CN110668993A - Production device and method of pesticide intermediate 1,2,3, 6-tetrahydrophthalimide - Google Patents
Production device and method of pesticide intermediate 1,2,3, 6-tetrahydrophthalimide Download PDFInfo
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- CN110668993A CN110668993A CN201911075863.4A CN201911075863A CN110668993A CN 110668993 A CN110668993 A CN 110668993A CN 201911075863 A CN201911075863 A CN 201911075863A CN 110668993 A CN110668993 A CN 110668993A
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- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D209/00—Heterocyclic compounds containing five-membered rings, condensed with other rings, with one nitrogen atom as the only ring hetero atom
- C07D209/02—Heterocyclic compounds containing five-membered rings, condensed with other rings, with one nitrogen atom as the only ring hetero atom condensed with one carbocyclic ring
- C07D209/44—Iso-indoles; Hydrogenated iso-indoles
- C07D209/48—Iso-indoles; Hydrogenated iso-indoles with oxygen atoms in positions 1 and 3, e.g. phthalimide
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Abstract
The invention provides a production device and a method of a pesticide intermediate 1,2,3, 6-tetrahydrophthalimide; the production method comprises the following steps: according to the production device adopting the technical scheme, phthalic anhydride and an ammonia source are mixed and then subjected to low-temperature reaction, the obtained reaction product is continuously conveyed to a dehydration ring-closing reaction device for dehydration ring-closing reaction, and finally the obtained molten product is cooled and sliced to obtain the pesticide intermediate 1,2,3, 6-tetrahydrophthalimide. Compared with the prior art, the production method provided by the invention is realized by the production device with a specific structure and a connection relation, has the advantages of simple process, short reaction retention time and the like, can realize continuous production, controls the whole flow and saves labor; and the low-temperature reaction and the dehydration ring-closing reaction are completely separated, so that the back mixing of water and phthalic anhydride is avoided, the side reaction is less, no waste water is generated, and the product purity and the yield are improved.
Description
Technical Field
The invention relates to the technical field of organic chemical synthesis, in particular to a device and a method for producing a pesticide intermediate 1,2,3, 6-tetrahydrophthalimide.
Background
1,2,3, 6-tetrahydrophthalimide is a chemical product and is mainly used for organic synthesis of pesticide intermediates and the like. At present, a chinese patent with publication number CN208430066U discloses a device for preparing captan, wherein the first mixing device is provided with a phthalic anhydride inlet and an ammonia water inlet; under the direct contact of phthalic anhydride and ammonia water, the phthalic anhydride and water can be hydrolyzed, so that side reaction is caused, and a large amount of wastewater can be generated; moreover, the device for producing the product has the defects of complicated process steps, long reaction retention time and difficulty in realizing continuous production.
Disclosure of Invention
In view of the above, the invention aims to provide a device and a method for producing a pesticide intermediate 1,2,3, 6-tetrahydrophthalimide, and the production method provided by the invention has the advantages of simple process, short reaction retention time, capability of realizing continuous production, avoidance of back mixing of water and phthalic anhydride, less side reaction and no wastewater, thereby improving the purity and yield of the product.
The invention provides a production device of a pesticide intermediate 1,2,3, 6-tetrahydrophthalimide, which comprises the following components:
a low temperature reaction device; the low-temperature reaction device is provided with a phthalic anhydride inlet, an ammonia source inlet and a discharge hole;
the feeding stranding cage is connected with the feeding hole of the low-temperature reaction device; the feeding stranding cage is provided with a discharge hole;
the feed inlet is connected with the discharge outlet of the feeding stranding cage; the dehydration closed-loop reaction device is provided with a steam outlet and a discharge hole;
and the feed inlet is connected with the discharge outlet of the dehydration closed-loop reaction device.
Preferably, the low temperature reaction device comprises a plurality of high viscosity reactors connected in series.
Preferably, the phthalic anhydride inlet is provided with a first weighing device; and a second weighing device is arranged at the ammonia source inlet.
Preferably, the dehydration closed-loop reaction device comprises a plurality of reaction kettles connected in series.
The invention also provides a production method of the pesticide intermediate 1,2,3, 6-tetrahydrophthalimide, which comprises the following steps:
according to the production device adopting the technical scheme, phthalic anhydride and an ammonia source are mixed and then subjected to low-temperature reaction, the obtained reaction product is continuously conveyed to a dehydration ring-closing reaction device for dehydration ring-closing reaction, and finally the obtained molten product is cooled and sliced to obtain the pesticide intermediate 1,2,3, 6-tetrahydrophthalimide.
Preferably, the ammonia source is selected from ammonia gas or ammonium bicarbonate.
Preferably, the molar ratio of the phthalic anhydride to the ammonia source is 1: (1-1.5).
Preferably, the process of mixing phthalic anhydride and an ammonia source and then carrying out a low-temperature reaction specifically comprises the following steps:
adding phthalic anhydride into a low-temperature reaction device, keeping the temperature at 0-30 ℃, adding an ammonia source under the stirring condition of the rotating speed of 60-120 r/min, and reacting for 10-20 min to obtain a reaction product.
Preferably, the temperature of the dehydration ring-closing reaction is 130-180 ℃, and the time is 110-150 min.
The invention provides a production device and a method of a pesticide intermediate 1,2,3, 6-tetrahydrophthalimide; the production method comprises the following steps: according to the production device adopting the technical scheme, phthalic anhydride and an ammonia source are mixed and then subjected to low-temperature reaction, the obtained reaction product is continuously conveyed to a dehydration ring-closing reaction device for dehydration ring-closing reaction, and finally the obtained molten product is cooled and sliced to obtain the pesticide intermediate 1,2,3, 6-tetrahydrophthalimide. Compared with the prior art, the production method provided by the invention is realized by the production device with a specific structure and a connection relation, has the advantages of simple process, short reaction retention time and the like, can realize continuous production, controls the whole flow and saves labor; and the low-temperature reaction and the dehydration ring-closing reaction are completely separated, so that the back mixing of water and phthalic anhydride is avoided, the side reaction is less, no waste water is generated, and the product purity and the yield are improved.
Drawings
Fig. 1 is a schematic structural diagram of a production apparatus for a pesticide intermediate 1,2,3, 6-tetrahydrophthalimide provided by an embodiment of the present invention;
fig. 2 is a schematic structural diagram of a production apparatus for a pesticide intermediate 1,2,3, 6-tetrahydrophthalimide provided in embodiment 1 of the present invention.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a production device of a pesticide intermediate 1,2,3, 6-tetrahydrophthalimide, which comprises the following components:
a low temperature reaction device; the low-temperature reaction device is provided with a phthalic anhydride inlet, an ammonia source inlet and a discharge hole;
the feeding stranding cage is connected with the feeding hole of the low-temperature reaction device; the feeding stranding cage is provided with a discharge hole;
the feed inlet is connected with the discharge outlet of the feeding stranding cage; the dehydration closed-loop reaction device is provided with a steam outlet and a discharge hole;
and the feed inlet is connected with the discharge outlet of the dehydration closed-loop reaction device.
Referring to fig. 1, fig. 1 is a schematic structural diagram of a production apparatus for a pesticide intermediate 1,2,3, 6-tetrahydrophthalimide according to an embodiment of the present invention; wherein, 1 is low temperature reaction unit, 2 is the phthalic anhydride import, 3 is the import of ammonia source, 4 is low temperature reaction unit's discharge gate, 5 is the feed inlet of feeding hank cage, 6 is the feeding hank cage, 7 is the discharge gate of feeding hank cage, 8 is the feed inlet of dehydration closed loop reaction unit, 9 is dehydration closed loop reaction unit, 10 is steam outlet, 11 is the discharge gate of dehydration closed loop reaction unit, 12 is the feed inlet of slicer, 13 is the slicer, 14 is first weighing device, 15 is the second weighing device.
In the present invention, the low-temperature reaction apparatus (1) is used for mixing phthalic anhydride and an ammonia source and further performing a low-temperature reaction. In the invention, the low-temperature reaction device (1) is provided with a phthalic anhydride inlet (2), an ammonia source inlet (3) and a discharge hole (4). Wherein the phthalic anhydride inlet (2) is used for conveying raw material phthalic anhydride into the low-temperature reaction device (1); the phthalic anhydride inlet (2) is preferably provided with a first weighing device (14) for weighing raw material phthalic anhydride; the first weighing device (14) is preferably a weightless scale. In the present invention, the phthalic anhydride inlet (2) is preferably connected to a silo for storing phthalic anhydride.
In the invention, the ammonia source inlet (3) is used for conveying a raw material ammonia source into the low-temperature reaction device (1); the ammonia source inlet (3) is preferably provided with a second weighing device (15) for weighing the raw material ammonia source; the second weighing means (15) is preferably a loss-in-weight scale or a flow meter. In a preferred embodiment of the invention, the ammonia source inlet (3) is preferably connected with a storage bin for storing ammonium bicarbonate as the ammonia source, and the second weighing device (15) is a weightless scale; in another preferred embodiment of the invention, the ammonia source inlet (3) is preferably connected to an ammonia gas delivery line as ammonia source, and the second weighing device (15) is a flow meter.
In the invention, the discharge port (4) is used for discharging reaction products obtained in the low-temperature reaction device (1).
In the present invention, the low temperature reaction apparatus (1) preferably comprises several high viscosity reactors connected in series, more preferably two high viscosity reactors connected in series. The high-viscosity reactor can realize strong mixing of raw materials.
In the invention, the feeding stranding cage (6) is used for continuously conveying the reaction product discharged from the low-temperature reaction device (1) into a dehydration closed-loop reaction device (9). In the invention, the feeding stranding cage (6) is provided with a feeding hole (5) and a discharging hole (7); the feeding hole (5) is connected with the discharging hole (4) of the low-temperature reaction device (1), and the discharging hole (7) is connected with the feeding hole (8) of the dehydration closed-loop reaction device (9).
In the invention, the dehydration ring-closure reaction device (9) is used for performing dehydration ring-closure reaction to obtain a dehydrated molten product 1,2,3, 6-tetrahydrophthalimide. In the invention, the dehydration closed-loop reaction device (9) is provided with a feed inlet (8), a steam outlet (10) and a discharge outlet (11); wherein the feed inlet (8) is connected with a discharge hole (7) of the feed stranding cage (6); the steam outlet (10) is used for continuously discharging water vapor removed in the reaction process; the discharge hole (11) is connected with the feed inlet (12) of the slicing machine (13).
In the invention, the dehydration closed-loop reaction device (9) preferably comprises a plurality of reaction kettles connected in series, more preferably two reaction kettles connected in series; the reaction kettle can be provided with a vacuum environment, and is favorable for the dehydration process.
In the invention, the slicing machine (13) is used for cooling and slicing the molten product obtained by the dehydration closed-loop reaction device (9) to obtain a product.
The production device provided by the invention adopts a specific structure and a connection relation, can realize continuous production, controls the whole flow and saves labor; and the low-temperature reaction and the dehydration ring-closing reaction are completely separated, so that the back mixing of water and phthalic anhydride is avoided, the side reaction is less, no waste water is generated, and the product purity and the yield are improved.
The invention also provides a production method of the pesticide intermediate 1,2,3, 6-tetrahydrophthalimide, which comprises the following steps:
according to the production device adopting the technical scheme, phthalic anhydride and an ammonia source are mixed and then subjected to low-temperature reaction, the obtained reaction product is continuously conveyed to a dehydration ring-closing reaction device for dehydration ring-closing reaction, and finally the obtained molten product is cooled and sliced to obtain the pesticide intermediate 1,2,3, 6-tetrahydrophthalimide.
According to the production device adopting the technical scheme, firstly, the phthalic anhydride and the ammonia source are mixed and then subjected to low-temperature reaction. In the present invention, the purity of the phthalic anhydride (phthalic anhydride) is preferably 99.5% or more. In the present invention, the ammonia source is preferably selected from ammonia gas or ammonium bicarbonate; the purity of the ammonia gas is preferably 99% or more. The present invention is not particularly limited with respect to the sources of the phthalic anhydride and the ammonia source, and commercially available products well known to those skilled in the art may be used.
In the present invention, the molar ratio of the phthalic anhydride to the ammonia source is preferably 1: (1 to 1.5), more preferably 1: (1.2-1.3).
In the invention, the preferable process of mixing the phthalic anhydride and the ammonia source and then carrying out the low-temperature reaction is as follows:
adding phthalic anhydride into a low-temperature reaction device, keeping the temperature at 0-30 ℃, adding an ammonia source under the stirring condition of the rotating speed of 60-120 r/min, and reacting for 10-20 min to obtain a reaction product;
more preferably:
adding phthalic anhydride into a low-temperature reaction device, keeping the temperature at 10-20 ℃, adding an ammonia source under the stirring condition of the rotating speed of 100-110 r/min, and reacting for 10-20 min to obtain a reaction product.
After the low-temperature reaction is finished, the obtained reaction product is continuously conveyed to a dehydration closed-loop reaction device to carry out dehydration closed-loop reaction. In the invention, the continuous conveying process is realized by a feeding stranding cage.
In the invention, the temperature of the dehydration ring-closing reaction is preferably 130-180 ℃, and more preferably 145-150 ℃; the time of the dehydration ring-closure reaction is preferably 110min to 150min, and more preferably 110min to 130 min.
After the dehydration ring-closure reaction is finished, the obtained molten product is cooled and sliced to obtain the pesticide intermediate 1,2,3, 6-tetrahydrophthalimide.
The production method provided by the invention is realized by the production device with a specific structure and a connection relation, has the advantages of simple process, short reaction retention time and the like, can realize continuous production, controls the full flow and saves labor; and the low-temperature reaction and the dehydration ring-closing reaction are completely separated, so that the back mixing of water and phthalic anhydride is avoided, the side reaction is less, no waste water is generated, and the product purity and the yield are improved.
The invention provides a production device and a method of a pesticide intermediate 1,2,3, 6-tetrahydrophthalimide; the production method comprises the following steps: according to the production device adopting the technical scheme, phthalic anhydride and an ammonia source are mixed and then subjected to low-temperature reaction, the obtained reaction product is continuously conveyed to a dehydration ring-closing reaction device for dehydration ring-closing reaction, and finally the obtained molten product is cooled and sliced to obtain the pesticide intermediate 1,2,3, 6-tetrahydrophthalimide. Compared with the prior art, the production method provided by the invention is realized by the production device with a specific structure and a connection relation, has the advantages of simple process, short reaction retention time and the like, can realize continuous production, controls the whole flow and saves labor; and the low-temperature reaction and the dehydration ring-closing reaction are completely separated, so that the back mixing of water and phthalic anhydride is avoided, the side reaction is less, no waste water is generated, and the product purity and the yield are improved.
To further illustrate the present invention, the following examples are provided for illustration. The raw materials used in the following examples of the present invention are all commercially available products, wherein the purity of phthalic anhydride is 99.5% and the purity of ammonia gas is 99%.
Example 1
The schematic structural diagram of the production device of the pesticide intermediate 1,2,3, 6-tetrahydrophthalimide provided in embodiment 1 of the present invention is shown in fig. 2.
The production method comprises the following steps:
according to the molar ratio of phthalic anhydride to ammonia gas of 1: 1.3, feeding phthalic anhydride into a low-temperature reaction device at the speed of 150kg/h, introducing ammonia gas at the speed of 22kg/h, controlling the temperature to be 13-18 ℃, stirring at the speed of 100r/min, and staying for 15 min; transferring the reaction product (solid material) into a dehydration closed-loop reaction device through a feeding stranding cage, preserving heat at 145 ℃, keeping the temperature for 120min, discharging water vapor in time in the process to obtain a molten product, cooling the obtained molten product, entering a slicing machine for slicing, and obtaining 146.2kg of product one hour after stabilization.
The detection proves that the purity of the imine is 98.7 percent, and the yield is 97.6 percent.
Example 2
With the production apparatus in example 1, the production method was as follows:
according to the molar ratio of phthalic anhydride to ammonia gas of 1: 1.2 feeding, namely feeding phthalic anhydride into a low-temperature reaction device at the speed of 150kg/h, introducing ammonia gas at the speed of 20kg/h, controlling the temperature to be 13-18 ℃, stirring at the speed of 100r/min, and standing for 15min, transferring a reaction product (solid material) into a dehydration closed-loop reaction device through a feeding stranding cage, preserving heat at the temperature of 150 ℃ for 110min, discharging water vapor in time in the process to obtain a molten product, cooling the obtained molten product, feeding the cooled molten product into a slicing machine for slicing, and obtaining 145.0kg of a product after stabilizing for one hour.
The detection proves that the purity of the imine is 98.4 percent, and the yield is 97.3 percent.
Example 3
The production apparatus in example 1 was used, with the difference that: changing an ammonia gas inlet into an ammonium bicarbonate inlet, and adding an ammonium bicarbonate bin and a weight loss scale; the production method comprises the following steps:
according to the molar ratio of phthalic anhydride to ammonium bicarbonate of 1: 1.3 feeding, namely feeding phthalic anhydride into a low-temperature reaction device at the speed of 150kg/h, controlling the temperature to be 13-18 ℃, feeding ammonium bicarbonate at the speed of 78kg/h, stirring at the speed of 110r/min, standing for 20min, transferring a reaction product (solid material) into a dehydration closed-loop reaction device through a feeding stranding cage, preserving heat at the temperature of 150 ℃ for 130min, discharging water vapor in time during the process to obtain a molten product, cooling the obtained molten product, feeding the cooled molten product into a slicing machine for slicing, and obtaining 145.5kg of a product after stabilizing for one hour.
The detection proves that the purity of the imine is 98.0 percent, and the yield is 96.6 percent.
Example 4
The production apparatus in example 1 was used, with the difference that: changing an ammonia gas inlet into an ammonium bicarbonate inlet, and adding an ammonium bicarbonate bin and a weight loss scale; the production method comprises the following steps:
according to the molar ratio of phthalic anhydride to ammonium bicarbonate of 1: 1.3 feeding, namely feeding phthalic anhydride into a low-temperature reaction device at the speed of 150kg/h, controlling the temperature to be 0-5 ℃, feeding ammonium bicarbonate at the speed of 78kg/h, stirring at the speed of 110r/min, standing for 20min, transferring a reaction product (solid material) into a dehydration closed-loop reaction device through a feeding stranding cage, preserving heat at the temperature of 150 ℃ for 130min, discharging water vapor in time in the process to obtain a molten product, cooling the obtained molten product, feeding the cooled molten product into a slicing machine for slicing, and obtaining 144.3kg of a product after stabilizing for one hour.
The detection proves that the imine purity is 97.6 percent, and the yield is 96.2 percent.
Example 5
The production apparatus in example 1 was used, with the difference that: changing an ammonia gas inlet into an ammonium bicarbonate inlet, and adding an ammonium bicarbonate bin and a weight loss scale; the production method comprises the following steps:
according to the molar ratio of phthalic anhydride to ammonium bicarbonate of 1: 1.3 feeding, namely feeding phthalic anhydride into a low-temperature reaction device at the speed of 150kg/h, controlling the temperature to be 6-12 ℃, feeding ammonium bicarbonate at the speed of 78kg/h, stirring at the speed of 110r/min, standing for 20min, transferring a reaction product (solid material) into a dehydration closed-loop reaction device through a feeding stranding cage, preserving heat at the temperature of 150 ℃ for 130min, discharging water vapor in time during the process to obtain a molten product, cooling the obtained molten product, feeding the cooled molten product into a slicing machine for slicing, and obtaining 145.2kg of a product after stabilizing for one hour.
The detection proves that the purity of the imine is 97.8 percent, and the yield is 96.8 percent.
Example 6
The production apparatus in example 1 was used, with the difference that: changing an ammonia gas inlet into an ammonium bicarbonate inlet, and adding an ammonium bicarbonate bin and a weight loss scale; the production method comprises the following steps:
according to the molar ratio of phthalic anhydride to ammonium bicarbonate of 1: 1.3 feeding, namely feeding phthalic anhydride into a low-temperature reaction device at the speed of 150kg/h, controlling the temperature to be 19-25 ℃, feeding ammonium bicarbonate at the speed of 78kg/h, stirring at the speed of 110r/min, standing for 20min, transferring a reaction product (solid material) into a dehydration closed-loop reaction device through a feeding stranding cage, preserving heat at the temperature of 150 ℃ for 130min, discharging water vapor in time during the process to obtain a molten product, cooling the obtained molten product, feeding the cooled molten product into a slicing machine for slicing, and obtaining 144.4kg of a product after stabilizing for one hour.
The detection proves that the imine purity is 96.8 percent, and the yield is 96.3 percent.
Example 7
The production apparatus in example 1 was used, with the difference that: changing an ammonia gas inlet into an ammonium bicarbonate inlet, and adding an ammonium bicarbonate bin and a weight loss scale; the production method comprises the following steps:
according to the molar ratio of phthalic anhydride to ammonium bicarbonate of 1: 1.3 feeding, namely feeding phthalic anhydride into a low-temperature reaction device at the speed of 150kg/h, controlling the temperature to be 26-30 ℃, feeding ammonium bicarbonate at the speed of 78kg/h, stirring at the speed of 110r/min, standing for 20min, transferring a reaction product (solid material) into a dehydration closed-loop reaction device through a feeding stranding cage, preserving heat at the temperature of 150 ℃ for 130min, discharging water vapor in time in the process to obtain a molten product, cooling the obtained molten product, then feeding the cooled molten product into a slicing machine for slicing, and obtaining 143.7kg of a product after stabilizing for one hour.
The detection proves that the imine purity is 96.5 percent, and the yield is 95.8 percent.
Comparative example 1
The kettle type batch method is adopted for production, and the molar ratio of phthalic anhydride to ammonia gas is 1: 1.3, feeding 150kg of phthalic anhydride into a 500L reaction kettle, cooling the system to below 20 ℃, introducing ammonia gas, controlling the temperature to be 13-18 ℃, introducing 22kg of ammonia gas, reacting for 15min at a stirring speed of 100r/min, heating to 145 ℃, keeping the temperature for 120min, discharging water vapor in time in the process to obtain a molten product, cooling, and feeding the molten product into a slicer to obtain 146.23kg of a product.
The detection proves that the purity of the imine is 97.1 percent, and the yield is 96.2 percent.
Compared with the batch method, the production method provided by the embodiments 1 to 7 of the invention can realize continuous production, has simple process steps and operation, and has higher imine purity and yield than the batch method, thereby being more labor-saving, safe and environment-friendly.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (9)
1. An apparatus for producing a pesticide intermediate 1,2,3, 6-tetrahydrophthalimide, comprising:
a low temperature reaction device; the low-temperature reaction device is provided with a phthalic anhydride inlet, an ammonia source inlet and a discharge hole;
the feeding stranding cage is connected with the feeding hole of the low-temperature reaction device; the feeding stranding cage is provided with a discharge hole;
the feed inlet is connected with the discharge outlet of the feeding stranding cage; the dehydration closed-loop reaction device is provided with a steam outlet and a discharge hole;
and the feed inlet is connected with the discharge outlet of the dehydration closed-loop reaction device.
2. The production plant according to claim 1, wherein the low temperature reaction unit comprises several high viscosity reactors in series.
3. The production device according to claim 1, wherein the phthalic anhydride inlet is provided with a first weighing device; and a second weighing device is arranged at the ammonia source inlet.
4. The production device according to claim 1, wherein the dehydration closed-loop reaction device comprises a plurality of reaction kettles connected in series.
5. A production method of a pesticide intermediate 1,2,3, 6-tetrahydrophthalimide comprises the following steps:
the production device of any one of claims 1 to 4 is adopted, phthalic anhydride and an ammonia source are mixed and then subjected to low-temperature reaction, the obtained reaction product is continuously conveyed to a dehydration ring-closure reaction device for dehydration ring-closure reaction, and finally the obtained molten product is cooled and sliced to obtain the pesticide intermediate 1,2,3, 6-tetrahydrophthalimide.
6. The production method according to claim 5, wherein the ammonia source is selected from ammonia gas or ammonium bicarbonate.
7. The process according to claim 5, wherein the molar ratio of the phthalic anhydride to the ammonia source is 1: (1-1.5).
8. The production method according to claim 5, wherein the low-temperature reaction after mixing the phthalic anhydride and the ammonia source is specifically carried out by:
adding phthalic anhydride into a low-temperature reaction device, keeping the temperature at 0-30 ℃, adding an ammonia source under the stirring condition of the rotating speed of 60-120 r/min, and reacting for 10-20 min to obtain a reaction product.
9. The production method according to claim 5, wherein the temperature of the dehydration ring-closing reaction is 130 to 180 ℃ and the time is 110 to 150 min.
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| CN201911075863.4A CN110668993A (en) | 2019-11-06 | 2019-11-06 | Production device and method of pesticide intermediate 1,2,3, 6-tetrahydrophthalimide |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115353481A (en) * | 2022-08-31 | 2022-11-18 | 宁夏格瑞精细化工有限公司 | Catalytic synthesis method of cis-1, 2,3, 6-tetrahydrophthalimide |
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| CN208430066U (en) * | 2018-05-31 | 2019-01-25 | 宁夏格瑞精细化工有限公司 | A kind of device preparing captan |
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| CN115353481A (en) * | 2022-08-31 | 2022-11-18 | 宁夏格瑞精细化工有限公司 | Catalytic synthesis method of cis-1, 2,3, 6-tetrahydrophthalimide |
| CN115353481B (en) * | 2022-08-31 | 2024-03-29 | 宁夏格瑞精细化工有限公司 | Catalytic synthesis method of cis-1, 2,3, 6-tetrahydrophthalimide |
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