CN108440622B - Extraction and purification method and extraction and purification device for avermectin - Google Patents
Extraction and purification method and extraction and purification device for avermectin Download PDFInfo
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- CN108440622B CN108440622B CN201810362653.2A CN201810362653A CN108440622B CN 108440622 B CN108440622 B CN 108440622B CN 201810362653 A CN201810362653 A CN 201810362653A CN 108440622 B CN108440622 B CN 108440622B
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- 239000005660 Abamectin Substances 0.000 title claims abstract description 68
- RRZXIRBKKLTSOM-XPNPUAGNSA-N avermectin B1a Chemical compound C1=C[C@H](C)[C@@H]([C@@H](C)CC)O[C@]11O[C@H](C\C=C(C)\[C@@H](O[C@@H]2O[C@@H](C)[C@H](O[C@@H]3O[C@@H](C)[C@H](O)[C@@H](OC)C3)[C@@H](OC)C2)[C@@H](C)\C=C\C=C/2[C@]3([C@H](C(=O)O4)C=C(C)[C@@H](O)[C@H]3OC\2)O)C[C@H]4C1 RRZXIRBKKLTSOM-XPNPUAGNSA-N 0.000 title claims abstract description 54
- 238000000034 method Methods 0.000 title claims abstract description 51
- 238000000605 extraction Methods 0.000 title claims abstract description 29
- 238000000746 purification Methods 0.000 title claims abstract description 25
- 238000003756 stirring Methods 0.000 claims abstract description 140
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 138
- 238000002425 crystallisation Methods 0.000 claims abstract description 51
- 230000008025 crystallization Effects 0.000 claims abstract description 51
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 47
- 238000002386 leaching Methods 0.000 claims abstract description 35
- 239000012535 impurity Substances 0.000 claims abstract description 24
- 238000001816 cooling Methods 0.000 claims abstract description 21
- 239000000463 material Substances 0.000 claims abstract description 21
- 238000011282 treatment Methods 0.000 claims abstract description 12
- 230000001502 supplementing effect Effects 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 6
- 238000000855 fermentation Methods 0.000 claims abstract description 6
- 230000004151 fermentation Effects 0.000 claims abstract description 6
- 238000001914 filtration Methods 0.000 claims abstract description 6
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 30
- 238000004821 distillation Methods 0.000 claims description 19
- 239000000843 powder Substances 0.000 claims description 18
- 239000007788 liquid Substances 0.000 claims description 16
- IBSREHMXUMOFBB-JFUDTMANSA-N 5u8924t11h Chemical compound O1[C@@H](C)[C@H](O)[C@@H](OC)C[C@@H]1O[C@@H]1[C@@H](OC)C[C@H](O[C@@H]2C(=C/C[C@@H]3C[C@@H](C[C@@]4(O3)C=C[C@H](C)[C@@H](C(C)C)O4)OC(=O)[C@@H]3C=C(C)[C@@H](O)[C@H]4OC\C([C@@]34O)=C/C=C/[C@@H]2C)/C)O[C@H]1C.C1=C[C@H](C)[C@@H]([C@@H](C)CC)O[C@]11O[C@H](C\C=C(C)\[C@@H](O[C@@H]2O[C@@H](C)[C@H](O[C@@H]3O[C@@H](C)[C@H](O)[C@@H](OC)C3)[C@@H](OC)C2)[C@@H](C)\C=C\C=C/2[C@]3([C@H](C(=O)O4)C=C(C)[C@@H](O)[C@H]3OC\2)O)C[C@H]4C1 IBSREHMXUMOFBB-JFUDTMANSA-N 0.000 claims description 14
- 229950008167 abamectin Drugs 0.000 claims description 14
- 229920006395 saturated elastomer Polymers 0.000 claims description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 238000002834 transmittance Methods 0.000 claims description 8
- 239000012141 concentrate Substances 0.000 claims description 4
- 230000008878 coupling Effects 0.000 claims description 4
- 238000010168 coupling process Methods 0.000 claims description 4
- 238000005859 coupling reaction Methods 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 238000012856 packing Methods 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 239000000945 filler Substances 0.000 claims description 3
- 238000011049 filling Methods 0.000 claims description 2
- 238000005086 pumping Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 abstract description 19
- 230000007613 environmental effect Effects 0.000 abstract description 2
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 12
- 238000004090 dissolution Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 239000000498 cooling water Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 3
- 102000004169 proteins and genes Human genes 0.000 description 3
- 108090000623 proteins and genes Proteins 0.000 description 3
- 239000005894 Emamectin Substances 0.000 description 2
- 230000000853 biopesticidal effect Effects 0.000 description 2
- CXEGAUYXQAKHKJ-NSBHKLITSA-N emamectin B1a Chemical compound C1=C[C@H](C)[C@@H]([C@@H](C)CC)O[C@]11O[C@H](C\C=C(C)\[C@@H](O[C@@H]2O[C@@H](C)[C@H](O[C@@H]3O[C@@H](C)[C@H](NC)[C@@H](OC)C3)[C@@H](OC)C2)[C@@H](C)\C=C\C=C/2[C@]3([C@H](C(=O)O4)C=C(C)[C@@H](O)[C@H]3OC\2)O)C[C@H]4C1 CXEGAUYXQAKHKJ-NSBHKLITSA-N 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000000575 pesticide Substances 0.000 description 2
- 239000008213 purified water Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- AZSNMRSAGSSBNP-UHFFFAOYSA-N 22,23-dihydroavermectin B1a Natural products C1CC(C)C(C(C)CC)OC21OC(CC=C(C)C(OC1OC(C)C(OC3OC(C)C(O)C(OC)C3)C(OC)C1)C(C)C=CC=C1C3(C(C(=O)O4)C=C(C)C(O)C3OC1)O)CC4C2 AZSNMRSAGSSBNP-UHFFFAOYSA-N 0.000 description 1
- SPBDXSGPUHCETR-JFUDTMANSA-N 8883yp2r6d Chemical compound O1[C@@H](C)[C@H](O)[C@@H](OC)C[C@@H]1O[C@@H]1[C@@H](OC)C[C@H](O[C@@H]2C(=C/C[C@@H]3C[C@@H](C[C@@]4(O[C@@H]([C@@H](C)CC4)C(C)C)O3)OC(=O)[C@@H]3C=C(C)[C@@H](O)[C@H]4OC\C([C@@]34O)=C/C=C/[C@@H]2C)/C)O[C@H]1C.C1C[C@H](C)[C@@H]([C@@H](C)CC)O[C@@]21O[C@H](C\C=C(C)\[C@@H](O[C@@H]1O[C@@H](C)[C@H](O[C@@H]3O[C@@H](C)[C@H](O)[C@@H](OC)C3)[C@@H](OC)C1)[C@@H](C)\C=C\C=C/1[C@]3([C@H](C(=O)O4)C=C(C)[C@@H](O)[C@H]3OC\1)O)C[C@H]4C2 SPBDXSGPUHCETR-JFUDTMANSA-N 0.000 description 1
- 240000008415 Lactuca sativa Species 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000012258 culturing Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- QLFZZSKTJWDQOS-YDBLARSUSA-N doramectin Chemical compound O1[C@@H](C)[C@H](O)[C@@H](OC)C[C@@H]1O[C@@H]1[C@@H](OC)C[C@H](O[C@@H]2C(=C/C[C@@H]3C[C@@H](C[C@@]4(O3)C=C[C@H](C)[C@@H](C3CCCCC3)O4)OC(=O)[C@@H]3C=C(C)[C@@H](O)[C@H]4OC\C([C@@]34O)=C/C=C/[C@@H]2C)/C)O[C@H]1C QLFZZSKTJWDQOS-YDBLARSUSA-N 0.000 description 1
- 229960003997 doramectin Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 229960002418 ivermectin Drugs 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 235000012045 salad Nutrition 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Classifications
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0018—Evaporation of components of the mixture to be separated
- B01D9/0027—Evaporation of components of the mixture to be separated by means of conveying fluid, e.g. spray-crystallisation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/02—Crystallisation from solutions
-
- 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
- C07H1/08—Separation; Purification from natural products
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Biochemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Biotechnology (AREA)
- General Health & Medical Sciences (AREA)
- Genetics & Genomics (AREA)
- Molecular Biology (AREA)
- Crystallography & Structural Chemistry (AREA)
- Saccharide Compounds (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention relates to an extraction and purification method and an extraction and purification device of avermectin, which comprise the steps of filtering an avermectin fermentation liquor by a plate frame, flash drying, leaching by methanol, concentrating leaching liquor, removing impurities, and recrystallizing, wherein the water supplementing time in the impurity removing treatment process is 6-7 times of the original volume when the leaching liquor is concentrated to the crystallization, and the water washing is assisted by adopting a tank bottom straight-through steam method, so that the water washing efficiency is improved, the water consumption of the impurity removing treatment (only 0.5-1 time of the volume of the methanol concentrated liquor) is reduced, and the environmental protection pressure of enterprises is reduced; on the premise of ensuring the concentration efficiency, the problem that the material is difficult to start stirring to dissolve due to the fact that large hard materials are generated in the early stage of cooling is solved.
Description
Technical field:
the invention relates to an extraction and purification method and an extraction and purification device for abamectin, and belongs to the technical field of pesticide product production.
The background technology is as follows:
avermectin is a novel antibiotic and has the characteristics of novel structure and dual purposes of farm animals. With the improvement of the living standard of people and the call of green foods, the biopesticide is favored in the current pesticide market, and the avermectin is the most popular and highly competitive new product in the current biopesticide market. Moreover, with the massive development of downstream derived products such as emamectin, ivermectin, emamectin, doramectin, eplerinomectin and salad, the demand of avermectin on the market will increase, and in particular the demand of avermectin fine powder will increase.
In the prior art, the extraction of the avermectin comprises the steps of filtering an avermectin fermentation liquid through a plate frame, flash drying, leaching with methanol, concentrating and removing the methanol to obtain a concentrated solution, removing impurities, crystallizing for three times and wetting powder for three times to obtain avermectin fine powder. In the extraction method, the impurity removal treatment mainly utilizes a water washing method to remove water-soluble sugar, protein and other impurities in the avermectin leaching concentrated solution, thereby improving the intrinsic quality of the avermectin. At present, a toluene extraction method is widely adopted for impurity removal treatment, namely, toluene is used as an extractant to extract a leaching concentrated solution of the previous methanol removal into a toluene phase, and then a water washing method is adopted to remove impurities in the toluene phase.
The Chinese patent document CN103613624B discloses a refining method of abamectin, which is characterized in that the impurity treatment is to add hot water into concentrated methanol solution after concentration for washing, then cool and pump out wastewater with water-soluble sugar and protein on the upper layer, repeat washing for 2-3 times until the water layer is clear and the residual sugar is less than 0.05g/100ml; although the method well removes the impurities such as water-soluble sugar, protein and the like in the avermectin leaching solution, the time for adding hot water in the process is selected in the process of removing the methanol concentrated solution, at the moment, the concentrated solution is thick paste, the water washing is only on the surface of the material, the water washing efficiency is low, the water quantity is large (the water adding quantity is 5-10 times of the volume of the methanol concentrated solution, and the water washing is repeated for 2-3 times); in addition, after the upper water is pumped out by the process for cooling, the lower material is formed into a large hard block, so that great difficulty is brought to the dissolution and crystallization of the methanol in the later stage, and the whole stirring and dissolution process has great damage to the extraction device.
The invention comprises the following steps:
aiming at the defects of the prior art, the invention provides an extraction and purification method of abamectin, which has high water washing impurity removal efficiency and small water consumption.
The invention also provides an extraction and purification device of avermectin, which solves the problem that large hard blocks are difficult to dissolve and crystallize in the later working procedure of the conventional water washing process.
The invention is realized by the following technical scheme:
the extraction and purification method of the avermectin comprises the steps of filtering an avermectin fermentation liquid by a plate frame, flash drying, leaching by methanol, concentrating leaching liquid, removing impurities, and recrystallizing, and is characterized in that the impurity removing treatment is specifically as follows:
(1) Introducing the avermectin leaching solution into a double-effect concentrator, concentrating at the temperature of 65-70 ℃ and the vacuum degree of 0.04-0.06 mpa, transferring into a concentrating crystallization tank, and supplementing purified hot water to obtain a mixed leaching solution;
(2) Starting a methanol distillation valve of a concentrating and crystallizing tank, introducing saturated steam from the bottom of the tank to continuously concentrate the mixed leaching solution, stirring the mixed leaching solution simultaneously in the concentrating process, stopping introducing the saturated steam when the temperature on a methanol distillation and collection pipeline reaches 90-95 ℃, cooling the leaching and concentrating solution when the residual quantity of methanol in the leaching and concentrating solution is less than or equal to 1wt%, standing and layering, and pumping out upper water;
(3) Filling methanol with the volume of 1.5-2 times of the lower layer caking material from the bottom of the concentrating and crystallizing tank and the temperature of 55-60 ℃, starting an inner layer paddle type stirring paddle of the concentrating and crystallizing tank, starting an outer layer frame type stirring paddle after the outer layer stirring slowly rotates along with the material, and stirring until the lower layer material is completely dissolved to obtain a to-be-crystallized liquid;
(4) And cooling and crystallizing the to-be-crystallized liquid, centrifuging and recrystallizing for three times to obtain the abamectin fine powder.
According to the present invention, the concentration in the step (1) is preferably performed to 6 to 7 times the original volume.
According to the invention, the temperature of the purified hot water fed in step (1) is preferably 70-80 ℃, and the feeding amount is 0.5-1 times of the volume of the concentrated solution.
According to the invention, the saturated steam temperature in the step (2) is 150-160 ℃, and the temperature on the methanol distillation collecting pipeline is reached to 90-95 ℃ in 3-4 hours.
The invention adopts the saturated steam introduced into the tank bottom, so that the concentration rate can be improved, and meanwhile, the saturated steam is liquefied into water after entering the tank to contact materials, and the concentration process is also a water washing process.
According to the invention, in the step (3), the concentration of the methanol fed into the tank bottom is 95-98 wt%.
According to the invention, in the step (3), the stirring rotation speed of the inner-layer paddle type stirring paddle is 40-60 r/min, and the stirring time is 10-15 min; the stirring speed of the outer frame type stirring paddle is 20-30 r/min, and the stirring time is 20-30 min.
According to the invention, in the step (4), the transmittance of the dichloromethane solution of the obtained abamectin fine powder is more than or equal to 96%.
The double-effect concentrator is efficient and energy-saving concentrating equipment for the traditional Chinese medicine leaching liquor, and the water supplementing is started when the leaching liquor is crystallized, namely, the original volume is 6-7 times, so that the water washing effect is improved.
According to the method for detecting the transmittance of the dichloromethane dissolution liquid of the fine avermectin powder, which is preferred in the invention, 1g of the fine avermectin powder is taken to be dissolved in 10ml of dichloromethane, the transmittance of the dichloromethane dissolution liquid is detected by a spectrophotometer under the spectrum of 448nm, the water-soluble impurities in the fine avermectin powder can not be dissolved and are turbid due to the fact that the dichloromethane is a fat-soluble solvent, the amount of the water-soluble impurities in the fine avermectin powder can be qualitatively measured by detecting the transmittance of the dichloromethane dissolution liquid, and then the water washing effect of the impurity removal treatment step is evaluated.
The invention also provides a concentrating crystallization tank for the extraction and purification method of avermectin.
A concentrating crystallization tank for an abamectin extraction and purification method comprises a crystallization tank body and a stirrer; the crystallization tank body is of a closed tank body structure with a cavity inside, and the top end of the crystallization tank body is provided with a nitrogen inlet, a methanol distillation port and an inverted umbrella-shaped splash-proof device; the cooling coil is arranged on the outer side of the periphery of the crystallization tank body, one end of the cooling coil is a water inlet, the other end of the cooling coil is a water inlet, and the stirrer comprises a motor, a stirring shaft and a stirring paddle; the motor drives the stirring shaft, and the stirring shaft drives the stirring paddle to rotate.
According to the invention, preferably, the stirring paddles comprise an inner-layer paddle stirring paddle and an outer-layer frame stirring paddle, the outer-layer frame stirring paddle is positioned outside the inner-layer paddle stirring paddle, the inner-layer paddle stirring paddle and the outer-layer frame stirring paddle are coaxially arranged, the motor comprises an inner-layer paddle stirring motor and an outer-layer frame stirring motor, the inner-layer paddle stirring motor drives a stirring shaft to drive the inner-layer paddle stirring paddle to rotate, the outer-layer frame stirring motor drives the stirring shaft to drive the outer-layer frame stirring paddle to rotate, and the inner-layer paddle stirring motor is connected with the outer-layer frame stirring motor through a coupling.
According to the invention, packing filler is filled between the inner-layer paddle type stirring motor and the outer-layer frame type stirring motor for sealing.
According to the invention, the outer layer frame type stirring paddle is a frequency conversion frame type stirring paddle, the output revolution is 0.1-30 r/min, and the output power is 1.5-1.8 kw per cubic tank volume; the inner-layer paddle type stirring paddle is a variable-frequency paddle type stirring paddle, the output revolution is 0.1-60 min, and the output power is 1.8-2.0 kw per cubic tank volume.
According to a preferred embodiment of the invention, the bottom of the concentrating crystallization tank is provided with a hot methanol inlet/crystallization liquid outlet and a steam inlet.
The inverted umbrella-shaped splash-proof device has the main function of preventing avermectin leaching liquor from splashing in the later stage of direct steam concentration at the bottom of the tank, so that distilled methanol solvent is impure and recovery is influenced;
when the stirring paddle is used for distillation, frame stirring is started, and as the gap between the frame stirring and the tank wall is smaller and the stirring range is large, the heat transfer process is performed during distillation, and the water washing is more sufficient; in the initial stage of dissolving the lower layer caking material, the material is cooled hard in the early stage, and the paddle type stirring is started, and the paddle type stirring blade is small and has a certain inclination angle, so that the resistance is small when the paddle type stirring is started, and the stirring is easy to start; after the middle part of the material is dissolved and softened, frame type stirring is started to promote the material to be dissolved rapidly and completely.
The invention has the following positive effects:
1. according to the method, the water supplementing time in the impurity removing treatment process is advanced, water supplementing is started when the leaching solution is concentrated until crystallization occurs, namely, the original volume is 6-7 times, and water washing is assisted by adopting a tank bottom direct steam method, so that the water washing efficiency is improved, the water consumption of the impurity removing treatment is reduced, and the environmental protection pressure of enterprises is reduced;
2. according to the method, when the temperature on the methanol distillation collecting pipeline reaches 90-95 ℃, the saturated steam is stopped, the whole process is easy to operate and control, the terminal point is easy to judge, and the distillation operation standardization is realized.
3. According to the method, the light transmittance of the dichloromethane solution of the abamectin fine powder is used as a standard for measuring the impurity removing effect of the previous step, so that the method is more accurate (water-soluble impurities can be measured, and not only residual sugar) and the method can be used for measuring the impurity removing effect of the previous step;
4. the concentrating crystallization tank improves the operability of the impurity removal treatment process. The equipment skillfully adopts independently controlled coaxial stirring, and solves the problem that the stirring is difficult to be started to dissolve materials due to the fact that the materials with large hard blocks are generated by early-stage cooling under the premise of ensuring the concentration efficiency.
Drawings
FIG. 1 is a schematic structural diagram of a concentrating crystallization tank for an extraction and purification method of avermectin
In the figure, 1, an inner-layer paddle type stirring motor, 2, a coupling, 3, packing sealing, 4, an outer-layer frame type stirring motor, 5, a nitrogen inlet, 6, an outer-layer frame type stirring paddle, 7, an inner-layer paddle type stirring paddle, 8, a support (a discharge hole with DN 80), 9, a hot methanol inlet/crystallization liquid outlet, 10, a steam inlet, 11, an inverted umbrella type splash guard, 12, a cooling coil (a steam/cooling water inlet and outlet)
The specific embodiment is as follows:
example 1
A concentrating crystallization tank for avermectin extraction and purification method has a structure shown in figure 1 and comprises a crystallization tank body and a stirrer; the crystallization tank body is of a closed tank body structure with a cavity inside, and the top end of the crystallization tank body is provided with a nitrogen inlet 5, a methanol distillation port and an inverted umbrella-shaped splash-proof device 11; the cooling coil 12 is arranged on the outer side of the periphery of the crystallization tank body, one end of the cooling coil 12 is a water inlet, the other end of the cooling coil is a water inlet, and the stirrer comprises a motor, a stirring shaft and a stirring paddle; the motor drives the stirring shaft, and the stirring shaft drives the stirring paddle to rotate.
The stirring rake includes inlayer oar formula stirring rake 6 and outer frame stirring rake 7, and outer frame stirring rake 6 is located the outside of inlayer oar formula stirring rake 7, and inlayer oar formula stirring rake 6 and outer frame stirring rake 7 coaxial setting, the motor include inlayer oar formula stirring motor 1 and outer frame stirring motor 4, inlayer oar formula stirring motor 1 drive (mixing) shaft drive inlayer oar formula stirring rake 7 rotation, outer frame stirring motor 4 drive (mixing) shaft drive outer frame stirring rake 6 rotation, inlayer oar formula stirring motor 1 passes through shaft coupling 2 with outer frame stirring motor 4 and is connected. Packing filler 3 is filled between the inner-layer paddle stirring motor 1 and the outer-layer frame stirring motor 4 for sealing.
The outer layer frame type stirring paddle 6 is a frequency conversion frame type stirring paddle, the output revolution is 0.1-30 r/min, and the output power is 1.5-1.8 kw per cubic tank volume; the inner-layer paddle type stirring paddle 7 is a variable-frequency paddle type stirring paddle, the output revolution is 0.1-60 min, and the output power is 1.8-2.0 kw per cubic tank volume.
The bottom of the concentration crystallization tank is provided with a hot methanol inlet/crystallization liquid outlet 9 and a steam inlet 10.
The method for extracting and purifying the avermectin by utilizing the concentrating crystallization tank comprises the following steps:
filtering avermectin fermentation liquor by a plate frame, flash drying, leaching with methanol to obtain avermectin leaching liquor, concentrating 28000L avermectin leaching liquor (with the titer of 13000 u/ml) by a double-effect concentrator at the temperature of 65-70 ℃ and the vacuum degree of 0.04-0.06 mpa until crystallization appears on a test mirror, namely concentrating to 4000L, transferring into a concentrating crystallization tank, and supplementing purified water with the concentration liquid volume of 2000L and the temperature of 70 ℃;
starting a methanol distillation valve of a concentration crystallization tank, starting frame stirring of the concentration crystallization tank, starting a tank bottom saturated steam valve to continuously concentrate leaching concentrated solution, concentrating and washing with water for 3-4 hours, wherein the temperature on a methanol distillation collecting pipeline reaches 95 ℃, closing the tank bottom saturated steam valve, after methanol distillation is finished, opening a coil pipe of the concentration crystallization tank, cooling water to room temperature, standing and layering, extracting upper water, and detecting that the residual quantity of methanol is 0.8%;
adding 3000L of methanol with the temperature of 60 ℃ and the concentration of 96% from the bottom of a concentrating crystallization tank, starting the inner-layer paddle type stirring of the concentrating crystallization tank, adjusting the paddle type stirring speed to 50r/min at variable frequency, keeping the temperature and stirring for 15min, slowly rotating the outer-layer frame type stirring along with the starting of the materials, opening the outer-layer frame type stirring at a point, adjusting the speed to 20r/min at variable frequency, keeping the temperature and stirring for 30min, and completely dissolving the lower-layer materials;
opening a coil pipe of a concentrating crystallization tank, cooling and crystallizing at 4 ℃, cooling for 12 hours, preserving heat and crystallizing for 2 hours, centrifuging, recrystallizing for three times to obtain abamectin fine powder, and detecting the light transmittance of a dichloromethane solution of the abamectin fine powder to 97 percent;
example 2
A concentrating and crystallizing tank for an extraction and purification method of abamectin has the same structure as in example 1.
The method for extracting and purifying the avermectin by utilizing the concentrating crystallization tank comprises the following steps:
filtering avermectin fermentation liquor by a plate frame, flash drying, leaching with methanol to obtain avermectin leaching liquor, concentrating 24000L avermectin leaching liquor (titer: 14200 u/ml) by a double-effect concentrator at the temperature of 65-70 ℃ and the vacuum degree of 0.04-0.06 mpa until crystallization appears on a test mirror, namely concentrating to 3600L, transferring into a concentrating crystallization tank, and supplementing purified water with the concentration liquid volume of 1800L and the temperature of 80 ℃;
starting a methanol distillation valve of a concentration crystallization tank, starting frame stirring of the concentration crystallization tank, starting a tank bottom saturated steam valve to continuously concentrate leaching concentrated solution, concentrating and washing with water for 3-4 hours, wherein the temperature on a methanol distillation collecting pipeline reaches 92 ℃, closing the tank bottom saturated steam valve, after methanol distillation is finished, opening a coil pipe of the concentration crystallization tank, cooling water to room temperature, standing and layering, extracting upper water, and detecting that the residual quantity of methanol is 0.9%;
adding 2800L of methanol with the temperature of 60 ℃ and the concentration of 95% from the bottom of a concentrating and crystallizing tank, starting the inner-layer paddle type stirring of the concentrating and crystallizing tank, adjusting the paddle type stirring speed to 60r/min at variable frequency, keeping the temperature and stirring for 10min, slowly rotating the outer-layer frame type stirring along with the starting of the material, opening the outer-layer frame type stirring at a point, adjusting the speed to 30r/min at variable frequency, keeping the temperature and stirring for 20min, and completely dissolving the lower-layer material;
and (3) opening a coil pipe of a concentrating crystallization tank, cooling with cooling water at 4 ℃ for crystallization, cooling for 12 hours, preserving heat and culturing crystals for 2 hours, centrifuging, recrystallizing for three times to obtain abamectin fine powder, and detecting the light transmittance of the dichloromethane solution of the abamectin fine powder to 98%.
Example 3
A concentrating and crystallizing tank for an extraction and purification method of abamectin has the same structure as in example 1.
The extraction and purification method of avermectin by using a concentration crystallization tank is the same as that of example 1, except that the temperature of the saturated steam is 158 ℃.
Experimental example 1
The conditions of the fine avermectin powder prepared by the extraction and purification method of the avermectin in the embodiment 2 are the same as those in the embodiment 2.
Comparative example 1
The method for extracting and purifying avermectin as described in experimental example 1 has the same conditions as experimental example 1, and is characterized in that the special concentration crystallization tank for avermectin adopts variable-frequency anchor type stirring (belt transmission)
Experimental example 2
The conditions of the fine avermectin powder prepared by the extraction and purification method of avermectin as described in the embodiment 2 are the same as those of the embodiment 2, except that the temperature is 60-65 ℃ when the methanol is dissolved
Comparative example 2
The method for extracting and purifying avermectin as described in experimental example 2 has the same conditions as experimental example 2, and is characterized in that the special concentration crystallization tank for avermectin adopts variable-frequency anchor type stirring (belt transmission)
Experimental example 3
The method for extracting and purifying avermectin as described in the embodiment 3 is the same as the embodiment 2, except that the temperature is 65-70 ℃ and the concentration is 98% when methanol is dissolved.
Comparative example 3
The method for extracting and purifying avermectin as described in experimental example 3 has the same conditions as those of the embodiment 2, and is characterized in that the special concentration crystallization tank for avermectin adopts variable-frequency anchor stirring (belt transmission).
The time taken for the experimental examples 1 to 3 and comparative examples 1 to 3 to be turned on by stirring, and the experimental results in the on state are compared with those shown in the following table 1:
TABLE 1 influence of different treatments on stirring
Claims (5)
1. The extraction and purification method of avermectin comprises the steps of filtering an avermectin fermentation liquor frame, flash drying, leaching with methanol, concentrating leaching liquor, removing impurities and recrystallizing,
the impurity removal treatment is specifically as follows:
(1) Introducing avermectin leaching solution into a double-effect concentrator, concentrating to 6-7 times of the original volume under the conditions of the temperature of 65-70 ℃ and the vacuum degree of 0.04-0.06 mpa, transferring into a concentrating crystallization tank, and supplementing purified hot water to obtain mixed leaching solution; the temperature of the purified hot water is 70-80 ℃, and the adding amount is 0.5-1 times of the volume of the concentrated solution;
the concentrating crystallization tank comprises a crystallization tank body and a stirrer; the crystallization tank body is of a closed tank body structure with a cavity inside, and the top end of the crystallization tank body is provided with a nitrogen inlet, a methanol distillation port and an inverted umbrella-shaped splash-proof device; the cooling coil is arranged on the outer side of the periphery of the crystallization tank body, one end of the cooling coil is a water inlet, the other end of the cooling coil is a water inlet, and the stirrer comprises a motor, a stirring shaft and a stirring paddle; the motor drives the stirring shaft, the stirring shaft drives the stirring paddle to rotate, the stirring paddle comprises an inner-layer paddle stirring paddle and an outer-layer frame stirring paddle, the outer-layer frame stirring paddle is positioned outside the inner-layer paddle stirring paddle, the inner-layer paddle stirring paddle and the outer-layer frame stirring paddle are coaxially arranged, the motor comprises an inner-layer paddle stirring motor and an outer-layer frame stirring motor, the inner-layer paddle stirring motor drives the stirring shaft to drive the inner-layer paddle stirring paddle to rotate, and the outer-layer frame stirring motor drives the stirring shaft to drive the outer-layer frame stirring paddle to rotate, and the inner-layer paddle stirring motor is connected with the outer-layer frame stirring motor through a coupling;
(2) Starting a methanol distillation valve of a concentrating and crystallizing tank, introducing saturated steam from the bottom of the tank to continuously concentrate the mixed leaching solution, stirring the mixed leaching solution simultaneously in the concentrating process, stopping introducing the saturated steam when the temperature on a methanol distillation and collection pipeline reaches 90-95 ℃, cooling the leaching and concentrating solution to room temperature when the residual quantity of methanol in the leaching and concentrating solution is less than or equal to 1wt%, standing and layering, and pumping out upper water; the saturated steam temperature is 150-160 ℃, and the temperature on a methanol distillation and collection pipeline reaches 90-95 ℃ in 3-4 hours;
(3) Filling methanol with the volume of 1.5-2 times of the lower layer caking material from the bottom of the concentrating and crystallizing tank and the temperature of 55-60 ℃, starting an inner layer paddle type stirring paddle of the concentrating and crystallizing tank, starting an outer layer frame type stirring paddle after the outer layer stirring slowly rotates along with the material, and stirring until the lower layer material is completely dissolved to obtain a to-be-crystallized liquid;
(4) And cooling and crystallizing the to-be-crystallized liquid, centrifuging and recrystallizing for three times to obtain the abamectin fine powder.
2. The extraction and purification method of avermectin as claimed in claim 1, wherein,
in the step (3), the concentration of the methanol fed into the tank bottom is 95-98 wt%.
3. The extraction and purification method of avermectin as claimed in claim 1, wherein,
in the step (3), the stirring rotation speed of the inner-layer paddle type stirring paddle is 40-60 r/min, and the stirring time is 10-15 min; the stirring speed of the outer frame type stirring paddle is 20-30 r/min, and the stirring time is 20-30 min.
4. The extraction and purification method of avermectin as claimed in claim 1, wherein,
in the step (4), the transmittance of the dichloromethane solution of the obtained avermectin fine powder is more than or equal to 96 percent.
5. The extraction and purification method of avermectin as claimed in claim 1, wherein,
packing filler is filled between the inner-layer paddle type stirring motor and the outer-layer frame type stirring motor for sealing, the outer-layer frame type stirring paddle is a frequency conversion frame type stirring paddle, the output revolution is 0.1-30 r/min, and the output power is 1.5-1.8 kw per cubic tank volume; the inner-layer paddle type stirring paddle is a variable-frequency paddle type stirring paddle, the output revolution is 0.1-60 min, the output power is 1.8-2.0 kw per cubic tank volume, and the bottom of the concentration crystallization tank is provided with a hot methanol inlet/crystallization liquid outlet and a steam inlet.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102060897A (en) * | 2011-01-07 | 2011-05-18 | 石家庄市兴柏生物工程有限公司 | Method for preparing abamectin |
| CN102993252A (en) * | 2012-12-31 | 2013-03-27 | 齐鲁制药（内蒙古）有限公司 | Method and device for extracting avermectins |
| CN103613624A (en) * | 2013-12-05 | 2014-03-05 | 宁夏启元药业有限公司 | Refining method of avermectin |
| CN203886551U (en) * | 2014-06-26 | 2014-10-22 | 宁波大红鹰生物工程股份有限公司 | Reactor |
| CN106188188A (en) * | 2016-08-23 | 2016-12-07 | 华北制药集团爱诺有限公司 | A kind of preparation method of avilamycin |
| CN106478369A (en) * | 2016-08-30 | 2017-03-08 | 齐鲁制药（内蒙古）有限公司 | A kind of low energy consumption recovery system of AVM Extraction solvent and technique |
-
2018
- 2018-04-20 CN CN201810362653.2A patent/CN108440622B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102060897A (en) * | 2011-01-07 | 2011-05-18 | 石家庄市兴柏生物工程有限公司 | Method for preparing abamectin |
| CN102993252A (en) * | 2012-12-31 | 2013-03-27 | 齐鲁制药（内蒙古）有限公司 | Method and device for extracting avermectins |
| CN103613624A (en) * | 2013-12-05 | 2014-03-05 | 宁夏启元药业有限公司 | Refining method of avermectin |
| CN203886551U (en) * | 2014-06-26 | 2014-10-22 | 宁波大红鹰生物工程股份有限公司 | Reactor |
| CN106188188A (en) * | 2016-08-23 | 2016-12-07 | 华北制药集团爱诺有限公司 | A kind of preparation method of avilamycin |
| CN106478369A (en) * | 2016-08-30 | 2017-03-08 | 齐鲁制药（内蒙古）有限公司 | A kind of low energy consumption recovery system of AVM Extraction solvent and technique |
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