CN219922937U - Albendazole production is with alkylation reaction system - Google Patents
Albendazole production is with alkylation reaction system Download PDFInfo
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- CN219922937U CN219922937U CN202321022258.2U CN202321022258U CN219922937U CN 219922937 U CN219922937 U CN 219922937U CN 202321022258 U CN202321022258 U CN 202321022258U CN 219922937 U CN219922937 U CN 219922937U
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- 238000005804 alkylation reaction Methods 0.000 title claims abstract description 57
- HXHWSAZORRCQMX-UHFFFAOYSA-N albendazole Chemical compound CCCSC1=CC=C2NC(NC(=O)OC)=NC2=C1 HXHWSAZORRCQMX-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 229960002669 albendazole Drugs 0.000 title claims abstract description 33
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 30
- 239000007788 liquid Substances 0.000 claims abstract description 80
- 229910052979 sodium sulfide Inorganic materials 0.000 claims abstract description 66
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims abstract description 66
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 39
- 238000006243 chemical reaction Methods 0.000 claims abstract description 33
- 239000002253 acid Substances 0.000 claims abstract description 18
- 238000011084 recovery Methods 0.000 claims abstract description 13
- 239000002699 waste material Substances 0.000 claims abstract description 13
- 239000003513 alkali Substances 0.000 claims abstract description 10
- 238000004064 recycling Methods 0.000 claims abstract description 9
- YXXYBJDTATZCOJ-UHFFFAOYSA-N 4-propylsulfanylbenzene-1,2-diamine Chemical compound CCCSC1=CC=C(N)C(N)=C1 YXXYBJDTATZCOJ-UHFFFAOYSA-N 0.000 claims abstract description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 204
- 239000007789 gas Substances 0.000 claims description 25
- GBMDVOWEEQVZKZ-UHFFFAOYSA-N methanol;hydrate Chemical compound O.OC GBMDVOWEEQVZKZ-UHFFFAOYSA-N 0.000 claims description 21
- 238000003756 stirring Methods 0.000 claims description 19
- 238000010992 reflux Methods 0.000 claims description 18
- 238000001816 cooling Methods 0.000 claims description 14
- 238000002425 crystallisation Methods 0.000 claims description 14
- 230000008025 crystallization Effects 0.000 claims description 14
- 239000010865 sewage Substances 0.000 claims description 14
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 claims description 11
- 229910000037 hydrogen sulfide Inorganic materials 0.000 claims description 11
- 238000005070 sampling Methods 0.000 claims description 10
- 239000011259 mixed solution Substances 0.000 claims description 9
- 239000000706 filtrate Substances 0.000 claims description 8
- 238000009833 condensation Methods 0.000 claims description 6
- 230000005494 condensation Effects 0.000 claims description 6
- 238000000605 extraction Methods 0.000 claims description 4
- 239000012530 fluid Substances 0.000 claims description 3
- 239000002994 raw material Substances 0.000 abstract description 10
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 9
- 239000012071 phase Substances 0.000 description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 8
- 239000002351 wastewater Substances 0.000 description 7
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 239000000843 powder Substances 0.000 description 5
- 238000000034 method Methods 0.000 description 4
- 239000011780 sodium chloride Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- QUWHIBBGKKRYFW-UHFFFAOYSA-N (4-amino-3-nitrophenyl) thiocyanate Chemical compound NC1=CC=C(SC#N)C=C1[N+]([O-])=O QUWHIBBGKKRYFW-UHFFFAOYSA-N 0.000 description 2
- CYNYIHKIEHGYOZ-UHFFFAOYSA-N 1-bromopropane Chemical compound CCCBr CYNYIHKIEHGYOZ-UHFFFAOYSA-N 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 238000004065 wastewater treatment Methods 0.000 description 2
- DPJCXCZTLWNFOH-UHFFFAOYSA-N 2-nitroaniline Chemical compound NC1=CC=CC=C1[N+]([O-])=O DPJCXCZTLWNFOH-UHFFFAOYSA-N 0.000 description 1
- ZMZDMBWJUHKJPS-UHFFFAOYSA-M Thiocyanate anion Chemical compound [S-]C#N ZMZDMBWJUHKJPS-UHFFFAOYSA-M 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011033 desalting Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- -1 firstly Chemical compound 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- ZMZDMBWJUHKJPS-UHFFFAOYSA-N hydrogen thiocyanate Natural products SC#N ZMZDMBWJUHKJPS-UHFFFAOYSA-N 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000007363 ring formation reaction Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The utility model relates to an alkylation reaction system for albendazole production, which comprises an alkylation reaction kettle and a sodium sulfide recovery system; the alkylation reaction kettle comprises a first kettle body, a feed inlet, a first feed pipe, a second feed pipe, a liquid discharge pipe, a 2-amino-4-propylsulfanyl aniline discharge pipe and a water phase discharge pipe, wherein the feed inlet, the first feed pipe, the second feed pipe and the liquid discharge pipe are arranged on the first kettle body; the sodium sulfide recovery system comprises an alkaline water collecting tank, an acid reaction kettle and an alkaline reaction kettle which are sequentially communicated, and a feed liquid inlet of the alkaline water collecting tank is communicated with the water phase discharge pipe; and a feed liquid outlet of the alkali reaction kettle is communicated with the second feed pipe through a sodium sulfide recycling pipeline. The utility model can recycle excessive sodium sulfide in the waste liquid and then recycle the waste liquid for alkylation reaction, thereby greatly avoiding the waste of sodium sulfide, saving sodium sulfide raw materials and reducing raw material cost.
Description
Technical Field
The utility model belongs to the field of albendazole production equipment, and particularly relates to an alkylation reaction system for albendazole production.
Background
The albendazole is prepared by taking o-nitroaniline as a raw material and sequentially carrying out a thiocyanate reaction, an alkylation reaction and a cyclization reaction, wherein in order to enable 2-nitro-4-thiocyanatoaniline to react completely in the alkylation reaction, sodium sulfide is usually required to be added twice, and excessive sodium sulfide is often required to be added, under the passing condition, the adding amount of sodium sulfide is 2 times of the theoretical required amount, and unutilized sodium sulfide enters a wastewater treatment system along with wastewater to be treated, so that on one hand, great waste of sodium sulfide raw material is caused, and on the other hand, the difficulty of wastewater treatment is increased.
Disclosure of Invention
The utility model aims to overcome the defect of great waste of sodium sulfide raw materials caused by discharge of excessive sodium sulfide along with wastewater in the prior art, and provides an alkylation reaction system for albendazole production.
In order to achieve the above purpose, the technical scheme adopted by the utility model is as follows:
an alkylation reaction system for albendazole production comprises an alkylation reaction kettle and a sodium sulfide recovery system; the alkylation reaction kettle comprises a first kettle body, a feed inlet, a first feed pipe, a second feed pipe, a liquid discharge pipe, a 2-amino-4-propylsulfanyl aniline discharge pipe and a water phase discharge pipe, wherein the feed inlet, the first feed pipe, the second feed pipe and the liquid discharge pipe are arranged on the first kettle body;
the sodium sulfide recovery system comprises an alkaline water collecting tank, an acid reaction kettle and an alkaline reaction kettle which are sequentially communicated, and a feed liquid inlet of the alkaline water collecting tank is communicated with the water phase discharge pipe; and a feed liquid outlet of the alkali reaction kettle is communicated with the second feed pipe through a sodium sulfide recycling pipeline.
As a further technical scheme, the alkaline water collecting tank is also provided with a liquid suction pipe, and the liquid discharge pipe is provided with a liquid suction pump;
the acid reaction kettle comprises a second kettle body, a second stirring device and a pH sensor which are arranged in the second kettle body, and an alkaline water inlet, an acid liquor inlet, a hydrogen sulfide gas outlet and a liquid outlet which are arranged on the second kettle body;
the alkali reaction kettle comprises a third kettle body, a third stirring device arranged in the third kettle body, and an air inlet pipe and a sodium sulfide liquid outlet arranged on the third kettle body;
the liquid suction pipe is communicated with the alkaline water inlet through a first pipeline, the hydrogen sulfide gas outlet is communicated with the air inlet pipe through a second pipeline, and the sodium sulfide liquid outlet is communicated with the second feed pipe through a sodium sulfide recycling pipeline.
As a further technical scheme, the inlet end of the air inlet pipe is arranged at the upper part of the third kettle body, and the outlet end of the air inlet pipe is arranged at the lower part of the third kettle body and is positioned below the stirring blade of the stirring device;
and a sampling tube is further arranged on the sodium sulfide liquid outlet.
As a further technical scheme, the third kettle body is further provided with a gas outlet and a circulating pipeline, two ends of the circulating pipeline are respectively communicated with the gas outlet and the sodium sulfide liquid outlet, and a circulating pump is arranged on the circulating pipeline.
As a further technical scheme, the liquid outlet is sequentially provided with a cooling crystallization kettle and a plate-and-frame filter press according to the flow direction of waste liquid, and a filtrate outlet of the plate-and-frame filter press is communicated with a sewage treatment system.
As a further technical scheme, the feed liquid inlet of the cooling crystallization kettle is communicated with the liquid outlet of the acid reaction kettle through a third pipeline, the feed liquid outlet of the cooling crystallization kettle is communicated with the feed liquid inlet of the plate-and-frame filter press through a fourth pipeline, and the filtrate outlet of the plate-and-frame filter press is communicated with the sewage treatment system through a sewage pipeline.
As a further technical scheme, the first kettle body, the second kettle body and the third kettle body have the same structure and comprise jackets arranged outside the corresponding kettle bodies, medium fluid arranged in a hollow cavity of the jackets, and a medium inlet and a medium outlet which are communicated with the hollow cavity of the jackets.
As a further technical scheme, the alkylation reaction kettle further comprises a first stirring device arranged in the first kettle body, a kettle body steam outlet and a reflux port arranged at the top of the first kettle body, and a methanol secondary condensing system arranged above the first kettle body.
As a further technical scheme, the secondary condensation system comprises a methanol primary condenser and a methanol secondary condenser communicated with the methanol primary condenser;
the top of the first-stage methanol condenser is provided with a first-stage methanol steam inlet, the bottom is provided with a methanol condensate outlet and a methanol steam outlet pipe, the inlet end of the methanol steam outlet pipe is higher than the inlet end of the methanol condensate outlet,
the methanol secondary condenser is provided with a secondary methanol steam inlet, a methanol-water mixed solution outlet and a non-condensable gas outlet;
the methanol steam inlet is communicated with the kettle body steam outlet through a first steam pipeline, and the methanol condensate outlet is communicated with a methanol collecting tank through a methanol collecting pipeline;
the methanol steam outlet pipe is communicated with the second-stage methanol steam inlet through a second steam pipeline, and the methanol water mixed solution outlet is communicated with the reflux port of the first kettle body through a reflux pipeline; the methanol-water mixed solution outlet is also communicated with a methanol-water collecting tank through a methanol-water collecting pipeline.
As a further technical scheme, the reflux pipeline is also provided with a sampling port.
Compared with the prior art, the utility model has the beneficial effects that:
according to the utility model, the excessive sodium sulfide in the waste liquid is recovered by arranging the sodium sulfide recovery system and then recycled for alkylation reaction, so that the waste of sodium sulfide is greatly avoided, the sodium sulfide raw material is saved, and the raw material cost is reduced.
Drawings
FIG. 1 is a schematic diagram of an embodiment of the present utility model;
in the figure, 1, alkylation reaction vessel, 2, first vessel, 3, feed inlet, 4, first feed pipe, 5, second feed pipe, 6, drain pipe, 7, 2-amino-4-propylsulfanilide drain pipe, 8, aqueous phase drain pipe, 9, alkaline water collecting tank, 10, acid reaction vessel, 11, alkaline reaction vessel, 12, liquid extraction pipe, 13, liquid extraction pump, 14, second vessel, 15, second stirring device, 16, pH sensor, 17, alkaline water inlet, 18, acid liquid inlet, 19, hydrogen sulfide gas outlet, 20, drain port, 21, third vessel, 22, third stirring device, 23, gas inlet pipe, 24, sodium sulfide liquid outlet, 25, first pipe, 26, second pipe, 27, sodium sulfide recycling pipe, 28, valve, 29, sampling pipe, 30, gas outlet, 31, circulating pipe, 32, circulating pump, 33, a cooling crystallization kettle, 34, a plate-and-frame filter press, 35, a sewage treatment system, 36, a third pipeline, 37, a fourth pipeline, 38, a sewage pipeline, 39, a hollow cavity, 40, a medium inlet, 41, a medium outlet, 42, a first stirring device, 43, a kettle steam outlet, 44, a reflux inlet, 45, a methanol primary condenser, 46, a power pump, 47, a methanol secondary condenser, 48, a primary methanol steam inlet, 49, a methanol condensate outlet, 50, a methanol steam outlet pipe, 51, a secondary methanol steam inlet, 52, a methanol water mixed liquid outlet, 53, a noncondensable gas outlet, 54, a first steam pipeline, 55, a methanol collecting pipeline, 56, a methanol collecting tank, 57, a second steam pipeline, 58, a reflux pipeline, 59, a methanol water collecting pipeline, 60, a methanol water collecting tank, 61 and a sampling port.
Detailed Description
The following description of the embodiments of the present utility model will be made apparent and fully in view of the accompanying drawings, in which some, but not all embodiments of the utility model are shown. All other embodiments, which can be made by those skilled in the art based on the embodiments of the utility model without making any inventive effort, are intended to be within the scope of the utility model.
In the description of the present utility model, it should be noted that the directions or positional relationships indicated by the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc. are based on the directions or positional relationships shown in the drawings, are merely for convenience of describing the present utility model and simplifying the description, and do not indicate or imply that the devices or elements referred to must have a specific orientation, be configured and operated in a specific orientation, and thus should not be construed as limiting the present utility model. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the present utility model, it should be noted that, unless explicitly specified and limited otherwise, the terms "mounted," "connected," and "connected" are to be construed broadly, and may be either fixedly connected, detachably connected, or integrally connected, for example; can be mechanically or electrically connected; can be directly connected or indirectly connected through an intermediate medium, and can be communication between two elements. The specific meaning of the above terms in the present utility model will be understood in specific cases by those of ordinary skill in the art.
The present utility model will be described in further detail with reference to the accompanying drawings.
One embodiment of an alkylation reaction system for albendazole production of the present utility model shown in fig. 1 comprises an alkylation reaction vessel 1 and a sodium sulfide recovery system; the alkylation reaction kettle 1 comprises a first kettle body 2, a feed inlet 3, a first feed pipe 4, a second feed pipe 5, a liquid discharge pipe 6, a 2-amino-4-propylsulfanyl aniline discharge pipe 7 and a water phase discharge pipe 8, wherein the feed inlet 3, the first feed pipe 4, the second feed pipe 5 and the liquid discharge pipe 6 are arranged on the first kettle body 2;
the sodium sulfide recovery system comprises an alkaline water collecting tank 9, an acid reaction kettle 10 and an alkaline reaction kettle 11 which are sequentially communicated, and a feed liquid inlet of the alkaline water collecting tank 9 is communicated with the water phase discharge pipe 8; the feed liquid outlet of the alkali reaction kettle 11 is communicated with the second feed pipe 5 through a sodium sulfide recycling pipeline 27. According to the utility model, the excessive sodium sulfide in the waste liquid is recovered by arranging the sodium sulfide recovery system and then recycled for alkylation reaction, so that the waste of sodium sulfide is greatly avoided, the sodium sulfide raw material is saved, and the raw material cost is reduced. When the sodium sulfide is recovered, hydrochloric acid is added into the acid reaction kettle 10 to enable the sodium sulfide to react with the hydrochloric acid to generate hydrogen sulfide gas, then sodium hydroxide in the alkali reaction kettle 11 is utilized to absorb hydrogen sulfide to generate sodium sulfide again, so that the recovery of the sodium sulfide in the wastewater is completed, and sodium sulfide solution generated by the alkali reaction kettle 11 is reused in alkylation reaction after reaching proper solubility, so that the addition amount of water and sodium sulfide powder in the alkylation reaction kettle 1 can be reduced, the use amount of the sodium sulfide powder is greatly saved, and the raw material cost of the sodium sulfide is reduced.
As an embodiment of the alkylation reaction system for albendazole production, the alkaline water collecting tank 9 is also provided with a liquid extracting pipe 12, and the liquid discharging pipe 6 is provided with a liquid extracting pump 13;
the acid reaction kettle 10 comprises a second kettle body 14, a second stirring device 15 and a pH sensor 16 which are arranged in the second kettle body 14, and an alkaline water inlet 17, an acid liquid inlet 18, a hydrogen sulfide gas outlet 19 and a liquid outlet 20 which are arranged on the second kettle body 14;
the alkali reaction kettle 11 comprises a third kettle body 21, a third stirring device 22 arranged in the third kettle body 21, and an air inlet pipe 23 and a sodium sulfide liquid outlet 24 arranged on the third kettle body 21;
the liquid suction pipe 12 is communicated with the alkaline water inlet 17 through a first pipeline 25, the hydrogen sulfide gas outlet 19 is communicated with the gas inlet pipe 23 through a second pipeline 26, and the sodium sulfide liquid outlet 24 is communicated with the second feed pipe 5 through a sodium sulfide recycling pipeline 27.
As an example of an alkylation reaction system for albendazole production of the present utility model,
the inlet end of the air inlet pipe 23 is arranged at the upper part of the third kettle body 21, and the outlet end is arranged at the lower part of the third kettle body 21 and is positioned below the stirring blades of the stirring device.
As an example of an alkylation reaction system for albendazole production, the sodium sulfide liquid outlet 24 is further provided with a sampling tube 29.
As an embodiment of the alkylation reaction system for albendazole production of the present utility model, a gas outlet 30 and a circulation pipe 31 are further disposed outside the third kettle body 21, two ends of the circulation pipe 31 are respectively connected to the gas outlet 30 and the sodium sulfide liquid outlet 24, and a circulation pump 32 is disposed on the circulation pipe 31.
As an example of an alkylation reaction system for albendazole production, the liquid outlet 20 is provided with a cooling crystallization kettle 33 and a plate-and-frame filter press 34 in sequence according to the flow direction of the waste liquid, and the filtrate outlet of the plate-and-frame filter press 34 is communicated with a sewage treatment system 35.
As an embodiment of an alkylation reaction system for albendazole production, a filtrate outlet of the plate-and-frame filter press 34 is communicated with a sewage treatment system 35, sodium chloride in waste liquid is crystallized by cooling a crystallization kettle 33, then solid-liquid separation is carried out by plate-and-frame filter pressing, and after recovery of sodium chloride is completed, the waste water enters the sewage treatment system 35 for further treatment.
As an embodiment of the albendazole producing alkylation reaction system of the present utility model, the liquid inlet of the cooling crystallization kettle 33 is connected to the liquid outlet 20 of the acid reaction kettle 10 via a third pipe 36, the liquid outlet of the cooling crystallization kettle 33 is connected to the liquid inlet of the plate-and-frame filter press 34 via a fourth pipe 37, and the filtrate outlet of the plate-and-frame filter press 34 is connected to the sewage treatment system 35 via a sewage pipe 38.
As one embodiment of the alkylation reaction system for albendazole production, the first kettle body 2, the second kettle body 14 and the third kettle body 21 have the same structure and comprise a jacket arranged outside the corresponding kettle body, a medium fluid arranged in a hollow cavity 39 of the jacket, and a medium inlet 40 and a medium outlet 41 which are communicated with the hollow cavity 39 of the jacket;
the alkylation reaction kettle 1 further comprises a first stirring device 42 arranged in the first kettle body 2, a kettle body steam outlet 43 and a reflux port 44 arranged at the top of the first kettle body 2, and a methanol secondary condensation system arranged above the first kettle body 2.
As an example of an alkylation reaction system for albendazole production of the present utility model, the secondary condensation system includes a methanol primary condenser 45, a methanol secondary condenser 47 in communication with the methanol primary condenser 45;
the top of the first-stage methanol condenser 45 is provided with a first-stage methanol steam inlet 48, the bottom is provided with a methanol condensate outlet 49 and a methanol steam outlet pipe 50, the inlet end of the methanol steam outlet pipe 50 is higher than the inlet end of the methanol condensate outlet 49,
the methanol secondary condenser 47 is provided with a secondary methanol steam inlet 51, a methanol-water mixed solution outlet 52 and a noncondensable gas outlet 53;
the methanol steam inlet is communicated with the kettle body steam outlet 43 through a first steam pipeline 54, and the methanol condensate outlet 49 is communicated with a methanol collecting tank 56 through a methanol collecting pipeline 55;
the methanol vapor outlet pipe 50 is communicated with the secondary methanol vapor inlet 51 through a second vapor pipe 57, and the methanol-water mixed solution outlet 52 is communicated with the reflux port 44 of the first kettle body 2 through a reflux pipe 58.
As an example of an alkylation reaction system for albendazole production of the present utility model, the methanol-water mixed solution outlet 52 is further connected to a methanol-water collecting tank 60 via a methanol-water collecting pipe 59.
As an example of an alkylation reaction system for albendazole production, the reflux pipe 58 is further provided with a sampling port 61.
As one embodiment of the alkylation reaction system for albendazole production, the utility model comprises a first feeding pipe 4, a second feeding pipe 5, a feeding port 3, a kettle body steam discharge port 43, a reflux port 44, a liquid discharge pipe 6, a water phase discharge pipe 8, a 2-amino-4-propylsulfanylaniline discharge pipe 7, a sampling port 61, a methanol collecting pipe 55, a methanol water collecting pipe 59, a methanol water collecting tank 60, a liquid suction pipe 12, an alkaline water inlet 17, a hydrogen sulfide gas outlet 19, a liquid discharge port 20, a circulating pipe 31, a sodium sulfide liquid outlet 24, a sodium sulfide recycling pipe 27, a liquid inlet and a liquid discharge port of a cooling crystallization kettle 33, and a filtrate outlet of a plate-and-frame filter press 34 are all provided with valves 28;
as an example of an alkylation reaction system for albendazole production of the present utility model, a power pump 46 is further provided on the second conduit 26, the third conduit 36, and the fourth conduit 37.
The application method of the utility model comprises the following steps:
in the preparation process of the first batch of albendazole, firstly, methanol and water are added into an alkylation reaction kettle 1 through a second feed pipe 5, 2-nitro-4-thiocyanatoaniline and sodium sulfide powder which are materials in the previous process are put into the alkylation reaction kettle 1 through a feed port 3 for stirring, steam is introduced into a jacket hollow cavity 39 of the alkylation reaction kettle 1, the temperature in the kettle is regulated to 40+/-5 ℃, and bromopropane is dropwise added into a first kettle body 2 through a first feed pipe 4; after finishing the dripping of bromopropane, heating the alkylation reaction kettle 1 to 50-55 ℃ through jacket steam, preserving heat and reacting for 2 hours, then introducing circulating water into a jacket hollow cavity 39 to reduce the temperature in the kettle to below 40 ℃, slowly adding sodium sulfide powder again, after finishing the feeding, raising the temperature to 80-85 ℃, refluxing for 3 hours, closing a valve 28 of a reflux pipeline 58, starting normal pressure distillation to recover methanol, performing two-stage condensation through a methanol secondary condenser 47, recovering the methanol to a methanol recovery tank, introducing waste water to a methanol water receiving tank, and finishing the distillation when the temperature reaches 90 ℃ and no reflux phenomenon exists;
then circulating water is introduced into a hollow cavity 39 of a jacket of the alkylation reaction kettle 1, the temperature is reduced to 80 ℃, toluene is added, standing is carried out for 30 minutes for layering, sampling is carried out, the content of 2-amino-4-propylsulfanyl aniline is not less than 98% by liquid phase analysis, the moisture content of a toluene phase is less than five parts per million, the toluene phase is discharged through a 2-amino-4-propylsulfanyl aniline discharge pipe 7 to enter a subsequent process, and after a water phase enters an alkaline water collecting tank 9 through a water phase discharge pipe 8, sodium sulfide is recovered;
after the wastewater in the alkaline water collecting tank 9 enters the acid reaction kettle 10 through the first pipeline 25, hydrochloric acid is added into the acid reaction kettle 10, the hydrochloric acid reacts with sodium sulfide to generate hydrogen sulfide gas and sodium chloride, the gas enters the alkaline reaction kettle 11 through the second pipeline 26 and reacts with sodium hydroxide in the alkaline reaction kettle 11 to generate sodium sulfide, when the sodium sulfide solution in the alkaline reaction kettle 11 reaches a proper concentration, the sodium sulfide solution is added into the alkylation reaction kettle 1 in the next batch production process, and water and sodium sulfide are provided for alkylation reaction, so that the addition amount of sodium sulfide powder and water in the alkylation reaction of the next batch is reduced;
the salt-containing wastewater in the alkali reaction kettle 11 is discharged into a cooling crystallization kettle 33 for cooling crystallization, is subjected to filter pressing and desalting through a plate-and-frame filter press 34, and is discharged into a sewage treatment system 35 for treatment.
The above described embodiments are only preferred examples of the utility model and are not exhaustive of the possible implementations of the utility model. Any obvious modifications thereof, which would be apparent to those skilled in the art without departing from the principles and spirit of the present utility model, should be considered to be included within the scope of the appended claims.
Claims (10)
1. An alkylation reaction system for albendazole production is characterized by comprising an alkylation reaction kettle (1) and a sodium sulfide recovery system; the alkylation reaction kettle (1) comprises a first kettle body (2), a feed inlet (3), a first feed pipe (4), a second feed pipe (5) and a liquid discharge pipe (6) which are arranged on the first kettle body (2), and a 2-amino-4-propylsulfanyl aniline discharge pipe (7) and a water phase discharge pipe (8) which are communicated with the liquid discharge pipe (6);
the sodium sulfide recovery system comprises an alkaline water collecting tank (9), an acid reaction kettle (10) and an alkaline reaction kettle (11) which are sequentially communicated, wherein a feed liquid inlet of the alkaline water collecting tank (9) is communicated with the water phase discharge pipe (8); the feed liquid outlet of the alkali reaction kettle (11) is communicated with the second feed pipe (5) through a sodium sulfide recycling pipeline (27).
2. An alkylation reaction system for albendazole production of claim 1,
a liquid extraction pipe (12) is further arranged on the alkaline water collecting tank (9), and a liquid extraction pump (13) is arranged on the liquid discharge pipe (6);
the acid reaction kettle (10) comprises a second kettle body (14), a second stirring device (15) and a pH sensor (16) which are arranged in the second kettle body (14), and an alkaline water inlet (17), an acid liquid inlet (18), a hydrogen sulfide gas outlet (19) and a liquid outlet (20) which are arranged on the second kettle body (14);
the alkali reaction kettle (11) comprises a third kettle body (21), a third stirring device (22) arranged in the third kettle body (21), and an air inlet pipe (23) and a sodium sulfide liquid outlet (24) arranged on the third kettle body (21);
the liquid suction pipe (12) is communicated with the alkaline water inlet (17) through a first pipeline (25), the hydrogen sulfide gas outlet (19) is communicated with the gas inlet pipe (23) through a second pipeline (26), and the sodium sulfide liquid outlet (24) is communicated with the second feed pipe (5) through a sodium sulfide recycling pipeline (27).
3. An alkylation reaction system for albendazole production of claim 2,
the inlet end of the air inlet pipe (23) is arranged at the upper part of the third kettle body (21), and the outlet end of the air inlet pipe is arranged at the lower part of the third kettle body (21) and is positioned below the stirring blades of the stirring device;
and a sampling tube (29) is further arranged on the sodium sulfide liquid outlet (24).
4. An alkylation reaction system for albendazole production of claim 3,
the third kettle body (21) is also provided with a gas outlet (30) and a circulating pipeline (31), two ends of the circulating pipeline (31) are respectively communicated with the gas outlet (30) and the sodium sulfide liquid outlet (24), and a circulating pump (32) is arranged on the circulating pipeline (31).
5. An alkylation reaction system for albendazole production of claim 2,
the liquid outlet (20) is sequentially provided with a cooling crystallization kettle (33) and a plate-and-frame filter press (34) according to the flow direction of waste liquid, and a filtrate outlet of the plate-and-frame filter press (34) is communicated with a sewage treatment system (35).
6. An alkylation reaction system for albendazole production of claim 5,
the liquid inlet of the cooling crystallization kettle (33) is communicated with a liquid outlet (20) of the acid reaction kettle (10) through a third pipeline (36), the liquid outlet of the cooling crystallization kettle (33) is communicated with the liquid inlet of the plate-and-frame filter press (34) through a fourth pipeline (37), and the filtrate outlet of the plate-and-frame filter press (34) is communicated with the sewage treatment system (35) through a sewage pipeline (38).
7. The alkylation reaction system for albendazole production of claim 1, wherein the first kettle body (2), the second kettle body (14) and the third kettle body (21) have the same structure, each comprise a jacket arranged outside the corresponding kettle body, a medium fluid arranged in a hollow cavity (39) of the jacket, and a medium inlet (40) and a medium outlet (41) which are communicated with the hollow cavity (39) of the jacket.
8. The alkylation reaction system for albendazole production of claim 1, wherein the alkylation reaction kettle (1) further comprises a first stirring device (42) arranged in the first kettle body (2), a kettle body steam outlet (43) and a reflux port (44) arranged at the top of the first kettle body (2), and a methanol secondary condensation system arranged above the first kettle body (2).
9. The alkylation reaction system for albendazole production of claim 8,
the secondary condensation system comprises a methanol primary condenser (45), and a methanol secondary condenser (47) communicated with the methanol primary condenser (45);
the top of the first-stage methanol condenser (45) is provided with a first-stage methanol steam inlet (48), the bottom is provided with a methanol condensate outlet (49) and a methanol steam outlet pipe (50), the inlet end of the methanol steam outlet pipe (50) is higher than the inlet end of the methanol condensate outlet (49),
the methanol secondary condenser (47) is provided with a secondary methanol steam inlet (51), a methanol-water mixed solution outlet (52) and a noncondensable gas outlet (53);
the methanol steam inlet is communicated with the kettle body steam outlet (43) through a first steam pipeline (54), and the methanol condensate outlet (49) is communicated with a methanol collecting tank (56) through a methanol collecting pipeline (55);
the methanol steam outlet pipe (50) is communicated with the secondary methanol steam inlet (51) through a second steam pipeline (57), and the methanol water mixed solution outlet (52) is communicated with the reflux port (44) of the first kettle body (2) through a reflux pipeline (58); the methanol-water mixed solution outlet (52) is also communicated with a methanol-water collecting tank (60) through a methanol-water collecting pipeline (59).
10. The alkylation reaction system for albendazole production of claim 9,
the reflux pipeline (58) is also provided with a sampling port (61).
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