Production system for bronopol refining

Abstract

The utility model relates to the technical field of bronopol production, in particular to a production system for bronopol refining, which comprises a crude product dissolving kettle, a discharge port of the crude product dissolving kettle is communicated with an extraction kettle, an organic phase outlet of the extraction kettle is communicated with a first impurity removal device, and a discharge port of the first impurity removal device is communicated with a second impurity removal device. A feed port of the second impurity removal device is communicated with an eluent conveying pipeline, an eluent outlet of the second impurity removal device is communicated with a buffer kettle, a discharge port of the buffer kettle is communicated with a distillation kettle, a discharge port of the distillation kettle is communicated with a drying device, and a discharge port of the drying device is communicated with a product storage tank. The production system is reasonable in design, part of impurities can be removed through extraction treatment of the extraction kettle, then pigments, small molecular impurities and metal ions can be removed through treatment of the first impurity removal device, the impurities can be further separated and removed through treatment of the second impurity removal device, and the purity of bronopol products is greatly improved.

Description

Technical Field

[0001] This utility model relates to the field of bromonitrile production technology, and in particular to a production system for the purification of bromonitrile. Background Technology

[0002] Brominnitrophenol is a novel bactericide and preservative, primarily used in cosmetics and leather preservation. It is also used as a bactericide in agriculture and medicine. Furthermore, it is a broad-spectrum and highly effective industrial bactericide used to prevent the growth and reproduction of bacteria and algae in papermaking, industrial circulating cooling water, metalworking lubricants, pulp, wood, coatings, and plywood, and is widely used in paper mill pulp and circulating cooling water systems. Currently, industrially, nitromethane, formaldehyde, and bromine are mainly used as raw materials. Crude brominnitrophenol is obtained through carbonyl methylation, bromination, and neutralization separation, followed by crystallization to obtain purified brominnitrophenol. However, the product obtained through crystallization contains some impurities and has relatively low purity. Therefore, to address these issues, it is necessary to develop a production system for the purification of brominnitrophenol. Utility Model Content

[0003] The technical problem to be solved by this utility model is to provide a production system for the purification of bromonitroethanol, which greatly improves the purity of bromonitroethanol, in order to address the shortcomings of the existing technology.

[0004] To solve the above-mentioned technical problems, the technical solution of this utility model is as follows:

[0005] A production system for the purification of bromonitrile includes a crude product dissolving vessel, the outlet of which is connected to an extraction vessel, the organic phase outlet of which is connected to a first impurity removal device, the outlet of which is connected to a second impurity removal device, the inlet of which is connected to an eluent delivery pipeline, the eluent outlet of which is connected to a buffer vessel, the outlet of which is connected to a distillation vessel, the outlet of which is connected to a drying device, and the outlet of which is connected to a product storage tank.

[0006] As an improved technical solution, the extraction vessel includes a vessel body, the top of which is provided with a feed inlet and an extractant inlet, the bottom and upper side of which are respectively provided with an aqueous phase outlet and an organic phase outlet, the outside of which is provided with a jacket, the vessel body is provided with a sight glass window, the inside of which is provided with a stirring shaft, one end of which is connected to a motor, and the stirring shaft is provided with multiple hollowed-out arc-shaped stirring plates.

[0007] As an improved technical solution, the first impurity removal device includes a body, with an inlet and an outlet at the top and bottom of the body, respectively. The interior of the body is provided with an activated carbon adsorption layer, a resin adsorption layer and an activated alumina adsorption layer from top to bottom.

[0008] As an improved technical solution, the second impurity removal device includes a body, the top of which is provided with a feed inlet and an eluent inlet, the bottom of which is provided with a liquid outlet and an eluent outlet, and the interior of which is provided with a silica gel adsorption layer.

[0009] As an improved technical solution, the distillation vessel includes a vessel body, the top of which is provided with a feed inlet and an vent, the bottom of which is provided with a discharge outlet, the exterior of which is provided with a jacket, and the interior of which is provided with a stirring shaft. One end of the stirring shaft is connected to a motor, and the stirring shaft is provided with multiple stirring rods, and the stirring rods are provided with multiple arc-shaped plates.

[0010] As an improved technical solution, the vent is connected to a condenser, and the condensate outlet of the condenser is connected to an organic solvent storage tank.

[0011] After adopting the above technical solution, the beneficial effects of this utility model are:

[0012] The production system for bromonitrile purification includes a crude product dissolving vessel, the outlet of which is connected to an extraction vessel, the organic phase outlet of which is connected to a first impurity removal device, the outlet of which is connected to a second impurity removal device, the inlet of which is connected to an eluent delivery pipeline, the eluent outlet of which is connected to a buffer vessel, the outlet of which is connected to a distillation vessel, the outlet of which is connected to a drying device, and the outlet of which is connected to a product storage tank. In actual production, the prepared crude bromonitol is added to a crude product dissolving vessel, dissolved with water and stirred, and then pumped to the extraction vessel. An extractant is then added, and after extraction, the organic phase containing bromonitol is collected. This organic phase is then pumped to the first impurity removal device. The purified liquid is then pumped to the second impurity removal device. After impurity removal, the bromonitol adsorbed in the second device is eluted with an eluent. The collected eluent is pumped to a buffer vessel, and then to a distillation vessel. After distillation, the organic solvent is removed, and the eluent is then pumped to a drying device. The dried bromonitol is stored in a product storage tank. This production system is rationally designed. The extraction process in the extraction vessel removes some impurities. The first impurity removal device removes pigments, small molecule impurities, and metal ions. The second impurity removal device further separates and removes impurities, significantly improving the purity of the bromonitol product.

[0013] The extraction vessel consists of a vessel body with a feed inlet and an extractant inlet at the top, and an aqueous phase outlet and an organic phase outlet at the bottom and upper side, respectively. The vessel body is fitted with a jacket and has a sight glass window. Inside the vessel body is a stirring shaft, one end of which is connected to a motor. The stirring shaft has multiple perforated arc-shaped stirring plates. In actual production, the crude bromonitrol solution enters the vessel body, followed by the addition of the extractant (ethyl acetate or dichloromethane). After the motor starts, it drives the stirring shaft and multiple stirring plates to rotate, achieving mixing of the solution and extractant. The heat transfer medium in the jacket provides the necessary temperature for extraction. After extraction, the mixture is allowed to settle and separate into layers. The upper organic phase is discharged from the organic phase outlet and enters the next processing equipment. This extraction vessel structure is rationally designed, greatly improving extraction efficiency and achieving preliminary separation of bromonitrol and impurities.

[0014] The first impurity removal device comprises a main body with an inlet at the top and an outlet at the bottom. Inside the main body, from top to bottom, are sequentially arranged an activated carbon adsorption layer, a resin adsorption layer, and an activated alumina adsorption layer. When the organic phase containing bromonitroethanol enters the main body, the activated carbon adsorption layer removes pigments and small molecule impurities, the resin adsorption layer removes charged impurity ions, and the activated alumina adsorption layer removes impurities containing polar groups such as hydroxyl and carboxyl groups, as well as metal ions, significantly improving the purity of bromonitroethanol.

[0015] The second impurity removal device comprises a main body with a feed inlet and eluent inlet at the top, and a liquid outlet and eluent outlet at the bottom. The interior of the main body contains a silica gel adsorption layer. The bromonitroethanol solution, after impurity removal by the first device, enters the main body. As it passes through the silica gel adsorption layer, the bromonitroethanol is adsorbed, while impurities flow out through the layer. The bromonitroethanol is then eluted using an eluent. This second impurity removal device is rationally designed, achieving further separation of bromonitroethanol and impurities, significantly improving the purity of the bromonitroethanol.

[0016] The distillation vessel comprises a vessel body with an inlet and an outlet at the top, a outlet at the bottom, and a jacket around the body. Inside the vessel body is a stirring shaft connected to a motor, with multiple stirring rods and arc-shaped plates mounted on them. The eluent enters the vessel body and is heated by a heat transfer medium in the jacket. The motor drives the stirring shaft, stirring rods, and arc-shaped plates to agitate the eluent, ensuring uniform heating. The distilled organic solvent is discharged through the outlet. This distillation vessel design is efficient and significantly improves distillation efficiency, facilitating the removal of organic solvents from bromonitroethanol feed solutions.

[0017] Because the vent is connected to the condenser, and the condensate outlet of the condenser is connected to the organic solvent storage tank, the organic solvent vapor, after being heated and distilled, is discharged from the vent and enters the condenser. The condensed organic solvent is then stored as an organic solvent, thus achieving the recycling of organic solvents. Attached Figure Description

[0018] Figure 1 This is a schematic diagram of the production system for the purification of bromonitroethanol according to this utility model;

[0019] Among them, 1-crude product dissolving vessel, 2-extraction vessel, 20-sight window, 21-stirring shaft, 22-motor, 23-arc-shaped stirring plate, 3-first impurity removal device, 30-activated carbon adsorption layer, 31-resin adsorption layer, 32-activated alumina adsorption layer, 4-second impurity removal device, 40-silica gel adsorption layer, 5-eluent conveying pipeline, 6-buffer vessel, 7-distillation vessel, 70-drain port, 71-stirring rod, 72-arc-shaped plate, 8-drying device, 9-product storage tank, 10-condenser, 11-organic solvent storage tank. Detailed Implementation

[0020] To make the objectives, technical solutions, and advantages of this utility model clearer, the present utility model will be further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the present utility model and are not intended to limit the present utility model.

[0021] A production system for the purification of bromonitroethanol, such as Figure 1 As shown, the system includes a crude product dissolving vessel 1, the outlet of which is connected to an extraction vessel 2. The organic phase outlet of the extraction vessel 2 is connected to a first impurity removal device 3. The outlet of the first impurity removal device 3 is connected to a second impurity removal device 4. The inlet of the second impurity removal device 4 is connected to an eluent delivery pipeline 5. The eluent outlet of the second impurity removal device 4 is connected to a buffer vessel 6. The outlet of the buffer vessel 6 is connected to a distillation vessel 7. The outlet of the distillation vessel 7 is connected to a drying device 8 (double cone dryer). The outlet of the drying device 8 is connected to a product storage tank 9. The first impurity removal device 3 includes a main body with an inlet and an outlet at the top and bottom, respectively. The interior of the main body, from top to bottom, consists of an activated carbon adsorption layer 30, a resin adsorption layer 31 (strong acid cation exchange resin), and an activated alumina adsorption layer 31. The second impurity removal device 4 includes a main body with an inlet and an eluent inlet at the top and an outlet and an eluent outlet at the bottom. The interior of the main body contains a silica gel adsorption layer 40.

[0022] In actual production, the prepared crude bromonitol is added to a crude product dissolving vessel, water is added and stirred to dissolve it, and then it is pumped to the interior of an extraction vessel. An extractant is then added, and after extraction, the organic phase containing bromonitol is collected. This phase is then pumped to the first impurity removal device via a resin transfer pump. After treatment with an activated carbon adsorption layer, pigments and small molecule impurities are removed. After treatment with a resin adsorption layer, charged impurity ions are removed. After treatment with an activated oxychloride-aluminum adsorption layer, impurities containing polar groups such as hydroxyl and carboxyl groups, as well as metal ions, are removed, significantly improving the purity of the bromonitol. The purified liquid is then pumped into the second impurity removal device. When passing through a silica gel adsorption layer, bromonitol is adsorbed, while impurities flow out through the silica gel. An eluent is then used to elute the bromonitol adsorbed on the silica gel. The collected eluent is pumped to a buffer vessel, and then to a distillation vessel. After distillation, the organic solvent is evaporated, and the eluent is then pumped to the interior of a drying device. The dried bromonitol is stored in a product storage tank. The above-mentioned production system is reasonably designed. Through the extraction process in the extraction vessel, some impurities can be removed. Then, after the first impurity removal device, pigments, small molecule impurities, and metal ions can be removed. Through the second impurity removal device, impurities can be further separated and removed, which greatly improves the purity of the bromonitrol product.

[0023] The extraction vessel 2 includes a vessel body with a feed inlet and an extractant inlet at the top. The bottom and upper side of the vessel body have aqueous phase outlets and organic phase outlets, respectively. The vessel body is fitted with a jacket and has a sight glass window 20. Inside the vessel body is a stirring shaft 21, one end of which is connected to a motor 22. Multiple perforated arc-shaped stirring plates 23 (fixed to the stirring shaft by mounting brackets) are mounted on the stirring shaft 21. In actual production, the crude bromonitrol solution enters the vessel body, followed by the addition of the extractant (ethyl acetate or dichloromethane). After the motor starts, it drives the stirring shaft and multiple stirring plates to rotate, achieving mixing of the solution and extractant. The heat transfer medium in the jacket provides the necessary temperature for extraction. After extraction, the mixture is allowed to settle and separate into layers. The upper organic phase is discharged from the organic phase outlet and enters the next processing equipment. This extraction vessel structure is rationally designed, greatly improving extraction efficiency and achieving preliminary separation of bromonitrol and impurities.

[0024] The distillation vessel 7 includes a vessel body with an inlet and an outlet 70 at the top and an outlet at the bottom. The vessel body is fitted with a jacket, and an agitator shaft is installed inside. One end of the agitator shaft is connected to a motor, and multiple agitator rods 71 ​​and multiple arc-shaped plates 72 are mounted on the shaft. The eluent enters the vessel body and is heated by a heat transfer medium in the jacket. The motor starts, driving the agitator shaft, multiple agitator rods, and arc-shaped plates to agitate the eluent, ensuring uniform heating. The distilled organic solvent is discharged from the outlet.

[0025] The vent 70 is connected to the condenser 10, and the condensate outlet of the condenser 10 is connected to the organic solvent storage tank 11. The organic solvent vapor after heating and distillation is discharged from the vent and enters the condenser. The condensed organic solvent is stored as an organic solvent, realizing the recycling of organic solvent.

[0026] The above description is only a preferred embodiment of the present utility model and is not intended to limit the present utility model. Any modifications, equivalent substitutions and improvements made within the spirit and principles of the present utility model should be included within the protection scope of the present utility model.

Claims

1. A production system for the purification of bromonitroethanol, characterized in that, The system includes a crude product dissolving vessel, the outlet of which is connected to an extraction vessel, the organic phase outlet of which is connected to a first impurity removal device, the outlet of which is connected to a second impurity removal device, the inlet of which is connected to an eluent delivery pipeline, the eluent outlet of which is connected to a buffer vessel, the outlet of which is connected to a distillation vessel, the outlet of which is connected to a drying device, and the outlet of which is connected to a product storage tank.

2. The production system for refining bronopol according to claim 1, characterized by The extraction vessel includes a vessel body, with a feed inlet and an extractant inlet at the top of the vessel body, an aqueous phase outlet and an organic phase outlet at the bottom and upper side of the vessel body, respectively, a jacket on the outside of the vessel body, a sight glass window on the vessel body, and a stirring shaft inside the vessel body. One end of the stirring shaft is connected to a motor, and the stirring shaft is equipped with multiple hollowed-out arc-shaped stirring plates.

3. The production system for refining bronopol according to claim 1, characterized by, The first impurity removal device includes a body, with an inlet and an outlet at the top and bottom of the body, respectively. The interior of the body is provided with an activated carbon adsorption layer, a resin adsorption layer and an activated alumina adsorption layer from top to bottom.

4. The production system for refining bronopol according to claim 1, characterized by The second impurity removal device includes a body, the top of which is provided with a feed inlet and an eluent inlet, the bottom of which is provided with a liquid outlet and an eluent outlet, and the interior of which is provided with a silica gel adsorption layer.

5. The production system for refining bronopol according to claim 1, characterized by, The distillation vessel includes a vessel body, with a feed inlet and an vent at the top and a discharge outlet at the bottom. The vessel body is fitted with a jacket on the outside and a stirring shaft inside. One end of the stirring shaft is connected to a motor, and the stirring shaft is equipped with multiple stirring rods, each with multiple arc-shaped plates.

6. The production system for refining bronopol according to claim 5, characterized by The vent is connected to the condenser, and the condensate outlet of the condenser is connected to the organic solvent storage tank.

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