. The cooling speed is controlled at 2-3 ℃/h. In the cooling process, the initial stirring speed is controlled at 55 r/min; the temperature is reduced to 23 ℃, and the stirring speed is controlled at 33 r/min; the temperature is reduced to 8 ℃, and the stirring speed is controlled at 17 r/min; the temperature is reduced to-2 ℃, and the stirring speed is controlled at 8 r/min. In the process of cooling, when the solution is slightly turbid, adding seed crystal abamectin B2a 5.7.7 g, continuing stirring for 90min, standing for 190min, filtering and drying to obtain solid abamectin B2a 3.48.48 kg. The detection proves that the effective content of the abamectin B2a is 97.9%, and the extraction yield reaches 97.8%.
Example 4
The detection result shows that the concentration content of the abamectin B2a in the abamectin crystal mother liquor is 36.9 percent. Concentrating under reduced pressure until no liquid flows out (removing solvent) to obtain solid 4.1 kg; adding 30.8L of triethylene glycol-diethyl ether into the solid, stirring and dissolving at the temperature of 55 ℃, and filtering to obtain 30.7L of abamectin solution. Adding 143g of silica gel decolorizing sand into the abamectin solution, stirring for 95min, and filtering. Adding purified water into the filtered abamectin solution, cooling and crystallizing, and reducing the temperature of the mixed solution from the initial 55 ℃ to-3 ℃. The cooling speed is controlled at 2-3 ℃/h. In the cooling process, the initial stirring speed is controlled at 57 r/min; the temperature is reduced to 22 ℃, and the stirring speed is controlled at 32 r/min; the temperature is reduced to 7 ℃, and the stirring speed is controlled at 16 r/min; the temperature is reduced to-3 ℃, and the stirring speed is controlled at 6 r/min. In the process of cooling, when the solution is slightly turbid, adding 2a 7g of seed crystal abamectin B2, continuing stirring for 95min, standing for 195min, filtering and drying to obtain 3.59kg of solid abamectin B2a 3.59. The detection proves that the effective content of the abamectin B2a is 97.7%, and the extraction yield reaches 97.5%.
Example 5
The detection result shows that the concentration content of the abamectin B2a in the abamectin crystal mother liquor 10L is 38.6%. Concentrating under reduced pressure until no liquid flows out (removing solvent) to obtain solid 4.5 kg; adding 36L of triethylene glycol-methyl ether into the solid, stirring and dissolving at 60 ℃, and filtering to obtain 36L of abamectin solution. Adding 180g of silica gel decolorizing sand into the abamectin solution, stirring for 95min, and filtering. Adding purified water into the filtered abamectin solution, cooling and crystallizing, and reducing the temperature of the mixed solution from the initial 60 ℃ to-5 ℃. The cooling speed is controlled at 2-3 ℃/h. In the cooling process, the initial stirring speed is controlled at 60 r/min; the temperature is reduced to 20 ℃, and the stirring speed is controlled at 30 r/min; the temperature is reduced to 5 ℃, and the stirring speed is controlled at 15 r/min; the temperature is reduced to-5 ℃, and the stirring speed is controlled at 5 r/min. In the process of cooling, when the solution is slightly turbid, adding 2a 9g of seed crystal abamectin B2, continuing stirring for 100min, standing for 200min, filtering and drying to obtain solid abamectin B2a 3.75.75 kg. Through detection, the effective content of the abamectin B2a is 97.4%, and the extraction yield reaches 97.1%.
Comparative example 1
Adding toluene into 10L of abamectin crystallization mother liquor, heating to 80-100 ℃, completely melting, filtering out a filter aid, recovering a filtrate, cooling the filtrate to 10-0 ℃ again, growing crystals after a large number of crystals are separated out, carrying out vacuum filtration, rinsing the obtained filter cake with toluene at 0-10 ℃ until the color turns white, and drying to obtain white crystal powder which is detected as an abamectin B2a crude product.
Adding toluene into the abamectin B2a crude product, heating to 80-100 ℃, dissolving (at the moment, adding activated carbon, performing color removal treatment), filtering, recovering the filtrate, cooling the filtrate to 10-0 ℃ again, growing crystals after a large amount of crystals are separated out, performing vacuum filtration, rinsing the obtained filter cake with toluene at 0-10 ℃ until the color turns white, and drying to obtain the recrystallized abamectin B2 a. And repeatedly recrystallizing for 2 times to obtain the refined abamectin B2a product with the purity of 88.5 percent. The yield thereof was found to be 92%.
Comparative example 2
Crystallizing 10L of mother liquor of Avermectin B1a, adding 7.3L of n-butyl acetate, heating to 60 deg.C, stirring for 1 hr to obtain extractive solution, adding 2.8L of saturated saline, stirring at 85 deg.C for 1 hr, standing for 15 min for layering, removing water phase, washing for 2 times to obtain n-butyl acetate solution
The method comprises the steps of firstly, rapidly cooling a n-butyl acetate solution to 20 ℃ by using a water bath, then adjusting the stirring speed to 10r/min, cooling at the cooling rate of 3 ℃ per hour, cooling to 0 ℃ and keeping the temperature for 2 hours for crystal growth, and carrying out suction filtration to obtain 1.21kg of crude crystals of the abamectin B2 a.
Adding 3L of n-butyl acetate into the crude avermectin B2a crystal, adding 10g of activated carbon, stirring and heating to 80 ℃, keeping the temperature for 0.5h after the crude avermectin B2a crystal is completely dissolved, performing suction filtration, recovering filtrate to a crystallization tank, quickly cooling the n-butyl acetate solution to 20 ℃ by using water bath, then adjusting the stirring speed to 10r/min, cooling at the cooling rate of 3 ℃ per hour, cooling to 0 ℃ and keeping the temperature for 2 hours for crystallization and crystal cultivation, then performing suction filtration and drying to obtain 902g of avermectin B2a fine powder, measuring the purity of B2a to be 91.3%, and the extraction yield is 91.5%.
Comparative example 3
Weighing 1000g of abamectin ointment into a crystallizing tank, adding 3500mL of crystallization solvent acetone, heating to 75 ℃, stirring for 2 hours, naturally cooling to 25 ℃ after complete dissolution, continuously cooling to-6 ℃ by using cold saline, keeping the temperature for 2 hours, keeping the low temperature state, putting into a suction filter, and performing vacuum suction filtration to obtain 1410g of crude abamectin B2.
Dissolving the crude product of the abamectin B2 in 5000mL of acetone, adding 80g of activated carbon, heating to 70 ℃, preserving heat for 30min, decoloring, filtering, naturally cooling the filtrate to 25 ℃ in a crystallizing tank, forcibly cooling to-6 ℃ by using cold saline, preserving heat for 2 hours, growing crystals, and carrying out vacuum filtration to obtain a secondary crystallization product 810 g. And adding 4000mL of acetone and 4.5g of activated carbon into the secondary crystallization product to perform tertiary crystallization to obtain a tertiary crystallization product. 600g of abamectin B2 fine powder is obtained after drying, wherein the content of B2 is 93.6%, and the content of B2a is 91.2%. The extraction yield was 83.2%.
Comparative example 4
Weighing 2000g of abamectin B1 crystallization mother liquor taking methanol as a solvent, cooling to 20 ℃, adding 1000g of ammonium sulfate aqueous solution with the mass concentration of 45%, starting stirring for 45 minutes, stopping stirring, standing for 3 hours, and discharging the lower-layer salt solution from the bottom. Then, 1000g of a 25% aqueous solution of dipotassium hydrogenphosphate was again added to the pot, stirred for 45 minutes, and then allowed to stand for 3 hours, and the lower layer feed liquid was discharged from the bottom of the pot.
And pumping the upper layer feed liquid into a vacuum evaporation tank for vacuum evaporation to remove methanol, thereby obtaining about 510g of abamectin ointment.
Preparing a coarse crystallization solution: 510g of abamectin ointment is dissolved by 800g of ethanol-water composite solvent at 50 ℃, and the mass concentration of ethanol in the composite solvent is 40%.
Decoloring by using a decoloring agent: and adding 100g of granular activated carbon into the crystallized coarse material liquid for decolorization, wherein the decolorization temperature is 50 ℃, and the stirring decolorization time is 30 minutes.
And (3) filtering: filtering to remove decolorizer and other impurities to obtain purified crystallized feed liquid 1047g which is light yellow.
Cooling the refined crystallized liquid to 20 deg.C, stirring slowly at 70rpm to cool and separate out avermectin B2 crystal, and growing crystal for 1.5 hr. And continuously cooling to 0-2 ℃, slowly stirring at the rotating speed of 70rpm to continuously separate out the abamectin B2 crystal, and growing the crystal for 2 hours again. The abamectin B2 crystal coarse powder is obtained by centrifugation, and 18g is obtained.
Recrystallizing the coarse avermectin B2 crystal powder once by using an isopropanol-water composite solvent. Washing the abamectin B2 crystal obtained by recrystallization with deionized water at 0-2 ℃, removing residual solvent and impurities, then filtering and drying to obtain 16g of abamectin B2 fine powder, and detecting by a high performance liquid chromatography, wherein the purity is 93.1 percent and the extraction yield is 90.6 percent.
Comparative example 5
Heating 1500ml of abamectin B1a crystallization mother liquor obtained after abamectin B1a is crystallized and separated in the abamectin B1a production process to 80 ℃, keeping the temperature, distilling for 2 hours under the vacuum condition of 0.065Mpa, and distilling out most of fractions until the ointment thick material is obtained.
Adding 1200ml of n-butyl acetate into 400g of thick paste, heating to 60 ℃, stirring for 1 hour until the thick paste is completely dissolved to obtain an extract, adding 450ml of saturated saline, stirring for 1 hour at 85 ℃, standing for 15 minutes for layering, removing a water phase, and repeatedly washing for 2 times to obtain an n-butyl acetate solution.
The method comprises the steps of firstly, rapidly cooling a n-butyl acetate solution to 20 ℃ by using a water bath, then adjusting the stirring speed to 10r/min, cooling at the cooling rate of 3 ℃ per hour, cooling to 0 ℃, keeping the temperature for 2 hours for crystal growth, and carrying out suction filtration to obtain 170g of crude crystals of abamectin B2 a.
Adding 460ml of n-butyl acetate into the abamectin B2a coarse crystals, adding 1g of activated carbon, stirring and heating to 80 ℃, keeping the temperature for 0.5h after the abamectin B2a coarse crystals are completely dissolved, performing suction filtration, recovering filtrate to a crystallization tank, quickly cooling the n-butyl acetate solution to 20 ℃ by using water bath, then adjusting the stirring speed to 10r/min, cooling at the cooling rate of 3 ℃ per hour, cooling to 0 ℃ and keeping the temperature for 2 hours for crystallization and crystal cultivation, then performing suction filtration and drying to obtain 121g of abamectin B2a fine powder, and measuring the purity of B2a to be 91.5%.

Claims (6)

1. A method for extracting abamectin B2a by using abamectin crystallization mother liquor is characterized by comprising the following process steps:
1) decompressing and concentrating the abamectin crystallization mother liquor, and removing the solvent to obtain a solid;
2) adding triethylene glycol-methyl ether or triethylene glycol-ethyl ether into the solid obtained in the process 1), stirring and dissolving at the temperature of 40-60 ℃, and filtering to obtain an abamectin solution, wherein the dosage of the triethylene glycol-methyl ether or the triethylene glycol-ethyl ether is WSolid object:LTriethylene glycol monomethyl ether or triethylene glycol diethyl ether=1kg:6-8L;
3) Adding silica gel decolorizing sand into the abamectin solution for decolorizing, fully stirring and filtering, adding purified water into the obtained filtrate, cooling and crystallizing, standing, filtering and drying to obtain abamectin B2a, wherein the cooling and crystallizing conditions are as follows: the temperature of the mixed solution is reduced from the initial temperature of 40-60 ℃ to-5-0 ℃, and the speed of temperature reduction is controlled at 2-3 ℃/h;
in the cooling process, the initial stirring speed is controlled at 50-60 r/min; reducing the temperature to 20-25 ℃, and controlling the stirring speed at 30-35 r/min; reducing the temperature to 5-10 ℃, and controlling the stirring speed at 15-20 r/min; reducing the temperature to 0 ℃, and controlling the stirring speed at 5-10 r/min;
and in the process of cooling, when the solution is slightly turbid, adding seed crystals, continuously stirring for 80-100min, and standing.
2. The method for extracting abamectin B2a by using the abamectin crystallization mother liquor as claimed in claim 1, wherein in the process 1), the pressure for reduced pressure concentration is controlled to be-0.1-0.01 MPa, and the abamectin B2a is concentrated until no liquid flows out.
3. The method for extracting abamectin B2a by using the abamectin crystallization mother liquor as claimed in claim 1, wherein in the process 3), the using amount of the silica gel decolorizing sand is WSolid object:WSilica gel decolorization sand=1kg:20-40g。
4. The method for extracting abamectin B2a by using the abamectin crystallization mother liquor as claimed in claim 1, wherein the seed crystal is abamectin B2a, and the addition amount is as follows: wSolid object︰WAbamectin B2a=1kg︰1-2g。
5. The method for extracting the abamectin B2a by using the abamectin crystallization mother liquor as claimed in claim 1, wherein in the process 3), the decoloring and stirring time is 80-100 min.
6. The method for extracting abamectin B2a by using the abamectin crystallization mother liquor as claimed in claim 1, wherein the standing time is 180-200 min.
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