CN220047997U - Imidacloprid crystal form I continuous production device - Google Patents
Imidacloprid crystal form I continuous production device Download PDFInfo
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- CN220047997U CN220047997U CN202321144328.1U CN202321144328U CN220047997U CN 220047997 U CN220047997 U CN 220047997U CN 202321144328 U CN202321144328 U CN 202321144328U CN 220047997 U CN220047997 U CN 220047997U
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- kettle
- imidacloprid
- pipeline
- cooling
- crystal form
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- YWTYJOPNNQFBPC-UHFFFAOYSA-N imidacloprid Chemical compound [O-][N+](=O)\N=C1/NCCN1CC1=CC=C(Cl)N=C1 YWTYJOPNNQFBPC-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 239000005906 Imidacloprid Substances 0.000 title claims abstract description 35
- 229940056881 imidacloprid Drugs 0.000 title claims abstract description 35
- 239000013078 crystal Substances 0.000 title claims abstract description 30
- 238000010924 continuous production Methods 0.000 title claims abstract description 18
- 238000001816 cooling Methods 0.000 claims abstract description 37
- 238000007599 discharging Methods 0.000 claims abstract description 16
- 238000003860 storage Methods 0.000 claims abstract description 11
- 239000002904 solvent Substances 0.000 claims abstract description 9
- 238000002425 crystallisation Methods 0.000 claims description 40
- 230000008025 crystallization Effects 0.000 claims description 37
- 238000004090 dissolution Methods 0.000 claims description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- 238000010438 heat treatment Methods 0.000 claims description 4
- 239000002826 coolant Substances 0.000 claims description 3
- 239000000463 material Substances 0.000 abstract description 17
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 238000004140 cleaning Methods 0.000 abstract description 4
- 235000011194 food seasoning agent Nutrition 0.000 abstract description 2
- 239000004278 EU approved seasoning Substances 0.000 abstract 1
- 238000000034 method Methods 0.000 description 11
- 239000011521 glass Substances 0.000 description 10
- 230000008569 process Effects 0.000 description 6
- 241000607479 Yersinia pestis Species 0.000 description 4
- 239000003814 drug Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000003507 refrigerant Substances 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 239000011343 solid material Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 230000001276 controlling effect Effects 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- SKCNYHLTRZIINA-UHFFFAOYSA-N 2-chloro-5-(chloromethyl)pyridine Chemical compound ClCC1=CC=C(Cl)N=C1 SKCNYHLTRZIINA-UHFFFAOYSA-N 0.000 description 1
- WRYCSMQKUKOKBP-UHFFFAOYSA-N Imidazolidine Chemical compound C1CNCN1 WRYCSMQKUKOKBP-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 210000003169 central nervous system Anatomy 0.000 description 1
- 238000012824 chemical production Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 235000013409 condiments Nutrition 0.000 description 1
- 230000002596 correlated effect Effects 0.000 description 1
- 230000000857 drug effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000000749 insecticidal effect Effects 0.000 description 1
- 239000002917 insecticide Substances 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- DJZWNSRUEJSEEB-UHFFFAOYSA-N n-(4,5-dihydro-1h-imidazol-2-yl)nitramide Chemical compound [O-][N+](=O)NC1=NCCN1 DJZWNSRUEJSEEB-UHFFFAOYSA-N 0.000 description 1
- 230000000361 pesticidal effect Effects 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 210000002784 stomach Anatomy 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The utility model relates to a continuous production device of imidacloprid crystal form I, which comprises a feeding device, a dissolving device, a crystallizing device and a centrifuging device, wherein the feeding device comprises a storage tank, a feeding machine and a solvent proportion pump, the dissolving device comprises a batching kettle and a dissolving kettle, the crystallizing device comprises a crystallizing kettle and a cooling kettle, stirrers are respectively arranged in the batching kettle, the dissolving kettle, the crystallizing kettle and the cooling kettle, and the batching kettle, the dissolving kettle, the crystallizing kettle and the cooling kettle are connected in series through overflow pipelines; the centrifugal device comprises a discharging centrifugal machine and a pneumatic valve. The utility model improves the automation degree and the precision of the production process of the imidacloprid crystal form I, and can effectively reduce the phenomena of misfeeding and inaccurate proportion of seasonings; the control rate of the imidacloprid crystal form I is effectively improved, and bad material batches are stopped; the production efficiency is greatly improved, and the pipeline cleaning times in a parking state can be effectively reduced.
Description
Technical Field
The utility model belongs to the field of chemical production devices, and particularly relates to a continuous production device for imidacloprid crystal form I.
Background
Imidacloprid is a neonicotinoid insecticide with chemical formula C 9 H 10 ClN 5 O 2 . Has the advantages of broad spectrum, high efficiency, low toxicity, low residue, uneasy generation of resistance of pests, and multiple functions of contact killing, stomach toxicity, internal absorption, etc. After the pests are contacted with the medicament, the normal conduction of the central nervous system is blocked, so that the pests paralyze and die. The product has good quick-acting property, high prevention effect after 1 day of medicine, and the residual period is about 25 days. The pesticide effect and the temperature are positively correlated, the temperature is high, the insecticidal effect is good, and the pesticide is mainly used for preventing and controlling piercing-sucking mouthpart pests. At present, an important synthetic route of domestic imidacloprid adopts 2-chloro-5-chloromethylpyridine and 2-nitroiminoimidazolidine to be synthesized under the action of acid-binding agent sodium hydroxide, and the process route is as follows:
at present, the preparation process of imidacloprid still has the problems of high impurity content, high environmental protection pressure and the like. In order to meet the market demands and meet the increasingly strict product quality requirements of the market, the sustainable development direction of green chemistry is complied with, and high-quality products must be prepared. Two main forms of imidacloprid have been found, imidacloprid form I and imidacloprid form II, the melting point of form I is 143.8deg.C and the melting point of form II is 136.4deg.C. The same medicine with different crystal forms has obvious difference in the aspects of solubility, dissolution rate, melting point, density, hardness, appearance, stability, bioavailability and the like, so that the stability, bioavailability and curative effect of the medicine are affected. The literature reports that the drug effect of imidacloprid of the crystal form I is 4-5 times higher than that of the imidacloprid of the II type in certain preparation varieties, so that a process and a device suitable for mass production are required to be developed to produce the imidacloprid of the crystal form I.
The preparation method of the imidacloprid crystal form I has a plurality of modes, especially recrystallization, and is an important means for regulating and controlling the crystal form, purity and granularity of the finished product. The content of the impurities such as the imidazolidine, the bisimidacloprid and the like in the imidacloprid technical produced by the current enterprises is high, and the imidacloprid technical is a key factor influencing the quality of products. Therefore, research on its polymorphic regulation is needed to obtain better quality products to improve market competitiveness.
The traditional crystallization process has poor stability and different product performances of different batches. In such a large background, novel crystallization techniques have been rapidly developed, such as supercritical fluid crystallization techniques, film crystallization techniques, and the like. The novel crystallization technique largely avoids the disadvantages of the conventional process, but is currently difficult to use in large-scale industrial production because the equipment used in the novel crystallization technique is expensive and the yield is limited. Therefore, we have studied a kettle type series continuous device suitable for mass production application to prepare the crystal form I imidacloprid.
Disclosure of Invention
In order to solve the problems in the prior art, the utility model aims to provide the continuous production device for the imidacloprid crystal form I, which has the advantages of reasonable structure, compact layout and stable crystallization.
In order to solve the technical problems, the utility model adopts the following technical scheme: the utility model provides an imidacloprid crystal form I continuous production device, includes loading attachment, dissolving device, crystallization device, centrifugal device, loading attachment include storage tank, material loading machine, solvent proportion pump, the material loading machine include motor, screw conveyer, material loading pipeline, screw conveyer sets up in material loading pipeline, the motor sets up in material loading pipeline one end, passes through drive shaft connection with screw conveyer, the storage tank sets up in material loading pipeline top, the storage tank bottom passes through the pipeline and is connected with material loading pipeline upper side wall;
the dissolution device comprises a batching kettle and a dissolution kettle, the crystallization device comprises a crystallization kettle and a cooling kettle, stirrers are respectively arranged in the batching kettle, the dissolution kettle, the crystallization kettle and the cooling kettle, the batching kettle, the dissolution kettle, the crystallization kettle and the cooling kettle are connected in series through overflow pipelines, and are a first overflow pipeline, a second overflow pipeline and a third overflow pipeline, and metering pumps are arranged on the overflow pipelines;
the centrifugal device comprises a lower discharging centrifugal machine and a pneumatic valve, wherein the number of the lower discharging centrifugal machine is 2, the lower discharging centrifugal machine is connected with the cooling kettle in parallel through a pipeline, and the pneumatic valve is arranged on a connecting pipeline.
Further, the stirrers arranged in the batching kettle and the dissolution kettle are anchor stirrers, and the stirrers arranged in the crystallization kettle and the cooling kettle are push stirrers;
further, the upper parts of the batching kettle, the dissolution kettle, the crystallization kettle and the cooling kettle are provided with observation ports;
further, the upper part of the observation port is provided with a sight glass;
further, jackets are arranged on the batching kettle, the dissolution kettle, the crystallization kettle and the cooling kettle;
further, the jackets are provided with a water inlet and a water outlet;
further, the temperature of heating medium of jackets of the batching kettle and the dissolution kettle is 70-90 ℃;
further, the temperature of the cooling medium of the crystallization kettle jacket is 20-30 ℃;
further, the temperature of the refrigerant of the cooling kettle jacket is-10 to-15 ℃;
further, the first overflow pipeline, the second overflow pipeline and the third overflow pipeline form an included angle of 20-30 degrees with the horizontal plane.
By adopting the technology, compared with the prior art, the utility model has the remarkable advantages that:
1) By arranging the feeding machine, the automation degree and the precision of the solid material feeding process are improved, the feeding amount of the solid material can be controlled by controlling the rotating speed and the start and stop of the motor, and the phenomenon of misfeeding and mismatching of the seasoning proportion can be effectively reduced;
2) The solvent proportion pump can accurately control the feeding proportion of the solvent, and ensures the stable feeding proportion;
3) Through arranging the batching kettle and the dissolution kettle and introducing hot water with fixed temperature, the dissolution effect of the materials is ensured, and the phenomenon that the materials are not completely dissolved is avoided;
4) By arranging the crystallization kettle, the imidacloprid with the crystal form I is always in the kettle, so that the solid after crystallization is ensured to be the imidacloprid with the crystal form I; simultaneously, a stirrer is arranged to ensure that the solution and the solid are uniformly dispersed and uniformly flow from the overflow pipeline to the cooling kettle;
5) Through setting a cooling kettle, introducing a constant-temperature refrigerant, realizing rapid cooling precipitation of materials, and obtaining the crystal form I imidacloprid;
6) The serialization device makes imidacloprid crystal form I production efficiency improve by a wide margin, and it is more convenient to clear up pipeline and reation kettle, can effectively reduce the pipeline cleaning number of times of parking state.
Drawings
FIG. 1 is a schematic structural view of a continuous production device of imidacloprid form I;
the following figures are shown: 1-loading attachment, 11-storage tank, 12-solvent proportioning pump, 13-feeder, 131-motor, 132-screw conveyer, 133-feeding pipeline, 2-batching cauldron, 21-batching agitator, 22-batching cauldron jacket, 221-a water inlet, 222-a water outlet, 23-a sight glass, 24-first overflow pipeline, 241-a metering valve, 3-dissolution cauldron, 31-dissolution agitator, 32-dissolution cauldron jacket, 321-b water inlet, 322-b water outlet, 33-b sight glass, 34-second overflow pipeline, 341-b metering valve, 4-crystallization cauldron, 41-crystallization agitator, 42-crystallization cauldron jacket, 421-c water inlet, 422-c water outlet, 43-c sight glass, 44-third overflow pipeline, 441-c metering valve, 5-cooling cauldron, 51-cooling agitator, 52-cooling cauldron jacket, 521-d water inlet, 522-d water outlet, 53-d sight glass, 6-first lower discharge centrifuge, 61-a pneumatic valve, 7-second lower discharge centrifuge, 71-b pneumatic valve.
Detailed Description
In order to make the technical scheme and advantages of the present utility model more apparent, the present utility model will be further described in detail with reference to the following examples.
Example 1
The continuous production device of the imidacloprid crystal form I shown in fig. 1 comprises a feeding device 1, a dissolving device, a crystallizing device and a centrifuging device, wherein the feeding device 1 comprises a storage tank 11, a feeding machine 13 and a solvent proportion pump 12, the feeding machine comprises a motor 131, a screw conveyer 132 and a feeding pipeline 133, the screw conveyer 132 is arranged in the feeding pipeline 133, the motor 131 is arranged at one end of the feeding pipeline 133 and is connected with the screw conveyer 132 through a driving shaft, the storage tank 11 is arranged above the feeding pipeline 133, and the bottom of the storage tank 11 is connected with the upper side wall of the feeding pipeline 133 through a pipeline; the solvent proportion pump 12 can accurately control the feeding proportion of the solvent, and ensures the stable feeding proportion; through setting up material loading machine 13, improved degree of automation and the precision of solid material feeding process, through the rotational speed of control motor 131 and start and stop can control the solid material and throw the material volume, can effectually reduce throw wrong material and the phenomenon that condiment proportion is wrong.
The dissolving device comprises a batching kettle 2 and a dissolving kettle 3, the crystallizing device comprises a crystallizing kettle 4 and a cooling kettle 5, stirrers are respectively arranged in the batching kettle 2, the dissolving kettle 3, the crystallizing kettle 4 and the cooling kettle 5, the batching kettle 2, the dissolving kettle 3, the crystallizing kettle 4 and the cooling kettle 5 are connected in series through overflow pipelines, and an included angle of 20-30 degrees is formed between the first overflow pipeline 24, the second overflow pipeline 34 and the third overflow pipeline 44 and a horizontal plane; metering valves, namely an a metering valve 241, a b metering valve 341 and a c metering valve 441, are respectively arranged on the first overflow pipeline 24, the second overflow pipeline 34 and the third overflow pipeline 44; the stirrers arranged in the batching kettle 2 and the dissolution kettle 3 are anchor stirrers, namely a batching stirrer 21 and a dissolution stirrer 31; the stirrers arranged in the crystallization kettle 4 and the cooling kettle 5 are push stirrers, namely a crystallization stirrer 41 and a cooling stirrer 51; the upper parts of the batching kettle 2, the dissolution kettle 3, the crystallization kettle 4 and the cooling kettle 5 are provided with observation ports; the upper part of the observation port is provided with a sight glass, namely an a sight glass 23, a b sight glass 33, a c sight glass 43 and a d sight glass 53. Jackets are respectively arranged on the batching kettle 2, the dissolution kettle 3, the crystallization kettle 4 and the cooling kettle 5, namely a batching kettle jacket 22, a dissolution kettle jacket 32, a crystallization kettle jacket 42 and a cooling kettle jacket 52, and are respectively provided with a water inlet and a water outlet; the batching kettle jacket 22 is provided with an a water inlet 221 and an a water outlet 222, and the temperature of heating medium is 70-90 ℃; the dissolution kettle jacket 32 is provided with a b water inlet 321 and a b water outlet 322, and the temperature of the heating medium is 70-90 ℃; through setting up batching cauldron 2 and dissolution kettle 3 to let in 70 ~ 90 ℃ fixed temperature's hot water, guaranteed the dissolution effect of material, can not appear the material and do not dissolve complete phenomenon. The crystallization kettle jacket 42 is provided with a c water inlet 421 and a c water outlet 422, and the temperature of the cooling medium is 20-30 ℃; the cooling kettle jacket 52 is provided with a d water inlet 521 and a d water outlet 522, the temperature of the refrigerant is-10 to-15 ℃, and the refrigerant medium is introduced to realize the rapid cooling precipitation of the material, thus obtaining the crystal form I imidacloprid.
By arranging the crystallization kettle 4, the imidacloprid with the crystal form I is always present in the crystallization kettle 4, so that the solid after crystallization is ensured to be the imidacloprid with the crystal form I; simultaneously, a crystallization stirrer 41 is arranged to ensure that the solution and the solid are uniformly dispersed and uniformly flow from a third overflow pipeline 44 to the cooling kettle 5; the centrifugal device comprises a lower discharging centrifugal machine and a pneumatic valve, wherein the number of the lower discharging centrifugal machines is 2, the lower discharging centrifugal machine is respectively a first lower discharging centrifugal machine 6 and a second lower discharging centrifugal machine 7, the lower discharging centrifugal machine is connected with a cooling kettle in parallel through a pipeline, an a pneumatic valve 61 is arranged on a connecting pipeline of the first lower discharging centrifugal machine 6 and a crystallization kettle 5, and a b pneumatic valve 71 is arranged on a connecting pipeline of the second lower discharging centrifugal machine 7 and the first lower discharging centrifugal machine 6. The continuous device of the utility model greatly improves the production efficiency of the imidacloprid crystal form I, is more convenient for cleaning the pipeline and the reaction kettle, and can effectively reduce the pipeline cleaning times in a parking state.
The above embodiments are only preferred embodiments of the present utility model, and should not be construed as limiting the present utility model, and the protection scope of the present utility model should be defined by the claims, including the technical equivalents of the technical features in the claims, as the protection scope, that is, the equivalent replacement and improvement within the protection scope of the present utility model.
Claims (10)
1. The continuous production device for the imidacloprid crystal form I comprises a feeding device, a dissolving device, a crystallizing device and a centrifuging device, and is characterized in that the feeding device comprises a storage tank, a feeding machine and a solvent proportion pump, the feeding machine comprises a motor, a screw conveyer and a feeding pipeline, the screw conveyer is arranged in the feeding pipeline, the motor is arranged at one end of the feeding pipeline and is connected with the screw conveyer through a driving shaft, and the storage tank is arranged above the feeding pipeline, and the bottom of the storage tank is connected with the upper side wall of the feeding pipeline through a pipeline;
the dissolution device comprises a batching kettle and a dissolution kettle, the crystallization device comprises a crystallization kettle and a cooling kettle, stirrers are respectively arranged in the batching kettle, the dissolution kettle, the crystallization kettle and the cooling kettle, the batching kettle, the dissolution kettle, the crystallization kettle and the cooling kettle are connected in series through overflow pipelines, and are a first overflow pipeline, a second overflow pipeline and a third overflow pipeline, and metering pumps are arranged on the overflow pipelines;
the centrifugal device comprises a lower discharging centrifugal machine and a pneumatic valve, wherein the number of the lower discharging centrifugal machine is 2, the lower discharging centrifugal machine is connected with the cooling kettle in parallel through a pipeline, and the pneumatic valve is arranged on a connecting pipeline.
2. The continuous production device for imidacloprid crystal form I according to claim 1, wherein the stirrer arranged inside the batching kettle and the dissolution kettle is an anchor stirrer, and the stirrer arranged inside the crystallization kettle and the cooling kettle is a propelling stirrer.
3. The continuous production device for imidacloprid crystal form I according to claim 1, wherein the upper parts of the batching kettle, the dissolution kettle, the crystallization kettle and the cooling kettle are provided with observation openings.
4. A continuous production device for imidacloprid form i according to claim 3, wherein the upper portion of the viewing port is provided with a viewing mirror.
5. The continuous production device for imidacloprid crystal form I according to claim 1, wherein the batching kettle, the dissolution kettle, the crystallization kettle and the cooling kettle are all provided with jackets.
6. The continuous production device for imidacloprid form I according to claim 5, wherein the jackets are provided with a water inlet and a water outlet.
7. The continuous production device for imidacloprid crystal form I according to claim 5, wherein the heating medium temperature of the jacket of the batching kettle and the dissolution kettle is 70-90 ℃.
8. The continuous production device for imidacloprid form I according to claim 5, wherein the cooling medium temperature of the jacket of the crystallization kettle is 20-30 ℃.
9. The continuous production device for imidacloprid crystal form I according to claim 5, wherein the temperature of the cooling jacket is-10 to-15 ℃.
10. The continuous production device for imidacloprid crystal form I according to claim 1, wherein the first overflow pipeline, the second overflow pipeline and the third overflow pipeline form an included angle of 20-30 degrees with the horizontal plane.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202321144328.1U CN220047997U (en) | 2023-05-12 | 2023-05-12 | Imidacloprid crystal form I continuous production device |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202321144328.1U CN220047997U (en) | 2023-05-12 | 2023-05-12 | Imidacloprid crystal form I continuous production device |
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| Publication Number | Publication Date |
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| CN220047997U true CN220047997U (en) | 2023-11-21 |
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| CN202321144328.1U Active CN220047997U (en) | 2023-05-12 | 2023-05-12 | Imidacloprid crystal form I continuous production device |
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| Country | Link |
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