CN105503982A - Abamectin extraction process - Google Patents
Abamectin extraction process Download PDFInfo
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- CN105503982A CN105503982A CN201510791079.9A CN201510791079A CN105503982A CN 105503982 A CN105503982 A CN 105503982A CN 201510791079 A CN201510791079 A CN 201510791079A CN 105503982 A CN105503982 A CN 105503982A
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- toluene
- mycelium
- leaching
- extraction technology
- avermectin
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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
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- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- Biotechnology (AREA)
- General Health & Medical Sciences (AREA)
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- Preparation Of Compounds By Using Micro-Organisms (AREA)
Abstract
The present invention relates to an avermectin extraction process, the extraction process uses toluene as an extraction agent, can be directly used in a filtered fermentation broth, saves a flash evaporation dryer and a rectifying column of an original process, and the amount of the toluene as the extraction agent is far less than the amount of methanol as the extraction agent. The first advantage of the extraction process lies in eliminating of the flash evaporation dryer and the rectifying column, can reduce energy consumption, and has great significance to environmental protection and safe production, and secondly, the amount of the toluene is far less than the amount of the methanol, and the cost of production is greatly saved.
Description
Technical field
The present invention relates to a kind of extraction process, be specifically related to a kind of extraction process of Avrmectin, belong to biological pesticide technical field.
Background technology
Avrmectin (Avermectin), is a kind of macrolide antibiotics produced by A Foman streptomycete fermentation, has very strong insecticidal activity, is widely used as Insecticidal and acaricidal agent agricultural or for animals and uses.It is wide that it has insecticidal spectrum, has very strong insecticidal activity to nearly all insect and acarid and zooparasite; Meanwhile, this Avrmectin is easily degraded in soil and water, also remains without accumulation and persistence in vivo, does not pollute the environment.Therefore development prospect great potential.
In current Avrmectin production technique, after sheet frame crossed by fermented liquid, dry mycelium with flash dryer, and then with 80-100 doubly in mycelium the methyl alcohol of B1a weight go to soak, alcohol extracting 3-6 hour and constantly stir.Then filter out leaching liquid and be condensed into paste work in-process, be then warming up to 70 DEG C of dissolvings by 3 times of volumes methanol to the weight of paste work in-process B1a, be then down to normal temperature crystallization and go out Avrmectin crude product; Periodic crystallisation obtains finished product 2 times afterwards.What be different from knot crude product is carry out desolventing technology with the gac needing to add crystal weight 3%-5% during dissolve with methanol crystal twice afterwards.Use the object of flash distillation machine to be reduce the moisture in mycelium, prevent because the too high concentration of solvent methyl alcohol that causes of water content reduces, thus impact leaching effect.But because the air after flash distillation machine uses heating is dried, carry out fragmentation by stirring to mycelium, powder will be caused to contact with high temperature air, easily cause dust explosion, the safety coefficient of production is low simultaneously.In addition, the high-temperature gas of drying after mycelium enters in air through fly-ash separator, owing to can not effectively remove peculiar smell and minute dusts, and may to environment.Secondly, the energy consumption of flash distillation machine is very large, and the mycelium of every dry a ton consumes electricity about 180kwh; Steam is about 5t.Account for production cost 9.5 yuan/kg Avrmectin.In addition, also there is the problem such as alcohol extracting overlong time (being about 9 hours), methanol usage large (total amount is about mycelial 10-12 doubly) in this processing arrangement.
No. CN101362785B, Chinese patent discloses a kind of avermectin extraction technology, and this technique will use special purpose device lixiviate post, and needs methyl alcohol or ethanol to carry out the operations such as dynamic desorption, inflated with nitrogen, steam volatilization.Due to, relate to special purpose device lixiviate post, dynamic desorption, steam volatilization etc., the introducing due to steam makes the water content of methyl alcohol or ethanol increase.For satisfied use need, to methyl alcohol or ethanol rectifying yield, cause energy consumption to increase, and operation is also loaded down with trivial details.
In sum, find a kind ofly can abandon flash dryer, to shorten production time, new technique easy and simple to handle extremely urgent.
Summary of the invention
Technical problem to be solved by this invention be overcome prior art defect, a kind of avermectin extraction technology is provided, it is low, simple to operate that described avermectin extraction technology has cost, is suitable for the features such as suitability for industrialized production.
Technical problem of the present invention is solved by following technical scheme.
A kind of avermectin extraction technology, comprises the steps:
A, wet mycelium after filtering fermentation liquor, add toluene, opens stirring and leach;
B, in leaching process, to heat up under vacuum, and keep 30min.
C, be down to normal temperature and filter, leaching liquid concentrates, crystallization.
D, distillate composition toluene and collect through condensation, after leaving standstill, reuse after discharging a small amount of water in bottom.
Above-mentioned avermectin extraction technology, in described steps A, the amount adding toluene in wet mycelium is 3.5 times of wet mycelium.
Above-mentioned avermectin extraction technology, in described step B, leaching condition is: under-0.04MPA vacuum tightness, be warming up to material boiling until 94 DEG C time, and maintain 30min.
Above-mentioned avermectin extraction technology, in described step C, cools to normal temperature by the B material leached and filters; The mycelium the leached toluene of 3.5 times washs, and washings carries out next batch leaching.
Filter the leaching liquid obtained to distill, obtain ointment and carry out crystallization, through the complete conformance with standard requirement of quality product obtained according to original crystallization processes.
Above-mentioned avermectin extraction technology, in described step D, by the gas steamed in step B and C, condensation is collected, and time of repose is 3h, makes toluene and the abundant layering of water, and discharge the water of bottom, toluene is reused.
The avermectin extraction technology that the present invention proposes, volume of toluene m3 and wet mycelium weight kg are than being 3.5:1, under 0.04MPA vacuum tightness, open stirring be warming up to material azeotropic, until 94 DEG C time, maintain 30min, object is to make water in toluene and wet mycelium form azeotropic, steaming toluene and take away moisture in mycelium simultaneously, is the boiling point of toluene when vacuum tightness is-0.04MPA when temperature reaches 94 DEG C, i.e. moisture Ex-all in mycelium.The gas that simultaneously condensation steams, after condensation is collected, utilize toluene immiscible with water and proportion differs larger character, carry out natural layering, the water of discharge lower floor, upper toluene can reuse.
Avermectin extraction technology of the present invention has following remarkable advantage: (1) eliminates flash dryer, and protection of the environment also saves a large amount of electric energy and the consumption of steam; (2) toluene divides with moisture azeotropic removal of water in mycelium as leaching agent intensification, replace flash dryer to dewater, and the toluene energy condensation of evaporating together with water is reclaimed, recycling; (3) the toluene intensification leaching wet mycelium time is compared methyl alcohol leaching and will save 11 ~ 20 hours, greatly reduces the production time.(4) decrease methanol rectifying system, greatly reduce energy consumption of rectification and environmental risk factors.(5) make the usage quantity of workshop hazardous substance decrease 8 times, greatly reduce the harm of security risk and occupational health health.
Accompanying drawing explanation
Fig. 1 is the Avermectin B1a finished product chromatograms that embodiment 1 obtains;
Fig. 2 is the Avermectin B1a finished product chromatograms that embodiment 2 obtains;
Fig. 3 is the Avermectin B1a finished product chromatograms that embodiment 3 obtains.
Embodiment
Below by specific embodiment, the present invention is described in further detail, but these embodiments are only used for explaining the present invention, do not really want to limit the protection domain of embodiments of the present invention or patent.
Embodiment 1
A, get the wet mycelium 1000kg after Plate Filtration, B1a content is 8%.With the toluene of 3500L, carry out stirring leaching.
B, by toluene and mycelium mixing solutions when vacuum tightness is-0.04mpa, be warming up to 94 DEG C and maintain 30min.The condensation of gas steamed collected, collect 580L altogether, lower layer of water is 221L, toluene 359L altogether.Then toluene and mycelium mixing solutions are cooled to normal temperature, filter out mycelium, obtain filtrate 3020L, tire as 24159ug/ml.
C, the mycelium leached by steps A and step B repetition leaching step B with 3500L toluene; Vapor condensation collects 413L altogether, is toluene entirely.Filtrate be 3064L its tire as 1410ug/ml.
D, the mycelium leached by steps A and step B repetition leaching step C with 3500L toluene; Vapor condensation collects 376L altogether, is toluene entirely.Filtrate be 3114L its tire as 565ug/ml.
E, the filtrate obtained to be merged concentrated obtain paste work in-process in step B, C, D, toluene condensation is reclaimed, and collects 9103L altogether.Then carry out crystallization by original technique, finally go out finished product 67.8kg, its B1a purity is 97.9%, and mother liquor altogether 797.3kg, B1a content is 1.5%; Mother liquor is 918L altogether, tires as 13028ug/ml finished product and mother liquor total recovery are 97.8%
In this example, toluene leaching liquid yield is 99.8%; Toluene recovery rate is 98.2%; Finished product B1a purity is 97.9%, and finished product and mother liquor total recovery are 97.8%
Embodiment 2
A, get the wet mycelium 1000kg after Plate Filtration, B1a content is 7.7%.With the toluene of 3500L, carry out stirring leaching.
B, by toluene and mycelium mixing solutions when vacuum tightness is-0.04mpa, be warming up to 94 DEG C and maintain 30min.The condensation of gas steamed collected, collect 673L altogether, lower layer of water is 308L, toluene 365L altogether.Then toluene and mycelium mixing solutions are cooled to normal temperature, filter out mycelium, obtain filtrate 3002L, tire as 23290ug/ml.
C, the mycelium leached by steps A and step B repetition leaching step B with 3500L toluene; Vapor condensation collects 378L altogether, is toluene entirely.Filtrate be 3081L its tire as 1400ug/ml.
D, the mycelium leached by steps A and step B repetition leaching step C with 3500L toluene; Vapor condensation collects 363L altogether, is toluene entirely.Filtrate be 3098L its tire as 795ug/ml.
E, the filtrate obtained to be merged concentrated obtain paste work in-process in step B, C, D, toluene condensation is reclaimed, and collects 9083L altogether.Then carry out crystallization by original technique, finally go out finished product 65.4kg, its B1a purity is 97.6%, and mother liquor altogether 745kg, B1a content is 1.5%; Mother liquor is 885L altogether, tires as 12627ug/ml finished product and mother liquor total recovery are 97.4%
In this example, toluene leaching liquid yield is 99.6%; Toluene recovery rate is 97%; Finished product B1a purity is 97.9%, and finished product and mother liquor total recovery are 97.8%
Embodiment 3
A, get the wet mycelium 1000kg after Plate Filtration, B1a content is 8.1%.With the toluene of 3500L, carry out stirring leaching.
B, by toluene and mycelium mixing solutions when vacuum tightness is-0.04mpa, be warming up to 94 DEG C and maintain 30min.The condensation of gas steamed collected, collect 571L altogether, lower layer of water is 216L, toluene 355L altogether.Then toluene and mycelium mixing solutions are cooled to normal temperature, filter out mycelium, obtain filtrate 3019L, tire as 24550ug/ml.
C, the mycelium leached by steps A and step B repetition leaching step B with 3500L toluene; Vapor condensation collects 352L altogether, is toluene entirely.Filtrate be 3107L its tire as 1330ug/ml.
D, the mycelium leached by steps A and step B repetition leaching step C with 3500L toluene; Vapor condensation collects 385L altogether, is toluene entirely.Filtrate be 3068L its tire as 766ug/ml.
E, the filtrate obtained to be merged concentrated obtain paste work in-process in step B, C, D, toluene condensation is reclaimed, and collects 9106L altogether.Then carry out crystallization by original technique, finally go out finished product 70.9kg, its B1a purity is 97.8%, and mother liquor altogether 743kg, B1a content is 1.3%; Mother liquor is 947L altogether, tires as 10200ug/ml; Finished product and mother liquor total recovery are 97.5%
In this example, toluene leaching liquid yield is 99.5%; Toluene recovery rate is 97.1%; Finished product B1a purity is 97.8%, and finished product and mother liquor total recovery are 97.5%.
Below be only the preferred embodiments of the present invention, to those skilled in the art, under the premise without departing from the principles of the invention, the improvement that can make, modification, equivalent replacement etc., all should be included within protection scope of the present invention.
Claims (5)
1. an avermectin extraction technology, is characterized in that, comprises the steps:
A, wet mycelium after filtering fermentation liquor, add toluene, opens stirring and leach;
B, in leaching process, to heat up under vacuum, and keep 30min.
C, be down to normal temperature and filter, leaching liquid concentrates, crystallization.
D, distillate composition toluene and collect through condensation, after leaving standstill, reuse after discharging a small amount of water in bottom.
2. avermectin extraction technology according to claim 1, is characterized in that, in described steps A, the amount adding toluene in wet mycelium is 3.5 times of wet mycelium.
3. avermectin extraction technology according to claim 2, is characterized in that, in described step B, leaching condition is: under-0.04MPA vacuum tightness, be warming up to material boiling until 94 DEG C time, and maintain 30min.
4. avermectin extraction technology according to claim 3, is characterized in that, in described step C, the B material leached is cooled to normal temperature and filters; The mycelium the leached toluene of 3.5 times washs, and washings carries out next batch leaching.
5. avermectin extraction technology according to claim 4, is characterized in that, in described step D, by the gas steamed in step C, condensation is collected, and by leaving standstill, makes toluene and the abundant layering of water, and discharge the water of bottom, toluene is reused.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510791079.9A CN105503982A (en) | 2015-11-17 | 2015-11-17 | Abamectin extraction process |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510791079.9A CN105503982A (en) | 2015-11-17 | 2015-11-17 | Abamectin extraction process |
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| CN105503982A true CN105503982A (en) | 2016-04-20 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201510791079.9A Pending CN105503982A (en) | 2015-11-17 | 2015-11-17 | Abamectin extraction process |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN108440621A (en) * | 2018-04-19 | 2018-08-24 | 齐鲁制药（内蒙古）有限公司 | A kind of process for refining and purifying of avermectin |
| CN108489196A (en) * | 2018-03-30 | 2018-09-04 | 内蒙古拜克生物有限公司 | A kind of avermectin crystal drying means |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0082674A2 (en) * | 1981-12-21 | 1983-06-29 | Merck & Co. Inc. | Process for the whole broth extraction of avermectin |
| CN1281900A (en) * | 2000-07-25 | 2001-01-31 | 高东卫 | Extraction method of abamectin |
| CN1800035A (en) * | 2005-12-21 | 2006-07-12 | 史立皂 | Avermectin-containing waste liquor recovery process |
| CN1923840A (en) * | 2006-09-27 | 2007-03-07 | 河北瑞通美邦工程有限公司 | Extraction technology of avermectin |
-
2015
- 2015-11-17 CN CN201510791079.9A patent/CN105503982A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0082674A2 (en) * | 1981-12-21 | 1983-06-29 | Merck & Co. Inc. | Process for the whole broth extraction of avermectin |
| CN1281900A (en) * | 2000-07-25 | 2001-01-31 | 高东卫 | Extraction method of abamectin |
| CN1800035A (en) * | 2005-12-21 | 2006-07-12 | 史立皂 | Avermectin-containing waste liquor recovery process |
| CN1923840A (en) * | 2006-09-27 | 2007-03-07 | 河北瑞通美邦工程有限公司 | Extraction technology of avermectin |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN106478369B (en) * | 2016-08-30 | 2019-09-03 | 齐鲁制药（内蒙古）有限公司 | A kind of the low energy consumption recovery system and technique of avermectin Extraction solvent |
| CN108489196A (en) * | 2018-03-30 | 2018-09-04 | 内蒙古拜克生物有限公司 | A kind of avermectin crystal drying means |
| CN108440621A (en) * | 2018-04-19 | 2018-08-24 | 齐鲁制药（内蒙古）有限公司 | A kind of process for refining and purifying of avermectin |
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Application publication date: 20160420 |
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