CN110240622A - It is a kind of produce during avermectin without benzene desugar technique - Google Patents
It is a kind of produce during avermectin without benzene desugar technique Download PDFInfo
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- CN110240622A CN110240622A CN201910488132.6A CN201910488132A CN110240622A CN 110240622 A CN110240622 A CN 110240622A CN 201910488132 A CN201910488132 A CN 201910488132A CN 110240622 A CN110240622 A CN 110240622A
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- avermectin
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- grain
- benzene
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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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- 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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- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- Biotechnology (AREA)
- General Health & Medical Sciences (AREA)
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- Molecular Biology (AREA)
- Saccharide Compounds (AREA)
- Heterocyclic Carbon Compounds Containing A Hetero Ring Having Oxygen Or Sulfur (AREA)
Abstract
The invention discloses it is a kind of produce during avermectin without benzene desugar technique, including avermectin leaching liquid reduction vaporization desolventizing is obtained concentrate, the extraction of the first stirring solvent is added, stand removal upper phase and newborn phase, the heating of the second solvent is added, stirring is transferred to crystallizing tank decrease temperature crystalline, recrystallization and drying and other steps.The present invention eliminates toluene desugar process compared with traditional avermectin proposes alcohol technique, not only reduces cost for purification, has also evaded harm of the toluene to employee and environmental operations in purification process.
Description
Technical field
The present invention relates to avermectin production technical field, in particular to it is a kind of produce it is de- without benzene during avermectin
Sugared technique.
Background technique
Avermectin is ten similar hexa-atomic macrolide antibiotics of one group of structure, has very strong insecticidal activity, is made
For insecticide, it can kill almost all of Nemata, insects and acarid class, and disposable medication can reach 80~100%
Drive use up rate, and it is to the highly-safe of people and mammal, is a kind of good biological pesticide.Currently, avermectin
Desugar technique is usually that toluene is used to carry out organic extraction.This method is slow there are organic phase and inorganic phase layering and layering is difficult, has
Interface, water layer viscosity is big, and the residual quantity of toluene and effective component is high in water layer, and yield is low, and wastewater treatment is difficult, environmental pollution
The problems such as serious.
Summary of the invention
The technical problem to be solved in the present invention is to provide it is a kind of produce during avermectin without benzene desugar technique.
In order to solve the above-mentioned technical problem, the technical solution of the present invention is as follows:
It is a kind of produce during avermectin without benzene desugar technique, include the following steps:
(a) avermectin leaching liquid reduction vaporization desolventizing is obtained into concentrate, the first solvent is added and is warming up to 80-85 DEG C
45-60min is stirred, makes the concentrate and the first solvent be sufficiently mixed to obtain the first mixture, wherein first solvent
Additional amount and the volume ratio of concentrate are 3.0-3.5:1；
(b) first mixture is stood into 1-2h, removes upper phase and newborn phase, obtain containing avermectin effectively at
The first dope divided；
(c) the second solvent is added in first dope and is warming up to 60-65 DEG C, stirs 30-45min, is transferred to crystallization
Tank decrease temperature crystalline, recirculated water water-bath are cooled to 20 DEG C, maintain 1-2h, and the closed centrifugation of centrifuge obtains coarse-grain of avermectin；
(d) coarse-grain of the avermectin is recrystallized: is added second in coarse-grain of Xiang Suoshu avermectin
Solvent, the active carbon for adding coarse-grain quality 2-3% of the avermectin are warming up to 60-65 DEG C, stir 30-45min, secretly
Flow through filter, filtrate decrease temperature crystalline, wherein coarse-grain weight ratio of second solvent and avermectin is 7-8:1, and temperature is down to
20 DEG C, 1-2h is maintained, obtains avermectin fine powder after centrifugation, drying.
Preferably, the drying temperature control in the step (d) are as follows: room temperature dries 30min, 110-120 DEG C of drying 90-
120min。
Preferably, first solvent is the aqueous solution for the use of sulphur acid for adjusting pH being 6.0, and second solvent is ethyl alcohol.
By adopting the above technical scheme, the present invention eliminates toluene desugar process compared with traditional avermectin proposes alcohol technique,
Cost for purification is not only reduced, harm of the toluene to employee and environmental operations in purification process has also been evaded, is added and uses sulfuric acid
Effective desugar effect can be played by adjusting the aqueous solution that pH is 6.0, and avermectin can be effectively prevent under acidic environment
Degradation improves avermectin yield；Use ethyl alcohol as recrystallisation solvent, more environmentally friendly and crystallization effect is good, so that this hair
Bright is environmental friendly nontoxic without benzene desugar.
Specific embodiment
Specific embodiments of the present invention will be further explained below.It should be noted that for these implementations
The explanation of mode is used to help understand the present invention, but and does not constitute a limitation of the invention.In addition, invention described below
Technical characteristic involved in each embodiment can be combined with each other as long as they do not conflict with each other.
Embodiment 1
It is a kind of produce during avermectin without benzene desugar technique, include the following steps:
(a) avermectin leaching liquid reduction vaporization desolventizing is obtained into concentrate, the first solvent of addition is warming up to 83 DEG C and stirs
50min is mixed, the concentrate and the first solvent is made to be sufficiently mixed to obtain the first mixture, wherein the addition of first solvent
Amount and the volume ratio of concentrate are 3.3:1；First solvent can be selected but be not limited to the solvent without toluene: being added to have makes
The aqueous solution for being 6.0 with sulphur acid for adjusting pH；
(b) first mixture is stood into 1.5h, removes upper phase and newborn phase, obtain containing avermectin effectively at
The first dope divided；
(c) the second solvent is added in first dope and is warming up to 63 DEG C, stirs 40min, is transferred to crystallizing tank cooling
Crystallization, recirculated water water-bath are cooled to 20 DEG C, maintain 1.5h, and the closed centrifugation of centrifuge obtains coarse-grain of avermectin；Described
Two solvents can be selected but be not limited to ethyl alcohol；
(d) coarse-grain of the avermectin is recrystallized: is added second in coarse-grain of Xiang Suoshu avermectin
Solvent, the active carbon for adding coarse-grain quality 2.5% of avermectin are warming up to 63 DEG C, stir 40min, undercurrent mistake
Filter, filtrate decrease temperature crystalline, wherein coarse-grain weight ratio of second solvent and avermectin is 7.5:1, and temperature is down to 20
DEG C, 1.5h is maintained, obtains avermectin fine powder after centrifugation, drying；Drying temperature control are as follows: room temperature dries 30min, and 115
DEG C drying 115min.
Embodiment 2
It is a kind of produce during avermectin without benzene desugar technique, include the following steps:
(a) avermectin leaching liquid reduction vaporization desolventizing is obtained into concentrate, the first solvent of addition is warming up to 80 DEG C and stirs
45min is mixed, the concentrate and the first solvent is made to be sufficiently mixed to obtain the first mixture, wherein the addition of first solvent
Amount and the volume ratio of concentrate are 3.0:1；First solvent can be selected but be not limited to the solvent without toluene: being added to have makes
The aqueous solution for being 6.0 with sulphur acid for adjusting pH；
(b) first mixture is stood into 1h, removes upper phase and newborn phase, obtains containing avermectin effective component
The first dope；
(c) the second solvent is added in first dope and is warming up to 60 DEG C, stirs 30min, is transferred to crystallizing tank cooling
Crystallization, recirculated water water-bath are cooled to 20 DEG C, maintain 1h, and the closed centrifugation of centrifuge obtains coarse-grain of avermectin；Described second
Solvent can be selected but be not limited to ethyl alcohol；
(d) coarse-grain of the avermectin is recrystallized: is added second in coarse-grain of Xiang Suoshu avermectin
Solvent, the active carbon for adding coarse-grain quality 2% of avermectin are warming up to 60 DEG C, stir 30min, and undercurrent filters,
Filtrate decrease temperature crystalline, wherein coarse-grain weight ratio of second solvent and avermectin is 7:1, and temperature is down to 20 DEG C, is maintained
1h obtains avermectin fine powder after centrifugation, drying；The drying temperature control are as follows: room temperature dries 30min, 110 DEG C of drying
90min。
Embodiment 3
It is a kind of produce during avermectin without benzene desugar technique, include the following steps:
(a) avermectin leaching liquid reduction vaporization desolventizing is obtained into concentrate, the first solvent of addition is warming up to 85 DEG C and stirs
60min is mixed, the concentrate and the first solvent is made to be sufficiently mixed to obtain the first mixture, wherein the addition of first solvent
Amount and the volume ratio of concentrate are 3.5:1；First solvent can be selected but be not limited to the solvent without toluene: being added to have makes
The aqueous solution for being 6.0 with sulphur acid for adjusting pH；
(b) first mixture is stood into 2h, removes upper phase and newborn phase, obtains containing avermectin effective component
The first dope；
(c) the second solvent is added in first dope and is warming up to 65 DEG C, stirs 45min, is transferred to crystallizing tank cooling
Crystallization, recirculated water water-bath are cooled to 20 DEG C, maintain 2h, and the closed centrifugation of centrifuge obtains coarse-grain of avermectin；Described second
Solvent can be selected but be not limited to ethyl alcohol；
(d) coarse-grain of the avermectin is recrystallized: is added second in coarse-grain of Xiang Suoshu avermectin
Solvent, the active carbon for adding coarse-grain quality 3% of avermectin are warming up to 65 DEG C, stir 45min, and undercurrent filters,
Filtrate decrease temperature crystalline, wherein coarse-grain weight ratio of second solvent and avermectin is 8:1, and temperature is down to 20 DEG C, is maintained
2h obtains avermectin fine powder after centrifugation, drying；The drying temperature control are as follows: room temperature dries 30min, 120 DEG C of drying
120min。
The present invention eliminates toluene desugar process, not only reduces and be purified to compared with traditional avermectin proposes alcohol technique
This, has also evaded harm of the toluene to employee and environmental operations in purification process, be added using sulphur acid for adjusting pH be 6.0 it is water-soluble
Liquid can play effective desugar effect, and the degradation of avermectin can be effectively prevent under acidic environment, improve avermectin
Yield；Use ethyl alcohol as recrystallisation solvent, more environmentally friendly and crystallization effect is good, so that no benzene desugar technique ring of the invention
It protects nontoxic.
Above the embodiments of the present invention are described in detail, but the present invention is not limited to described embodiments.It is right
For those skilled in the art, in the case where not departing from the principle of the invention and spirit, these embodiments are carried out more
Kind change, modification, replacement and modification, still fall in protection scope of the present invention.
Claims (3)
1. it is a kind of produce during avermectin without benzene desugar technique, characterized by the following steps:
(a) avermectin leaching liquid reduction vaporization desolventizing is obtained into concentrate, the first solvent is added and is warming up to 80-85 DEG C of stirring
45-60min makes the concentrate and the first solvent be sufficiently mixed to obtain the first mixture, wherein the addition of first solvent
Amount and the volume ratio of concentrate are 3.0-3.5:1；
(b) first mixture is stood into 1-2h, removes upper phase and newborn phase, obtains containing avermectin effective component
First dope；
(c) the second solvent is added in first dope and is warming up to 60-65 DEG C, stirs 30-45min, is transferred to crystallizing tank drop
Temperature crystallization, recirculated water water-bath are cooled to 20 DEG C, maintain 1-2h, and the closed centrifugation of centrifuge obtains coarse-grain of avermectin；
(d) coarse-grain of the avermectin is recrystallized: the second solvent is added in coarse-grain of Xiang Suoshu avermectin,
The active carbon for adding coarse-grain quality 2-3% of the avermectin is warming up to 60-65 DEG C, stirs 30-45min, undercurrent mistake
Filter, filtrate decrease temperature crystalline, wherein coarse-grain weight ratio of second solvent and avermectin is 7-8:1, and temperature is down to 20
DEG C, 1-2h is maintained, obtains avermectin fine powder after centrifugation, drying.
2. it is according to claim 1 production avermectin during without benzene desugar technique, it is characterised in that: the step
(d) the drying temperature control in are as follows: room temperature dries 30min, 110-120 DEG C of drying 90-120min.
3. it is according to claim 1 production avermectin during without benzene desugar technique, it is characterised in that: described first
Solvent is the aqueous solution for the use of sulphur acid for adjusting pH being 6.0, and second solvent is ethyl alcohol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910488132.6A CN110240622A (en) | 2019-06-05 | 2019-06-05 | It is a kind of produce during avermectin without benzene desugar technique |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910488132.6A CN110240622A (en) | 2019-06-05 | 2019-06-05 | It is a kind of produce during avermectin without benzene desugar technique |
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| CN110240622A true CN110240622A (en) | 2019-09-17 |
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| CN201910488132.6A Pending CN110240622A (en) | 2019-06-05 | 2019-06-05 | It is a kind of produce during avermectin without benzene desugar technique |
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Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1800035A (en) * | 2005-12-21 | 2006-07-12 | 史立皂 | Avermectin-containing waste liquor recovery process |
| CN102060895A (en) * | 2011-01-07 | 2011-05-18 | 石家庄市兴柏生物工程有限公司 | Method for desugaring abamectin |
| CN102617668A (en) * | 2012-02-29 | 2012-08-01 | 大庆志飞生物化工有限公司 | Production process of high-purity abamectin fine powder |
| CN102977168A (en) * | 2012-12-17 | 2013-03-20 | 石家庄市兴柏生物工程有限公司 | Extraction and preparation method of abamectin B2a |
| CN103030676A (en) * | 2012-11-19 | 2013-04-10 | 河北威远生物化工股份有限公司 | Process for extracting component B1 and component B2 of abamectin step by step by using crystallization process |
| CN103613624A (en) * | 2013-12-05 | 2014-03-05 | 宁夏启元药业有限公司 | Refining method of avermectin |
| CN104650167A (en) * | 2015-03-10 | 2015-05-27 | 齐鲁制药（内蒙古）有限公司 | Preparation method of high-purity abamectin B2a |
| CN106977566A (en) * | 2017-04-20 | 2017-07-25 | 河北科技大学 | A kind of method that Avermectin B2 is extracted from abamectin ointment |
| CN107787963A (en) * | 2017-07-03 | 2018-03-13 | 齐鲁制药（内蒙古）有限公司 | A kind of preparation method of anti-caking AVM toluene ointment |
-
2019
- 2019-06-05 CN CN201910488132.6A patent/CN110240622A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1800035A (en) * | 2005-12-21 | 2006-07-12 | 史立皂 | Avermectin-containing waste liquor recovery process |
| CN102060895A (en) * | 2011-01-07 | 2011-05-18 | 石家庄市兴柏生物工程有限公司 | Method for desugaring abamectin |
| CN102617668A (en) * | 2012-02-29 | 2012-08-01 | 大庆志飞生物化工有限公司 | Production process of high-purity abamectin fine powder |
| CN103030676A (en) * | 2012-11-19 | 2013-04-10 | 河北威远生物化工股份有限公司 | Process for extracting component B1 and component B2 of abamectin step by step by using crystallization process |
| CN102977168A (en) * | 2012-12-17 | 2013-03-20 | 石家庄市兴柏生物工程有限公司 | Extraction and preparation method of abamectin B2a |
| CN103613624A (en) * | 2013-12-05 | 2014-03-05 | 宁夏启元药业有限公司 | Refining method of avermectin |
| CN104650167A (en) * | 2015-03-10 | 2015-05-27 | 齐鲁制药（内蒙古）有限公司 | Preparation method of high-purity abamectin B2a |
| CN106977566A (en) * | 2017-04-20 | 2017-07-25 | 河北科技大学 | A kind of method that Avermectin B2 is extracted from abamectin ointment |
| CN107787963A (en) * | 2017-07-03 | 2018-03-13 | 齐鲁制药（内蒙古）有限公司 | A kind of preparation method of anti-caking AVM toluene ointment |
Non-Patent Citations (1)
| Title |
|---|
| 孙富伟: "阿维菌素后处理工艺优化", 《中国优秀博硕士学位论文全文数据库(硕士)-工程科技Ⅰ辑》 * |
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Application publication date: 20190917 |
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