CN112516922A - Preparation process of fipronil - Google Patents
Preparation process of fipronil Download PDFInfo
- Publication number
- CN112516922A CN112516922A CN202011490736.3A CN202011490736A CN112516922A CN 112516922 A CN112516922 A CN 112516922A CN 202011490736 A CN202011490736 A CN 202011490736A CN 112516922 A CN112516922 A CN 112516922A
- Authority
- CN
- China
- Prior art keywords
- reactor
- liquid mixing
- burette
- sleeve
- mixing pipe
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- ZOCSXAVNDGMNBV-UHFFFAOYSA-N 5-amino-1-[2,6-dichloro-4-(trifluoromethyl)phenyl]-4-[(trifluoromethyl)sulfinyl]-1H-pyrazole-3-carbonitrile Chemical compound NC1=C(S(=O)C(F)(F)F)C(C#N)=NN1C1=C(Cl)C=C(C(F)(F)F)C=C1Cl ZOCSXAVNDGMNBV-UHFFFAOYSA-N 0.000 title claims abstract description 15
- 239000005899 Fipronil Substances 0.000 title claims abstract description 15
- 229940013764 fipronil Drugs 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 239000007788 liquid Substances 0.000 claims abstract description 35
- 238000002156 mixing Methods 0.000 claims abstract description 29
- 238000000034 method Methods 0.000 claims abstract description 15
- 239000000463 material Substances 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 5
- 210000001503 joint Anatomy 0.000 claims description 3
- 238000005192 partition Methods 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 10
- 230000002194 synthesizing effect Effects 0.000 abstract 1
- 230000001105 regulatory effect Effects 0.000 description 2
- 241001674044 Blattodea Species 0.000 description 1
- 241000257303 Hymenoptera Species 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 238000013016 damping Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 239000002917 insecticide Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- DQJCHOQLCLEDLL-UHFFFAOYSA-N tricyclazole Chemical compound CC1=CC=CC2=C1N1C=NN=C1S2 DQJCHOQLCLEDLL-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/02—Feed or outlet devices; Feed or outlet control devices for feeding measured, i.e. prescribed quantities of reagents
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D231/00—Heterocyclic compounds containing 1,2-diazole or hydrogenated 1,2-diazole rings
- C07D231/02—Heterocyclic compounds containing 1,2-diazole or hydrogenated 1,2-diazole rings not condensed with other rings
- C07D231/10—Heterocyclic compounds containing 1,2-diazole or hydrogenated 1,2-diazole rings not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members
- C07D231/14—Heterocyclic compounds containing 1,2-diazole or hydrogenated 1,2-diazole rings not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D231/44—Oxygen and nitrogen or sulfur and nitrogen atoms
Abstract
The invention relates to a preparation process of fipronil. Synthesizing the fipronil by adopting a continuous proportioning dropwise adding method; the device is structurally realized by adopting a device which comprises a plurality of burettes for dripping materials, wherein the burettes are annularly arranged and are arranged in an inverted frustum structure form, the lower parts of the burettes are provided with liquid mixing pipes communicated with the burettes, liquid inlets at the top and liquid outlets at the bottom of the liquid mixing pipes form horn mouths, and a main body of the liquid mixing pipe is spiral and is provided with a driving device for driving the liquid mixing pipe to rotate; the lower part of the liquid mixing pipe is provided with a reactor communicated with the liquid mixing pipe, the reactor is driven by a driving device to rotate, and a stirring device is arranged in the reactor. The invention adopts a continuous proportioning dropwise adding process, so that each reaction material reacts more uniformly in the reaction process, the reaction quality is improved, and the product yield is improved.
Description
Technical Field
The invention relates to a preparation process of fipronil, belonging to the technical field of pesticides.
Background
Fipronil is not environmentally friendly, although it is not used for rice control. But it is widely used in sanitary insecticide, mainly used for preventing and killing harmful organisms such as cockroaches, ants and the like, and has good use effect, so that fipronil still needs to be produced to a certain extent, and the reaction quality of the fipronil is improved.
Disclosure of Invention
The invention provides a preparation process of fipronil, which can further improve the quality of tricyclazole production.
The technical scheme adopted by the invention is as follows: a preparation process of fipronil, adopting a continuous proportioning dropwise adding method to synthesize the fipronil;
the continuous proportioning and dripping method is realized by adopting a device structure, the device comprises a plurality of burettes for dripping materials, the burettes are annularly arranged and are arranged in an inverted frustum structure, a liquid mixing pipe communicated with the burettes is arranged at the lower part of each burette, a liquid inlet at the top part and a liquid outlet at the bottom part of the liquid mixing pipe form bell mouths, and a main body of the liquid mixing pipe is spiral and is provided with a driving device for driving the liquid mixing pipe to rotate;
the lower part of the liquid mixing pipe is provided with a reactor communicated with the liquid mixing pipe, the reactor is driven by a driving device to rotate, and a stirring device is arranged in the reactor.
Furthermore, each burette is provided with a flow regulating valve.
Further, a return pipeline is arranged at the bottom of the reactor, extends to the upper part of the reactor and is communicated with the upper part of the reactor.
Further, a cover plate is arranged at the joint of the bottom of the reactor and the return pipe, and the cover plate can move to form two states: namely, the bottom of the reactor is communicated or separated with the return pipe.
Further, the device also comprises the following structure: the burette is characterized in that a vibration ring connected with each burette is arranged outside each burette, a sleeve pipe in butt joint is arranged on the side part of each vibration ring and each burette, and a flexible connecting piece is arranged in each sleeve pipe.
Furthermore, the flexible connecting piece is of a piston structure and comprises a sleeve arranged in the sleeve, the sleeve is divided into two isolated parts by a partition plate in the sleeve, air holes are formed in the two sides of the sleeve, and pressure of the two parts of the sleeve is adjusted through the air holes.
The invention has the advantages that: the invention adopts a continuous proportioning dropwise adding process, so that each reaction material reacts more uniformly in the reaction process, the reaction quality is improved, and the product yield is improved.
Drawings
FIG. 1 is a schematic structural diagram of the present invention.
Fig. 2 is an enlarged view of a portion a in fig. 1.
In the figure, 1 is a burette, 2 is a liquid mixing pipe, 3 is a reactor, 4 is a stirring device, 5 is a cover plate, 6 is a return pipeline, 7 is a vibration ring, 8 is a sleeve, 9 is a piston and 10 is an air hole.
Detailed Description
A preparation process of fipronil, adopting a continuous proportioning dropwise adding method to synthesize the fipronil;
the continuous proportioning and dripping method is realized by adopting a device structure, the device comprises a plurality of burettes for dripping materials, the burettes are annularly arranged and are arranged in an inverted frustum structure, a liquid mixing pipe communicated with the burettes is arranged at the lower part of each burette, a liquid inlet at the top part and a liquid outlet at the bottom part of the liquid mixing pipe form bell mouths, and a main body of the liquid mixing pipe is spiral and is provided with a driving device for driving the liquid mixing pipe to rotate;
the lower part of the liquid mixing pipe is provided with a reactor communicated with the liquid mixing pipe, the reactor is driven by a driving device to rotate, and a stirring device is arranged in the reactor.
Furthermore, each burette is provided with a flow regulating valve.
Further, a return pipeline is arranged at the bottom of the reactor, extends to the upper part of the reactor and is communicated with the upper part of the reactor.
Further, a cover plate is arranged at the joint of the bottom of the reactor and the return pipe, and the cover plate can move to form two states: namely, the bottom of the reactor is communicated or separated with the return pipe.
Further, the device also comprises the following structure: the burette is characterized in that a vibration ring connected with each burette is arranged outside each burette, a sleeve pipe in butt joint is arranged on the side part of each vibration ring and each burette, and a flexible connecting piece is arranged in each sleeve pipe.
Furthermore, the flexible connecting piece is of a piston structure and comprises a sleeve arranged in the sleeve, the sleeve is divided into two isolated parts by a partition plate in the sleeve, air holes are formed in the two sides of the sleeve, and pressure of the two parts of the sleeve is adjusted through the air holes.
The invention will be further explained below for a better understanding of the invention: the invention adopts a continuous proportioning dropping process, each reaction material is added through a respective burette, and under the action of the gravity of the burette, each reaction material enters the liquid mixing pipe at a certain speed for mixing.
The reactor is arranged in a mode that the reflux pipeline is arranged to enable materials to form a circular flow mode in the reactor, and surface-surface mixing is achieved.
The structure of the vibration ring outside the burette of the invention enables the vibration ring to drive each burette to vibrate in small amplitude, so that materials entering the burette can smoothly enter the liquid mixing pipe through each burette, and meanwhile, the burette and the vibration ring are connected by adopting a piston structure form, thus realizing the adjustment of the vibration amplitude of the burette by the adjustment of the piston damping, and further improving the reaction quality and efficiency.
Claims (6)
1. A preparation process of fipronil is characterized in that the fipronil is synthesized by adopting a continuous proportioning dropwise adding method;
the continuous proportioning and dripping method is realized by adopting a device structure, the device comprises a plurality of burettes for dripping materials, the burettes are annularly arranged and are arranged in an inverted frustum structure, a liquid mixing pipe communicated with the burettes is arranged at the lower part of each burette, a liquid inlet at the top part and a liquid outlet at the bottom part of the liquid mixing pipe form bell mouths, and a main body of the liquid mixing pipe is spiral and is provided with a driving device for driving the liquid mixing pipe to rotate;
the lower part of the liquid mixing pipe is provided with a reactor communicated with the liquid mixing pipe, the reactor is driven by a driving device to rotate, and a stirring device is arranged in the reactor.
2. The process according to claim 1, wherein each burette is provided with a flow control valve.
3. The process according to claim 1, wherein a return line is provided at the bottom of the reactor, and the return line extends to and is communicated with the upper part of the reactor.
4. The process according to claim 3, wherein a cover plate is arranged at the joint of the bottom of the reactor and the return pipe, and the cover plate can move to form two states: namely, the bottom of the reactor is communicated or separated with the return pipe.
5. The process according to claim 3, wherein the apparatus further comprises the following structure: the burette is characterized in that a vibration ring connected with each burette is arranged outside each burette, a sleeve pipe in butt joint is arranged on the side part of each vibration ring and each burette, and a flexible connecting piece is arranged in each sleeve pipe.
6. The process according to claim 5, wherein the flexible connecting member is a piston structure and comprises a sleeve disposed in the sleeve, the sleeve is divided into two parts by a partition, the two sides of the sleeve are provided with air holes, and the pressure of the two parts of the sleeve is adjusted through the air holes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011490736.3A CN112516922A (en) | 2020-12-16 | 2020-12-16 | Preparation process of fipronil |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011490736.3A CN112516922A (en) | 2020-12-16 | 2020-12-16 | Preparation process of fipronil |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112516922A true CN112516922A (en) | 2021-03-19 |
Family
ID=75000773
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011490736.3A Pending CN112516922A (en) | 2020-12-16 | 2020-12-16 | Preparation process of fipronil |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112516922A (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102093295A (en) * | 2011-03-10 | 2011-06-15 | 江苏长青农化股份有限公司 | Synthesis method of insecticide Fipronil |
| CN107661721A (en) * | 2017-03-13 | 2018-02-06 | 许昌义 | Pneumatic vibration formula helix tube blender |
| CN208678857U (en) * | 2018-07-25 | 2019-04-02 | 大理金明动物药业有限公司 | A kind of high-efficiency and energy-saving type Agitation Tank |
| CN210279095U (en) * | 2019-05-28 | 2020-04-10 | 无锡海特圣大光电材料科技有限公司 | Spiral stirring and feeding device for producing dimethomorph |
-
2020
- 2020-12-16 CN CN202011490736.3A patent/CN112516922A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102093295A (en) * | 2011-03-10 | 2011-06-15 | 江苏长青农化股份有限公司 | Synthesis method of insecticide Fipronil |
| CN107661721A (en) * | 2017-03-13 | 2018-02-06 | 许昌义 | Pneumatic vibration formula helix tube blender |
| CN208678857U (en) * | 2018-07-25 | 2019-04-02 | 大理金明动物药业有限公司 | A kind of high-efficiency and energy-saving type Agitation Tank |
| CN210279095U (en) * | 2019-05-28 | 2020-04-10 | 无锡海特圣大光电材料科技有限公司 | Spiral stirring and feeding device for producing dimethomorph |
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| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210319 |