CN100424090C - Extraction technology of avermectin - Google Patents
Extraction technology of avermectin Download PDFInfo
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- CN100424090C CN100424090C CNB2006100483498A CN200610048349A CN100424090C CN 100424090 C CN100424090 C CN 100424090C CN B2006100483498 A CNB2006100483498 A CN B2006100483498A CN 200610048349 A CN200610048349 A CN 200610048349A CN 100424090 C CN100424090 C CN 100424090C
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- lixiviate
- filter membrane
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- avrmectin
- vat liquor
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Abstract
The invention discloses an extracting technology of avermectin, which comprises the following steps: blending dried mycelium of avermectin and carbinol or alcohol with weight rate at 1: 5-1: 10 in the immersing tank; stirring under 20-25 deg.c for 3-6h; filtering the filtrate under 0.1-0.6Mpa through filter membrane system with aperture at 10um-2nm; transmitting filtrate to semiproduct manufacturing system; returning partial residual liquid to immersing tank; entering the other half filtrate in the filter membrane circulating system through circulating pump; draining the slag in the immersing tank after filtering.
Description
Technical field
The present invention relates to biological pesticide products production field, particularly a kind of avermectin extraction technology.
Background technology
Along with the raising of people's living standard and to the call of green food, biological pesticide gains great popularity in current agricultural chemicals market, and Avrmectin is most popular and have a biological pesticide product of development potentiality in the current biological pesticide market.
As a kind of novel biopesticide, Avrmectin has following distinct advantages: insecticidal spectrum is wide, and various insects, mite and zooparasite are all had very strong insecticidal activity; The insecticidal mechanism uniqueness do not have cross resistance with the medicament of using always, and efficiency time is long; Easily degraded in soil and water, it is residual also not have accumulation and persistence in vivo, does not pollute the environment, nuisanceless.Therefore, in occupation of increasing share, development prospect is very optimistic in agricultural chemicals and veterinary drug market for Avrmectin and derivative thereof.
In present avermectin extraction technology process, need remove wherein moisture content with Plate Filtration, after the mycelium oven dry, to leach with 5～10 times of ethanol to mycelium weight, alcohol extracting 3～6 hours (constantly stirring), sedimentation is 2～4 hours again, an alcohol extract Plate Filtration; With ethanol leaching 3～6h, the secondary alcohol extract is used Plate Filtration to mycelium after the filtration more again; With ethanol leaching 3～6h, three times alcohol extract is used Plate Filtration to mycelium after the filtration more again, and three times so repeatedly, tiring in the mycelium residue gets final product below 100～300mg/L.Filtrate enters next process as work in-process and handles.
Adopt this kind mode to filter and exist the defective that the alcohol extracting filtration time is long, the production cycle is long, the Plate Filtration precision is low and product purity is not high; Simultaneously, ethanol large usage quantity in the alcohol extract filtration procedure, its consumption is 15～30 times of mycelium weight, and because Plate Filtration is non-closed-loop operation, and material contacts with atmosphere in whole Plate Filtration process, ethanol volatilization loss is serious, the amount of alcohol of the annual volatilization loss of the Avrmectin factory that year designed capacity is 100 tons just reaches 2000～3000 tons, and the production environment smell is unpleasant unusually, noise is big, and the employee work environment is abominable, causes serious harm to healthy.
In sum, seeking a kind of airtight filter operation system fully, reduce the ethanol evaporation loss, shorten the production cycle, replace ethanol with cheap methyl alcohol as the mycelium leaching liquid, save production cost, is problem anxious to be solved during Avrmectin is produced.
Summary of the invention
The purpose of this invention is to provide a kind of avermectin extraction technology, to solve the problem that prior art exists.
For realizing the object of the invention, this avermectin extraction technology is characterized in that may further comprise the steps:
A. with the dried mycelium of Avrmectin and methyl alcohol or ethanol with 1: 5～1: 10 weight ratio in the lixiviate in-tank mixing, after continuing to stir 3～6 hours under 20～25 ℃ of temperature, make vat liquor;
B. under 0.1～0.6Mpa pressure, be that the filter membrane system of 10 μ m～2nm filters with above-mentioned vat liquor by the aperture;
C. send into the work in-process system of processing by the filtrate of filter membrane system, a raffinate part is returned the lixiviate jar, and another part passes through the filter membrane system circulating filtration behind recycle pump.
When described vat liquor volume is 3～5 times of dope volume, add methyl alcohol or ethanol lixiviate once more, it is 1.5～2.5 times of the former lixiviate liquid measure of Avrmectin that the lixiviate amount promptly adds methyl alcohol or alcoholic acid amount once more.
Adopt ceramic membrane, stainless steel membrane or hollow-fibre membrane in the described filter membrane system.Wherein the ceramic membrane aperture that can adopt Jiangsu Jiuwu High-Tech Co., Ltd. or German ATECH technological development company limited to produce is the ceramic filter membrane of 10 μ m～2nm; The aperture that stainless steel membrane can adopt Ruitong Meibang Engineering Co., Ltd., Hebei Prov. or triumphant membrane filtration technique company limited to produce is the stainless steel filtering membrane of 10 μ m～50nm; The aperture that hollow-fibre membrane can adopt Dutch X-FLOW company, film sky film engineering company limited of Tianjin University of Technology or membrane sepn Engineering Co., Ltd of Tianjin old name for the Arabian countries in the Middle East to produce is the hollow fiber ultrafiltration membrane of 10 μ m～2nm.
The described ratio that is controlled at the inner vat liquor flow that participates in circulating filtration of filter membrane system and the raffinate flow that returns the lixiviate jar is preferably 10: 1～and 16: 1.
The technical progress that the present invention obtains:
(1). owing to adopt technology of the present invention and adopt closed membrane filtration system filtration, can separate, clarify the Avrmectin vat liquor effectively, reduce secondary and three leaching process, filtration velocity is fast, the level of automation height, the filtering accuracy height, with existing production technique relatively, technological process can shorten 6～12 hours every day.
(2). owing to adopt closed membrane filtration system filtration, the Avrmectin product quality is improved, can improves product purity, shorten the production cycle, improve product production, greatly improved the not enough present situation of domestic Avrmectin supply and demand, reduce import, meet the need of market.
(3). adopt closed membrane filtration system filtration, thereby can adopt the more cheap solvent methanol of price as vat liquor, and avoided the volatilization of methyl alcohol or alcoholic acid to reveal the solvent loss that causes, reduced production cost, simultaneously greatly improved Working environment, it is healthy to help the operator.
(4). compare with existing technology, the application of membrane filtration system in avermectin extraction technology of closed effectively overcome the drawback of traditional Plate Filtration production technique, can save the time of secondary alcohol extracting and three alcohol extractings, shorten the production cycle, reduce production costs, product quality is improved, output improves, energy consumption reduces, by statistics, process recovery ratio of the present invention can improve 5～7%, and the Avrmectin yield can reach more than 95%, and membrane filtration system long service life has remarkable economic efficiency and social benefit.
Description of drawings
Fig. 1 is a process flow diagram of the present invention.Wherein 1 represents Avrmectin lixiviate jar, and 2 is the closed filter membrane system, and 3 is charging pump, and 4 is recycle pump.
Embodiment
Embodiment 1: as shown in Figure 1, after Avrmectin mycelium dry put into lixiviate jar 1, add organic solvent ethanol with 1: 5 weight ratio, after continuing down for 20～25 ℃ to stir 3～6 hours, normal temperature makes vat liquor, this vat liquor is that the ceramic filtration membrane system 2 of 10 μ m～2nms filter by the aperture through charging pump 3 under 0.1～0.6Mpa pressure then, the aperture that ceramic membranes adopt Jiangsu Jiuwu High-Tech Co., Ltd. or adopt German ATECH technological development company limited to produce in the filter membrane system 2 is 10 μ m～2nm ceramic filter membrane filtration, send into follow-up work in-process system of processing by the filtrate of filter membrane, do not return lixiviate jar 1 by the raffinate part of filter membrane, another part raffinate passes through ceramic filtration membrane system 2 circulating filtrations behind recycle pump 4, the ratio that is controlled at the inner vat liquor flow that participates in circulating filtrations of ceramic filtration membrane system 2 and the raffinate flow that returns lixiviate jar 1 is 10: 1, this moment, system carried out the clarification of Avrmectin vat liquor automatically, separate, leaching process, when lixiviate liquid measure volume is 3～5 times of raffinate amount volume, in lixiviate jar 1, add ethanol lixiviate once more, the alcoholic acid amount that add this moment is 1.5～2.5 times of the former lixiviate liquid measure of Avrmectin, when not tiring substantially in the mycelium, filter and finish, the residue that forms in the emptying lixiviate jar 1, and enter the by product treatment process.
Embodiment 2: the present embodiment difference from Example 1 is the weight ratio adding organic solvent ethanol with 1: 10; The ratio that is controlled at the inner vat liquor flow that participates in circulating filtrations of ceramic filtration membrane system 2 and the raffinate flow that returns lixiviate jar 1 is 16: 1; Filter membranes adopt stainless steel membranes in the filter membrane system 2, and the aperture that stainless steel membrane can adopt Ruitong Meibang Engineering Co., Ltd., Hebei Prov. or triumphant membrane filtration technique company limited to produce is 10 μ m～50nm stainless steel filtering membrane.
Embodiment 3: the present embodiment difference from Example 1 is the weight ratio adding organic solvent ethanol with 1: 7; The ratio that is controlled at the inner vat liquor flow that participates in circulating filtrations of ceramic filtration membrane system 2 and the raffinate flow that returns lixiviate jar 1 is 13: 1; Filter membranes adopt hollow-fibre membranes in the filter membrane system 2, and the aperture that hollow-fibre membrane can adopt Dutch X-FLOW company, film sky film engineering company limited of Tianjin University of Technology or membrane sepn Engineering Co., Ltd of Tianjin old name for the Arabian countries in the Middle East to produce is the hollow fiber ultrafiltration membrane of 10 μ m～2nm.
Embodiment 4: present embodiment and the various embodiments described above difference are with the methyl alcohol instead of ethanol.
Working process of the present invention is: the Avrmectin vat liquor is sent constantly into ceramic membrane, stainless steel membrane or hollow-fibre membrane system 2 filter assemblies through charging pump 3, carry out filtering separation; In this process, the continuous permeation ceramic membrane of the material less than membrane pore size, stainless steel membrane or hollow-fibre membrane in the material, and flow out from the filtrate outlet of ceramic membrane, stainless steel membrane or hollow fiber film assembly and to become high-quality Avrmectin work in-process, simultaneously the material greater than membrane pore size is that raffinate successively returns lixiviate jar 1 in the material, and enters ceramic membrane, stainless steel membrane or hollow-fibre membrane through charging pump 3 and carry out circulating filtration.When the lixiviate liquid measure is 3～5 times of raffinate amount, in lixiviate jar 1, begin to add methyl alcohol or ethanol lixiviate once more, add methyl alcohol or alcoholic acid amount this moment and be about 1.5～2.5 times of the former lixiviate liquid measure of Avrmectin, substantially do not tire in the mycelium this moment, filtration procedure finishes, and termination of pumping stops sepn process, with the work in-process of collecting is that Avrmectin sees through the aftertreatment that liquid carries out conventional steps, and obtains high-quality Avrmectin finished product.For stopping up, the fenestra that prevents ceramic membrane, stainless steel membrane or hollow-fibre membrane 2 reduces the membrane filtration effect, can regularly wash ceramic membrane, stainless steel membrane or hollow-fibre membrane 2 surfaces with clean-out system, adherent cake layer is rinsed well, membrane flux is recovered, thereby prevent that effectively film from polluting.
From above technological process as can be known, the present invention is directed to Avrmectin sheet frame extraction process production high-quality Avrmectin, the production technique that follows conventional lines, and adopt airtight ceramic membrane on this basis, stainless steel membrane or tubular fibre film separating system clarification Avrmectin vat liquor, material is at ceramic membrane, constantly circulation lixiviate in stainless steel membrane or the hollow-fibre membrane system, cross flow filter repeatedly, high-quality Avrmectin product is isolated in clarification, mycelium is tired and is constantly reduced in the jar of lixiviate simultaneously, substantially do not tire in the final mycelium, promptly tire when 100～300mg/l is following, finish the Avrmectin leaching process.
Claims (3)
1. avermectin extraction technology is characterized in that may further comprise the steps:
A. the dried mycelium of Avrmectin is mixed in lixiviate jar (1) with 1: 5～1: 10 weight ratio with methyl alcohol or ethanol, after continuing to stir 3～6 hours under 20～25 ℃ of temperature, make vat liquor;
B. under 0.1～0.6Mpa pressure, be that the closed filter membrane system (2) of 10 μ m～2nm filters with above-mentioned vat liquor by the aperture;
C. send into the work in-process system of processing by the filtrate of closed filter membrane system (2), a raffinate part is returned lixiviate jar (1), another part passes through closed filter membrane system (2) circulating filtration behind recycle pump (4), and, when being controlled at the inner vat liquor that participates in circulating filtration of closed filter membrane system (2) for 3～5 times of the raffinate volume that returns lixiviate jar (1), add methyl alcohol or ethanol lixiviate once more in lixiviate jar (1), the methyl alcohol of adding or alcoholic acid amount are 1.5～2.5 times of the former lixiviate liquid measure of Avrmectin.
2. avermectin extraction technology according to claim 1 is characterized in that described filter membrane adopts ceramic membrane, stainless steel membrane or hollow-fibre membrane.
3. avermectin extraction technology according to claim 1 is characterized in that the described vat liquor flow that is controlled at the inner participation of closed filter membrane system (2) circulating filtration is 10: 1～16: 1 with the ratio that returns the raffinate flow of lixiviate jar (1).
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2006100483498A CN100424090C (en) | 2006-09-27 | 2006-09-27 | Extraction technology of avermectin |
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| CNB2006100483498A CN100424090C (en) | 2006-09-27 | 2006-09-27 | Extraction technology of avermectin |
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| CN1923840A CN1923840A (en) | 2007-03-07 |
| CN100424090C true CN100424090C (en) | 2008-10-08 |
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| CNB2006100483498A Expired - Fee Related CN100424090C (en) | 2006-09-27 | 2006-09-27 | Extraction technology of avermectin |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102217591A (en) * | 2011-04-26 | 2011-10-19 | 张福志 | Environmentally-friendly abamectin ointment production process |
Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101362785B (en) * | 2008-10-06 | 2011-04-20 | 山东齐发药业有限公司 | Avermectin extraction technology and apparatus |
| CN103304608B (en) * | 2012-12-05 | 2015-10-21 | 福建凯立生物制品有限公司 | The production unit of the former powder of a kind of Zhongshengmycin and production method |
| CN102993252B (en) * | 2012-12-31 | 2015-07-29 | 齐鲁制药（内蒙古）有限公司 | A kind of extraction method of abamectin and device |
| CN104876990B (en) * | 2015-06-02 | 2017-11-14 | 宁夏泰瑞制药股份有限公司 | A kind of method for purifying emamectin benzoate crude product |
| CN105503982A (en) * | 2015-11-17 | 2016-04-20 | 石家庄市兴柏生物工程有限公司 | Abamectin extraction process |
| CN106039759B (en) * | 2016-06-16 | 2018-11-20 | 齐鲁制药（内蒙古）有限公司 | On-line filtration device in a kind of avermectin extraction process |
| CN106632552B (en) * | 2016-12-23 | 2019-05-14 | 宁夏泰益欣生物科技有限公司 | A kind of extracting method of Avermectin B1a |
| CN116530518B (en) * | 2023-04-19 | 2024-09-20 | 河北兴柏农业科技股份有限公司 | Streptomyces avermitilis mycelium water dispersible granule and preparation method thereof |
| CN116585747B (en) * | 2023-07-12 | 2023-10-27 | 江苏瑞科生物技术股份有限公司 | Lipopolysaccharide extraction device and extraction method |
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| CN102217591A (en) * | 2011-04-26 | 2011-10-19 | 张福志 | Environmentally-friendly abamectin ointment production process |
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