CN105461771B - Emamectin benzoate preparation system - Google Patents
Emamectin benzoate preparation system Download PDFInfo
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- CN105461771B CN105461771B CN201511022640.3A CN201511022640A CN105461771B CN 105461771 B CN105461771 B CN 105461771B CN 201511022640 A CN201511022640 A CN 201511022640A CN 105461771 B CN105461771 B CN 105461771B
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- kettle
- preparation system
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- emamectin benzoate
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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
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- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- Biotechnology (AREA)
- General Health & Medical Sciences (AREA)
- Genetics & Genomics (AREA)
- Molecular Biology (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The invention discloses a kind of emamectin benzoate preparation systems comprising stoste preparation system and drying system, stoste preparation system include the dilution dissolution kettle for passing sequentially through pipeline connection, distillation still, stills for air blowing, amination kettle, adjust sour kettle, concentration kettle；Drying system includes airstream drying tower and more than one cyclone separator.Advantage: structure is simple, simplifies production craft step, improves production efficiency；Entire preparation system is totally-enclosed production system, can prevent solvent from evaporateing into atmosphere, avoids environmental pollution, improves raw material availability, reduces production cost, improves earning rate to 90% or more；Dry powder blender can stir evenly emamectin benzoate powder, keep emamectin benzoate product quality uniform, guarantee product quality；Methane in dry condensation fluid reservoir can be pumped directly into dilution dissolution kettle by circulating pump, can be recycled the methane of recycling.
Description
Technical field:
The present invention relates to emamectin benzoate preparation technical fields, relate in particular to a kind of emamectin benzoate preparation system.
Background technique:
Emamectin benzoate full name is emamectin-benzoate, is the one kind synthesized since fermented product avermectin
New and effective semisynthetic antibiotics insecticide, it has the characteristics that the biological pesticides such as ultra high efficiency, low toxicity, low-residual, nuisanceless；Extensively
The prevention and treatment of the general various pests on the crops such as vegetables, fruit tree, cotton.Currently, the preparation of emamectin benzoate need methane is molten
Liquid, avermectin and oxidant carry out dissolution oxidation in stills for air blowing, and then, the solution after oxidation reaction is imported in washing kettle,
After stirring the impurity that removal oxidation reaction generates with phosphate aqueous solution, net system is precipitated 2 hours, and the organic solution after net system precipitating is led
Enter another washing kettle and react adjusting pH value with ice acid, then net system precipitates 2 hours, the organic solution after net system precipitating 2 imports
Drying equipment is simultaneously added desiccant and is removed water, and the organic solution after water removal imports amination kettle and aminating agent carries out aminating reaction,
Organic solution after aminating reaction imports washing kettle and adjusts pH value and carry out 2 washings, stands 2 hours after washing every time, water
Organic solution after washing imports concentration kettle and carries out being condensed into salt, and the solvent after being condensed into salt enters drying equipment and is dried, raw
At powdered finished product.It has the disadvantage that (1) leads that kettle step is more, and the production cycle is at 70 more than hour；(2) using chemistry
The mode of reaction removes the impurity of oxidation reaction generation, and acid-base accommodation preparation usage amount is big, and the impurity such as desiccant are contained in product,
Cause earning rate 80% or so；(3) when drying equipment is removed water, solvent evaporation is evaporate into air, causes environment dirty
Dye, while raw material are wasted, production cost is improved, earning rate is reduced；(4) organic solution is when concentration kettle carries out being condensed into salt,
The methane gas of generation is directly disposed as byproduct, is not made full use of, and production cost is increased；(5) after being condensed into salt
Solvent seasoning generate powdered finished product when, solvent is in line into air with hot wind, causes environmental pollution, while wasting former material
Material improves production cost, reduces earning rate；(6) when the solvent after being condensed into salt is dried in drying equipment, because of drying equipment
Thermal condition variation, cause in powdered finished product that emamectin benzoate content is inconsistent, influence product quality.
Summary of the invention:
The emamectin benzoate preparation system that the purpose of the present invention is to provide one kind can simplify production technology, improves earning rate.
The present invention is implemented by following technical solution: emamectin benzoate preparation system comprising stoste preparation system and drying system,
The stoste preparation system include the dilution dissolution kettle for passing sequentially through pipeline connection, distillation still, stills for air blowing, amination kettle, adjust sour kettle,
Concentration kettle, the oxidant storage tank being connected to the stills for air blowing, the aminating agent storage tank being connected to the amination kettle, with the sour kettle of the tune
The acid-base modifier storage tank of connection, the benzoic acid feed bin being connected to the concentration kettle；The drying system includes airstream drying tower
With more than one cyclone separator, the feed inlet of the airstream drying tower is connected with the discharge port of the concentration kettle；The gas
The discharge port of stream drying tower is connected with the feed inlet of the cyclone separator.
The stoste preparation system further includes distiller condenser, is distilled to recover tank, sets on the gas outlet of the distillation still
There is the distiller condenser, the water outlet of the distiller condenser is connected with the feed inlet for being distilled to recover tank, the distillation
Recycling can is connected with the inlet of the dilution dissolution kettle by water pump.
The stoste preparation system further includes concentration condenser, and concentration and recovery tank is set on the gas outlet of the concentration kettle
There is the concentration condenser, the water outlet of the concentration condenser is connected with the feed inlet of the concentration and recovery tank, the concentration
Recycling can is connected with the inlet of the dilution dissolution kettle by water pump.
The stoste preparation system further includes filter plant, and the pipeline between the stills for air blowing and the amination kettle is equipped with
The filter plant, the filter plant are any one of centrifuge or filtering tank.
The filtering tank includes hollow tank body, and at the tank body both ends, fission is movably equipped with top cover and conical bottom respectively
Lid is equipped with feed inlet on the top cover, is equipped with orifice plate between the tank body and the conical bottom cover, the orifice plate with
It is equipped with strainer between the tank body, covers in the conical bottom equipped with discharge port and anti-blowpipe.
More than one lengthening tank body is equipped between the tank body and the top cover.
It is equipped on the tank wall and is arranged equipped with heating tube or heat exchanger tube.
Being equipped at least three pieces on the inner wall of the distillation still, the stills for air blowing, the amination kettle and the concentration kettle is in
The spiral deflector of helical form setting.
The distillation still, the stills for air blowing, the amination kettle and the concentration kettle agitating shaft on be equipped with into reversed rotation
The upper layer and lower layer stirring blade of stream.
Spray head is equipped on the nozzle for adjusting the regulating acid agent feed pipe in sour kettle.
The drying system further includes air delivery tube and dry powder blender, and the discharge port of the cyclone separator passes through institute
Air delivery tube is stated to be connected to the feed inlet of the dry powder blender.
The dry powder blender is any one of Agravicmixer or conical mixer.
The drying system further includes dry condenser and dry condensation fluid reservoir, the air inlet of the dry condenser with
The gas outlet of the cyclone separator is connected to, and the liquid outlet of the dry condenser is connected to the dry condensation fluid reservoir.
The dry condensation fluid reservoir is connected to the concentration kettle by circulating pump.
Advantages of the present invention: structure is simple, simplifies production craft step, and the production cycle reduces by more than half, and improves
Production efficiency；The methane liquid that concentration kettle generates can be recycled by concentration condenser, avoid wasting；Entire preparation system
System is totally-enclosed production system, can prevent solvent from evaporateing into atmosphere, avoids environmental pollution, improves raw material availability, is reduced
Production cost improves earning rate to 90% or more；The emamectin benzoate powder that drying tower is discharged is sent to dry powder using cyclone separator
Mixing machine, dry powder blender can stir evenly emamectin benzoate powder, keep emamectin benzoate product quality uniform, guarantee product quality；Benefit
The methane solvent carried in air-flow that cyclone separator generates is recycled with dry condenser, avoids environmental pollution,
Raw material availability is improved, production cost is reduced, improves earning rate；Circulating pump can directly pump the methane in dry condensation fluid reservoir
Enter to dilution dissolution kettle, the methane of recycling can be recycled.
Detailed description of the invention:
Fig. 1 is overall structure diagram of the invention.
Fig. 2 is the overall structure diagram of filtering tank.
Fig. 3 be distillation still, stills for air blowing, amination kettle and concentration kettle structural schematic diagram.
Fig. 4 is the structural schematic diagram for adjusting sour kettle.
It dilutes dissolution kettle 1, distillation still 2, stills for air blowing 3, amination kettle 4, adjust sour kettle 5, concentration kettle 6, oxidant storage tank 7, amination
Agent storage tank 8, distiller condenser 10, is distilled to recover tank 11, water pump 12, concentration condenser 13, is concentrated back acid-base modifier storage tank 9
Closed cans 14, filtering tank 15, stirring blade 16, spray head 17, spiral deflector 18, benzoic acid feed bin 19, airstream drying tower 21, rotation
Wind separator 22, air delivery tube 23, dry powder blender 24, dry condenser 25, dry condensation fluid reservoir 26, circulating pump 27,
Tank body 31, feed inlet 33, frustum lumen type discharge port 34, orifice plate 35, strainer 36, anti-blowpipe 37, heat exchanger tube row 38, adds cover 32
Long tank body 39.
Specific embodiment:
Embodiment:
As shown in Figure 1, emamectin benzoate preparation system comprising stoste preparation system and drying system, stoste preparation system
System includes the dilution dissolution kettle 1 for passing sequentially through pipeline connection, distillation still 2, stills for air blowing 3, amination kettle 4, adjusts sour kettle 5, concentration kettle 6,
The oxidant storage tank 7 being connected to stills for air blowing 3, the aminating agent storage tank 8 being connected to amination kettle 4, with the acid-base accommodation for adjusting sour kettle 5 to be connected to
Agent storage tank 9, the benzoic acid feed bin 19 being connected to concentration kettle 6；Avermectin raw material, methane solvent is added into dilution dissolution kettle 1
And water, avermectin obtain abamectin solution in dilution dissolution kettle 1 after completely dissolution；Abamectin solution enters distillation still
Distillation goes moisture removal to obtain pure abamectin solution after 2；Abamectin solution and oxidant carry out aoxidizing in stills for air blowing 3 anti-
It should obtain oxidation product；Oxidation product and aminating agent carry out amination reduction reaction in amination kettle 4 and obtain the plain product of first dimension；First dimension
Plain product and acid-base modifier adjust sour kettle 5 adjust it is sour react, adjust the pH value that first ties up plain product；First ties up plain product and benzene
Formic acid generates emamectin benzoate after the concentration of concentration kettle 6；
The stoste preparation system further includes distiller condenser 10, is distilled to recover tank 11, is set on the gas outlet of distillation still 2
Have a distiller condenser 10, the water outlet of distiller condenser 10 is connected with the feed inlet for being distilled to recover tank 11, be distilled to recover tank 11 and
The inlet for diluting dissolution kettle 1 is connected by water pump 12；The avermectin liquid particles warp carried in the gas that distillation still 2 generates
Distiller condenser 10 enters distillation recovery tank 11 after forming avermectin liquid after condensing, and water pump 12 will be distilled to recover in tank 11
Avermectin liquid is pumped into dilution dissolution kettle 1 and continues to participate in reaction, avoids environmental pollution, improves the utilization of avermectin
Rate；
The stoste preparation system further includes concentration condenser 13, concentration and recovery tank 14, is set on the gas outlet of concentration kettle 6
Have concentration condenser 13, concentration condenser 13 water outlet be connected with the feed inlet of concentration and recovery tank 14, concentration and recovery tank 14 and
The inlet for diluting dissolution kettle 1 is connected by water pump 12；The methane liquid particle carried in the gas that concentration kettle 6 generates is concentrated
Condenser 13 enters concentration and recovery tank 14 after forming methane liquid after condensing, and water pump 12 is by the methane liquid in concentration and recovery tank 14
It is pumped into dilution dissolution kettle 1 and continues to participate in reaction, avoid environmental pollution；
The stoste preparation system further includes filter plant, and the pipeline between stills for air blowing 3 and amination kettle 4 is equipped with the mistake
Equipment is filtered, the filter plant is filtering tank 15, carries part organic salt, filtering tank in the oxidation product that stills for air blowing 3 generate
15 may filter that organic salt, prevent organic salt from entering the earning rate of the influence emamectin benzoate of amination kettle 4；
As shown in Fig. 2, filter tank 15 includes tank body 31, it is equipped with cover 32 at the top of tank body 31, charging is equipped on cover 32
Mouth 33；It is equipped with frustum lumen type discharge port 34 in 31 bottom of tank body, is equipped between 31 bottom of frustum lumen type discharge port 34 and tank body
Orifice plate 35 is equipped with strainer 36 between 31 bottom of orifice plate 35 and tank body；Anti-blowpipe is equipped on 34 side wall of frustum lumen type discharge port
37, anti-blowpipe 37 is connect with gas source by pipeline, when strainer 36 blocks, is dredged using gas；It is pushed up in tank body 31
A lengthening tank body 39 is equipped between portion and cover 32, the appearance liquid measure of tube body 31 can be increased by lengthening tank body 39；Outside tank body 31
Wall is equipped with heat exchanger tube row 38, and the temperature of heated oxide product guarantees being normally carried out for subsequent aminating reaction；
As shown in figure 3, being equipped with three pieces on the inner wall of distillation still 2, stills for air blowing 3, amination kettle 4 and concentration kettle 6 in the shape of a spiral
The spiral deflector 18 of setting；Spiral deflector 18 makes the liquid adjacent with each reaction kettle inner wall accelerate flowing, and then makes in kettle
Liquid is sufficiently mixed；Distillation still 2, stills for air blowing 3, amination kettle 4 and concentration kettle 6 agitating shaft be equipped at reversed eddy flow up and down two
Layer stirring blade 16, upper layer stirring blade 16 make the liquid in kettle form downward vortex, and lower layer's stirring blade 16 makes in kettle
Liquid forms upward vortex, and upper layer and lower layer stirring blade 16 can make the liquid in kettle accelerate mixing, improve stirring efficiency, together
When can be uniform by liquid agitation, enhance mixing effect；
As shown in figure 4, being equipped with spray head 17 on the nozzle for adjusting the regulating acid agent feed pipe in sour kettle 5, keep regulating acid agent uniform
The enhancing in the sour kettle 5 of tune that is sprayed at adjust sour effect.
The drying system includes airstream drying tower 21 and two cyclone separators 22, the feed inlet of airstream drying tower 21 with
The discharge port of concentration kettle 6 is connected；The discharge port of airstream drying tower 21 is connected with the feed inlet of cyclone separator 22；The dry system
System further includes air delivery tube 23 and dry powder blender 24, and the discharge port of cyclone separator 22 passes through air delivery tube 23 and dry powder
The feed inlet of mixing machine 24 is connected to；Dry powder blender 24 is conical mixer；Airstream drying tower 21 is dense by stoste preparation system
The emamectin benzoate concentrate that contracting kettle 6 generates is dried to emamectin benzoate powder, and the emamectin benzoate powder that airstream drying tower 21 generates is defeated through heat point
It send to cyclone separator 22, cyclone separator 22 recycles the emamectin benzoate particle carried in hot wind, and emamectin benzoate powder is by revolving
The discharge port of wind separator 22 falls into dry powder blender 24, and dry powder blender 24, which stirs evenly emamectin benzoate powder, produces emamectin benzoate
Quality is uniform；
The drying system further includes dry condenser 25 and dry condensation fluid reservoir 26, the air inlet of dry condenser 25 with
The gas outlet of cyclone separator 22 is connected to, and the liquid outlet of dry condenser 25 is connected to dry condensation fluid reservoir 26；Dry condensation
Fluid reservoir 26 is connected to concentration kettle 6 by circulating pump 27；A small amount of first can be carried in the gas being discharged by cyclone separator 22
Alkane liquid, dry condenser 25 will be discharged into dry condensation fluid reservoir 26 after methane liquid condensation, circulating pump 27 is condensed dry
Methane liquid in fluid reservoir 26 is pumped into dilution dissolution kettle 1 and is recycled, and avoids environmental pollution, improves methane liquid
Utilization rate.
Claims (8)
1. emamectin benzoate preparation system, which is characterized in that it includes stoste preparation system and drying system, the stoste preparation system
Including passing sequentially through the dilution dissolution kettle of pipeline connection, distillation still, stills for air blowing, amination kettle, adjusting sour kettle, concentration kettle, with the oxygen
Change the oxidant storage tank of kettle connection, the aminating agent storage tank being connected to the amination kettle, with the acid-base accommodation for adjusting sour kettle to be connected to
Agent storage tank, the benzoic acid feed bin being connected to the concentration kettle；The drying system includes airstream drying tower and more than one rotation
Wind separator, the feed inlet of the airstream drying tower are connected with the discharge port of the concentration kettle；The discharging of the airstream drying tower
Mouth is connected with the feed inlet of the cyclone separator.
2. emamectin benzoate preparation system according to claim 1, which is characterized in that the stoste preparation system further includes distillation
Condenser is distilled to recover tank, and the distiller condenser is equipped on the gas outlet of the distillation still, and the distiller condenser goes out
The mouth of a river is connected with the feed inlet for being distilled to recover tank, and the inlet of the distillation recovery tank and the dilution dissolution kettle passes through water
Pump is connected.
3. emamectin benzoate preparation system according to claim 1, which is characterized in that the stoste preparation system further includes concentration
Condenser, concentration and recovery tank are equipped with the concentration condenser on the gas outlet of the concentration kettle, and the concentration condenser goes out
The mouth of a river is connected with the feed inlet of the concentration and recovery tank, and the inlet of the concentration and recovery tank and the dilution dissolution kettle passes through water
Pump is connected.
4. emamectin benzoate preparation system according to claim 1, which is characterized in that the stoste preparation system further includes filtering
Equipment, the pipeline between the stills for air blowing and the amination kettle are equipped with the filter plant, and the filter plant is centrifuge
Or any one of filtering tank.
5. emamectin benzoate preparation system according to any one of claims 1 to 4, which is characterized in that in the distillation still, the oxygen
The inner wall for changing kettle, the amination kettle and the concentration kettle is equipped at least three pieces of spiral deflectors being arranged in the shape of a spiral.
6. emamectin benzoate preparation system according to any one of claims 1 to 4, which is characterized in that the distillation still, the oxidation
The upper layer and lower layer stirring blade of reversed eddy flow is equipped on the agitating shaft of kettle, the amination kettle and the concentration kettle.
7. emamectin benzoate preparation system according to any one of claims 1 to 4, which is characterized in that in the institute adjusted in sour kettle
The nozzle for stating regulating acid agent feed pipe is equipped with spray head.
8. emamectin benzoate preparation system according to claim 1, which is characterized in that the drying system further includes dry condensation
Device and dry condensation fluid reservoir, the air inlet of the dry condenser are connected to the gas outlet of the cyclone separator, described dry
The liquid outlet of dry condenser is connected to the dry condensation fluid reservoir.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201511022640.3A CN105461771B (en) | 2015-12-30 | 2015-12-30 | Emamectin benzoate preparation system |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201511022640.3A CN105461771B (en) | 2015-12-30 | 2015-12-30 | Emamectin benzoate preparation system |
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| Publication Number | Publication Date |
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| CN105461771A CN105461771A (en) | 2016-04-06 |
| CN105461771B true CN105461771B (en) | 2019-02-12 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201511022640.3A Active CN105461771B (en) | 2015-12-30 | 2015-12-30 | Emamectin benzoate preparation system |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102641712A (en) * | 2012-02-29 | 2012-08-22 | 大庆志飞生物化工有限公司 | Novel reaction kettle for producing methylamino avermectin benzoate |
| CN203613127U (en) * | 2013-12-23 | 2014-05-28 | 大庆志飞生物化工有限公司 | Avermectin benzoate production system |
| CN205347282U (en) * | 2015-12-30 | 2016-06-29 | 内蒙古嘉宝仕生物科技股份有限公司 | First dimension salt preparation system |
| CN205347285U (en) * | 2015-12-30 | 2016-06-29 | 内蒙古嘉宝仕生物科技股份有限公司 | First dimension salt preparation system |
| CN205443136U (en) * | 2015-12-30 | 2016-08-10 | 内蒙古嘉宝仕生物科技股份有限公司 | First dimension salt preparation system |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN205347284U (en) * | 2015-12-30 | 2016-06-29 | 内蒙古嘉宝仕生物科技股份有限公司 | First dimension salt preparation system |
-
2015
- 2015-12-30 CN CN201511022640.3A patent/CN105461771B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102641712A (en) * | 2012-02-29 | 2012-08-22 | 大庆志飞生物化工有限公司 | Novel reaction kettle for producing methylamino avermectin benzoate |
| CN203613127U (en) * | 2013-12-23 | 2014-05-28 | 大庆志飞生物化工有限公司 | Avermectin benzoate production system |
| CN205347282U (en) * | 2015-12-30 | 2016-06-29 | 内蒙古嘉宝仕生物科技股份有限公司 | First dimension salt preparation system |
| CN205347285U (en) * | 2015-12-30 | 2016-06-29 | 内蒙古嘉宝仕生物科技股份有限公司 | First dimension salt preparation system |
| CN205443136U (en) * | 2015-12-30 | 2016-08-10 | 内蒙古嘉宝仕生物科技股份有限公司 | First dimension salt preparation system |
Non-Patent Citations (1)
| Title |
|---|
| 甲胺基阿维菌素苯甲酸盐原药结晶工艺优化;张海健;《中国优秀硕士学位论文全文数据库（电子期刊）》;20120315;B016-288 |
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| CN105461771A (en) | 2016-04-06 |
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