CN112827445A - Production method and equipment for reducing thiazide impurities - Google Patents
Production method and equipment for reducing thiazide impurities Download PDFInfo
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- CN112827445A CN112827445A CN202011560420.7A CN202011560420A CN112827445A CN 112827445 A CN112827445 A CN 112827445A CN 202011560420 A CN202011560420 A CN 202011560420A CN 112827445 A CN112827445 A CN 112827445A
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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
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
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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
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
- B01J19/0013—Controlling the temperature of the process
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C335/00—Thioureas, i.e. compounds containing any of the groups, the nitrogen atoms not being part of nitro or nitroso groups
- C07C335/04—Derivatives of thiourea
- C07C335/06—Derivatives of thiourea having nitrogen atoms of thiourea groups bound to acyclic carbon atoms
- C07C335/08—Derivatives of thiourea having nitrogen atoms of thiourea groups bound to acyclic carbon atoms of a saturated carbon skeleton
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Abstract
The invention discloses equipment for reducing buprofezin impurities, which comprises a kettle body, a power bearing, a stirring shaft and a support frame, wherein the power bearing comprises a motor, a driving shaft and a rotor, the rotor is meshed with the kettle body, and the production method of the equipment for reducing the buprofezin impurities comprises the following steps: the method comprises the steps of placing tert-butyl isothiocyanate in a drying reaction kettle, heating, vacuumizing, decompressing, preserving heat, stirring, improving production equipment for removing impurities on the basis of the prior art, thereby effectively improving the stirring stability of the kettle body, further facilitating the removal of M291 impurities, improving the yield of the intermediate 1-isopropyl-3-tert-butylthiourea, improving a process method, and achieving the purpose of controlling the impurity M291 to fit the production through simple process operation.
Description
Technical Field
The invention relates to the technical field of pesticide production, in particular to a production method and equipment for reducing buprofezin impurities.
Background
The synthesis of the pediculicide takes ammonium thiocyanate as a raw material to react with tert-butyl alcohol in the presence of hydrochloric acid to obtain a mixture of tert-butyl thiocyanate and tert-butyl isocyanate (called mixed ester for short), the mixture is subjected to transposition to obtain tert-butyl isothiocyanate (called isopropyl for short), and then the tert-butyl isothiocyanate reacts with isopropylamine to obtain 1-isopropyl-3-tert-butylthiourea (called thiourea for short). In addition, N-methyl amine reacts with phosgene to obtain N-methyl-N-phenyl amino formyl chloride, and then reacts with chlorine to obtain N-chloromethyl-N-phenyl amino formyl chloride (chloride for short). And finally, reacting the chloride with thiourea in the presence of an alkali reagent to obtain the chlorpheniramine.
In the original pesticide of the chlorpheniramine, a high content of the impurity M291 (2-isopropylimino-3-isopropyl-5-phenyl-3, 4,5, 6-tetrahydro-2H-1, 3, 5-thiadiazine-4-ketone) is contained, and the impurity is difficult to remove through crystallization.
Disclosure of Invention
The invention provides a production method and equipment for reducing buprofezin impurities, aiming at solving the problem that the content of M291 impurities in a prochloraz technical material is high in the prior art.
Reduce equipment of buprofezin impurity, including the cauldron body, power bearing, (mixing) shaft and support frame, the cauldron body with the power bearing cooperation, and set up in the periphery side of (mixing) shaft, the (mixing) shaft runs through the cauldron body with support frame fixed connection, power bearing with support frame fixed connection, and set up in the inside of support frame, power bearing includes motor, drive shaft and rotor, the motor set up in the upside of support frame, and with the upside of drive shaft passes through the speed reducer and connects, the rotor set up in the downside of drive shaft, and with the cauldron body meshes mutually.
The rotor comprises external meshing teeth, a connecting seat and a connecting bolt, the connecting seat is provided with a connecting hole, the connecting seat is arranged on the lower side of the stirring shaft, the connecting hole penetrates through the connecting seat and is matched with the driving shaft, the external meshing teeth are arranged on the outer peripheral side of the connecting seat and are meshed with the kettle body, and the connecting bolt penetrates through the connecting seat and is abutted to the driving shaft.
The support frame comprises a base and a fixing frame, the base is arranged on the outer peripheral side of the kettle body, and the fixing frame is arranged on the upper side of the base and fixedly connected with the stirring shaft.
The base comprises an arc-shaped frame, a rolling shaft and a rotating disc, the arc-shaped frame is arranged on the outer peripheral side of the kettle body and is in rolling connection with the kettle body through the rolling shaft, and the rotating disc is arranged on the lower side of the base and is in rotating connection with the base.
The fixing frame comprises a fixing plate and a supporting column, wherein the fixing plate is arranged on the upper side of the supporting column and fixedly connected with the motor.
Wherein, the rolling disc includes stable support and rotation post, stable support with the cauldron body agrees with mutually, and set up in the upside of rotating the post, rotate the post set up in the upside of base, and with the base rotates and is connected.
The invention also provides a production method adopting the equipment for reducing buprofezin impurities, which comprises the following steps:
adding tert-butyl isothiocyanate into the reaction kettle, and heating to 50-90 ℃;
vacuumizing to-0.06-0.095 MPa, keeping the vacuum for 1-3 hours, and carrying out reduced pressure, heat preservation and stirring to obtain the impurity-removed tert-butyl isothiocyanate;
and performing addition, cyclization and crystallization to obtain the buprofezin technical.
The invention has the beneficial effects that: on the basis of the prior art, production equipment for removing impurities is improved, the stirring stability of the kettle body is effectively improved by utilizing the matching of a driving shaft and the kettle body, the M291 impurities are conveniently removed, the yield of the intermediate 1-isopropyl-3-tert-butylthiourea is improved, the process method is improved, the carbon disulfide in the tert-butyl isothiocyanate is removed through simple process operation, and the purpose of controlling the impurities M291 so as to fit the production is achieved.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
Fig. 1 is a schematic structural diagram of the device for reducing buprofezin impurities in the invention.
Fig. 2 is a schematic structural view of a rotor of the device for reducing buprofezin impurities according to the present invention.
Fig. 3 is a process step schematic diagram of the production method of the apparatus for reducing buprofezin impurity according to the present invention.
10-kettle body, 20-dynamic bearing, 30-stirring shaft, 40-support frame, 11-sphere kettle, 12-matching teeth, 13-connecting end, 21-motor, 22-driving shaft, 23-rotor, 41-base, 42-fixing frame, 231-external meshing teeth, 232-connecting seat, 233-connecting bolt, 234-connecting hole, 411-arc frame, 412-rolling shaft, 413-rotating disc, 414-stabilizing support, 415-rotating column, 421-fixing plate and 422-supporting column.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the drawings are illustrative and intended to be illustrative of the invention and are not to be construed as limiting the invention.
In the description of the present invention, it is to be understood that the terms "length", "width", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", and the like, indicate orientations or positional relationships based on the orientations or positional relationships illustrated in the drawings, and are used merely for convenience in describing the present invention and for simplicity in description, and do not indicate or imply that the devices or elements referred to must have a particular orientation, be constructed in a particular orientation, and be operated, and thus, are not to be construed as limiting the present invention. Further, in the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
Referring to fig. 1 to 3, the present invention provides a technical solution:
reduce buprofezin impurity's equipment, including cauldron body 10, power bearing 20, (mixing) shaft 30 and support frame 40, cauldron body 10 with power bearing 20 cooperation, and set up in the periphery side of (mixing) shaft 30, (mixing) shaft 30 run through cauldron body 10 with support frame 40 fixed connection, power bearing 20 with support frame 40 fixed connection, and set up in the inside of support frame 40, power bearing 20 includes motor 21, drive shaft 22 and rotor 23, motor 21 set up in the upside of support frame 40, and with the upside of drive shaft 22 passes through the speed reducer and connects, rotor 23 set up in the downside of drive shaft 22, and with cauldron body 10 meshes mutually.
In this embodiment, the kettle 10 is used for reaction, the power bearing 20 is used for assisting the kettle 10 to rotate, the stirring shaft 30 is used for matching with the kettle 10, so that the interior of the kettle 10 can be stirred, the support frame 40 is used for supporting the kettle 10 and the power bearing 20, the motor 21 is used for rotating the driving shaft 22, and the rotor 23 is driven by the driving shaft 22 to rotate, so that the kettle 10 also rotates.
Further, the rotor 23 includes an external gear 231, a connecting seat 232 having a connecting hole 234, and a connecting bolt 233, the connecting seat 232 is disposed at a lower side of the stirring shaft 30, the connecting hole 234 penetrates through the connecting seat 232 and is engaged with the driving shaft 22, the external gear 231 is disposed at an outer circumferential side of the connecting seat 232 and is engaged with the kettle 10, and the connecting bolt 233 penetrates through the connecting seat 232 and is abutted to the driving shaft 22.
In this embodiment, the external teeth 231 are engaged with the rotor 23 to rotate the kettle 10 when the rotor 23 rotates, the connecting seat 232 is used for connecting the driving shaft 22, and the connecting bolt 233 is used for improving the connecting strength between the driving shaft 22 and the rotor 23.
Further, the supporting frame 40 includes a base 41 and a fixing frame 42, the base 41 is disposed on the outer peripheral side of the kettle 10, and the fixing frame 42 is disposed on the upper side of the base 41 and is fixedly connected to the stirring shaft 30.
In this embodiment, the base 41 is engaged with the fixing frame 42, so that the base 41 can support the kettle 10, and the fixing frame 42 is used to fix the power bearing 20.
Further, the base 41 includes an arc frame 411, a rolling shaft 412 and a rotating disc 413, the arc frame 411 is disposed on the outer peripheral side of the kettle body 10 and is connected to the kettle body 10 in a rolling manner through the rolling shaft 412, and the rotating disc 413 is disposed on the lower side of the base 41 and is connected to the base 41 in a rotating manner.
In this embodiment, arc frame 411 with be used for supporting the rotation of the cauldron body 10, roll axis 412 then is used for realizing the cauldron body 10 with rotation between the arc frame 411 is connected, rolling disc 413 set up in the downside of the cauldron body 10, and then further promote the rotation strength of the cauldron body 10, arc frame 411 still with (mixing) shaft 30 fixed connection, the utilization the rotation of the cauldron body 10, and then the realization is right the stirring of the inside material of the cauldron body 10.
Further, the fixing frame 42 includes a fixing plate 421 and a supporting column 422, and the fixing plate 421 is disposed on the upper side of the supporting column 422 and is fixedly connected to the motor 21.
In this embodiment, the fixing plate 421 is used to fix the motor 21, and the supporting column 422 is used to cooperate with the power bearing 20, so that the power bearing 20 can rotate.
Further, the rotating disc 413 comprises a stabilizing support 414 and a rotating column 415, the stabilizing support 414 is engaged with the kettle body 10 and is disposed on the upper side of the rotating column 415, and the rotating column 415 is disposed on the upper side of the base 41 and is rotatably connected with the base 41.
In this embodiment, the stabilizing bracket 414 is used to support the kettle 10, and the rotating column 415 is used to match the stabilizing bracket 414, so that the stabilizing bracket 414 can be rotatably connected to the base 41.
Further, the kettle body 10 includes a sphere kettle 11, a matching tooth 12 and a connecting end 13, the connecting end 13 is disposed on the upper side of the sphere kettle 11 and is rotatably connected to the rolling shaft 412, and the matching tooth 12 is disposed on the outer peripheral side of the sphere kettle 11 and is matched with the external engaging tooth 231.
In this embodiment, the sphere kettle 11 is used for reaction, the engaging teeth 12 engage with the external engaging teeth 231 to drive the sphere kettle 11 to rotate, and the connecting end 13 is used for connecting the sphere kettle 11 and the arc-shaped frame 411 and covers the outer periphery of the upper end of the stirring shaft 30.
The invention also provides a production method adopting the equipment for reducing buprofezin impurities, which comprises the following steps:
adding tert-butyl isothiocyanate into the reaction kettle, and heating to 50-90 ℃;
vacuumizing to-0.06-0.095 MPa, keeping the vacuum for 1-3 hours, and carrying out reduced pressure, heat preservation and stirring to obtain the impurity-removed tert-butyl isothiocyanate;
and performing addition, cyclization and crystallization to obtain the buprofezin technical.
Further, the impurity removal means that the content of 2-isopropylimino-3-isopropyl-5-phenyl-3, 4,5, 6-tetrahydro-2H-1, 3, 5-thiadiazine-4-ketone is less than or equal to 0.1 percent.
Detailed description of the preferred embodiment 1
Putting 115g (0.1mol) of tert-butyl isothiocyanate into a reaction kettle, heating to 50 ℃, increasing the vacuum to-0.095 Mpa, keeping the vacuum stable, stirring for 1 hour, and losing 0.5% of tert-butyl isothiocyanate;
quantifying carbon disulfide in the tert-butyl isothiocyanate by liquid chromatography, and confirming that the content is reduced to 0.08%;
the obtained tert-butyl isothiocyanate is subjected to addition, cyclization and crystallization to obtain a buprofezin technical product, wherein the content of M291 is 0.05%.
Specific example 2
Putting 115g (0.1mol) of tert-butyl isothiocyanate into a reaction kettle, heating to 70 ℃, increasing the vacuum to-0.085 Mpa, keeping the vacuum stable, stirring for 1 hour, and losing 0.5% of tert-butyl isothiocyanate;
quantifying carbon disulfide in the tert-butyl isothiocyanate by liquid chromatography, and confirming that the content is reduced to 0.03%;
the obtained tert-butyl isothiocyanate is subjected to addition, cyclization and crystallization to obtain a buprofezin technical product, wherein the content of M291 is 0.02%.
Specific example 3
Putting 115g (0.1mol) of tert-butyl isothiocyanate into a reaction kettle, heating to 80 ℃, increasing the vacuum to-0.07 Mpa, keeping the vacuum stable, stirring for 2 hours, and losing 1.3% of tert-butyl isothiocyanate;
quantifying carbon disulfide in the tert-butyl isothiocyanate by liquid chromatography, and confirming that the content is reduced to 0.05%;
the obtained tert-butyl isothiocyanate is subjected to addition, cyclization and crystallization to obtain a buprofezin technical product, wherein the content of M291 is 0.02%.
Specific example 4
Putting 115g (0.1mol) of tert-butyl isothiocyanate into a reaction kettle, heating to 90 ℃, increasing the vacuum to-0.08 Mpa, keeping the vacuum stable, stirring for 2 hours, and losing 1.2% of tert-butyl isothiocyanate;
quantifying carbon disulfide in the tert-butyl isothiocyanate by liquid chromatography, and confirming that the content is reduced to 0.06%;
the obtained tert-butyl isothiocyanate is subjected to addition, cyclization and crystallization to obtain a buprofezin technical product, wherein the content of M291 is 0.03%.
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (7)
1. Reduce buprofezin impurity's equipment, its characterized in that, including the cauldron body, power bearing, (mixing) shaft and support frame, the cauldron body with the power bearing cooperation, and set up in the periphery side of (mixing) shaft, the (mixing) shaft runs through the cauldron body with support frame fixed connection, power bearing with support frame fixed connection, and set up in the inside of support frame, power bearing includes motor, drive shaft and rotor, the motor set up in the upside of support frame, and with the upside of drive shaft passes through the speed reducer and connects, the rotor set up in the downside of drive shaft, and with the cauldron body meshes mutually.
2. The apparatus for reducing buprofezin impurities according to claim 1, wherein the rotor includes external teeth, a connecting seat provided with a connecting hole, and a connecting bolt, the connecting seat is disposed at a lower side of the stirring shaft, the connecting hole penetrates through the connecting seat and is engaged with the driving shaft, the external teeth are disposed at an outer circumferential side of the connecting seat and is engaged with the kettle body, and the connecting bolt penetrates through the connecting seat and is abutted against the driving shaft.
3. The apparatus for reducing buprofezin impurities according to claim 1, wherein the supporting frame comprises a base and a fixing frame, the base is disposed on an outer circumferential side of the kettle body, and the fixing frame is disposed on an upper side of the base and is fixedly connected to the stirring shaft.
4. The apparatus for reducing buprofezin impurities according to claim 3, wherein the base comprises an arc-shaped frame, a rolling shaft and a rotating disc, the arc-shaped frame is arranged on the outer peripheral side of the kettle body and is in rolling connection with the kettle body through the rolling shaft, and the rotating disc is arranged on the lower side of the base and is in rotating connection with the base.
5. The apparatus for reducing buprofezin impurities according to claim 4, wherein the fixing frame comprises a fixing plate and a supporting column, the fixing plate is disposed on an upper side of the supporting column and is fixedly connected to the motor.
6. The apparatus for reducing buprofezin impurities according to claim 4, wherein the rotating disc comprises a stabilizing tray and a rotating column, the stabilizing tray is engaged with the autoclave body and is disposed at an upper side of the rotating column, and the rotating column is disposed at an upper side of the base and is rotatably connected to the base.
7. The production method using the apparatus for reducing buprofezin impurity according to claim 6, characterized by comprising the steps of:
adding tert-butyl isothiocyanate into the reaction kettle, and heating to 50-90 ℃;
vacuumizing to-0.06-0.095 MPa, keeping the vacuum for 1-3 hours, and carrying out reduced pressure, heat preservation and stirring to obtain the impurity-removed tert-butyl isothiocyanate;
and performing addition, cyclization and crystallization to obtain the buprofezin technical.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011560420.7A CN112827445A (en) | 2020-12-25 | 2020-12-25 | Production method and equipment for reducing thiazide impurities |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011560420.7A CN112827445A (en) | 2020-12-25 | 2020-12-25 | Production method and equipment for reducing thiazide impurities |
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| CN112827445A true CN112827445A (en) | 2021-05-25 |
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| CN202011560420.7A Pending CN112827445A (en) | 2020-12-25 | 2020-12-25 | Production method and equipment for reducing thiazide impurities |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN207628418U (en) * | 2017-12-07 | 2018-07-20 | 浙江富锦新材料有限公司 | A kind of reaction kettle for fire retardant production |
| CN209501525U (en) * | 2019-02-01 | 2019-10-18 | 南昌欧泉琳化妆品有限公司 | A kind of efficient anti-acne paste emulsion reaction tank |
| CN210385842U (en) * | 2019-07-05 | 2020-04-24 | 鹤壁宝来化工科技有限公司 | Chemical industry reation kettle that stirring effect is good |
| CN211070063U (en) * | 2019-07-25 | 2020-07-24 | 四川盛年同缔实业有限公司 | Petrochemical reation kettle |
| CN211514304U (en) * | 2019-12-26 | 2020-09-18 | 东联北方科技(北京)有限公司 | Adhesive stirring equipment |
-
2020
- 2020-12-25 CN CN202011560420.7A patent/CN112827445A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN207628418U (en) * | 2017-12-07 | 2018-07-20 | 浙江富锦新材料有限公司 | A kind of reaction kettle for fire retardant production |
| CN209501525U (en) * | 2019-02-01 | 2019-10-18 | 南昌欧泉琳化妆品有限公司 | A kind of efficient anti-acne paste emulsion reaction tank |
| CN210385842U (en) * | 2019-07-05 | 2020-04-24 | 鹤壁宝来化工科技有限公司 | Chemical industry reation kettle that stirring effect is good |
| CN211070063U (en) * | 2019-07-25 | 2020-07-24 | 四川盛年同缔实业有限公司 | Petrochemical reation kettle |
| CN211514304U (en) * | 2019-12-26 | 2020-09-18 | 东联北方科技(北京)有限公司 | Adhesive stirring equipment |
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Application publication date: 20210525 |