CN112500391A - Device and method for producing dithianon through continuous kettle type reaction - Google Patents

Device and method for producing dithianon through continuous kettle type reaction Download PDF

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CN112500391A
CN112500391A CN202011474736.4A CN202011474736A CN112500391A CN 112500391 A CN112500391 A CN 112500391A CN 202011474736 A CN202011474736 A CN 202011474736A CN 112500391 A CN112500391 A CN 112500391A
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reaction kettle
kettle
reaction
dithianon
pipe
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吴勇
高金平
柴明根
陈思颖
侯云飞
王光瀛
毕海寅
马超
贾志新
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JIANGXI HEYI CHEMICALS CO Ltd
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JIANGXI HEYI CHEMICALS CO Ltd
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D339/00Heterocyclic compounds containing rings having two sulfur atoms as the only ring hetero atoms
    • C07D339/08Six-membered rings

Abstract

The invention discloses a device and a method for producing dithianon by continuous kettle type reaction, which comprises a dilute nitric acid storage tank and a reaction kettle, wherein a compound feeding bin, a first air-lock valve, a feeding auger, a second air-lock valve and a feeding pipe are sequentially arranged above the reaction kettle from top to bottom, a reaction kettle condenser is arranged above the reaction kettle and is communicated with the reaction kettle, a reaction liquid receiving kettle is arranged on the right side of the reaction kettle, the reaction kettle and the reaction liquid receiving kettle are sequentially communicated through an overflow pipe, discharge pipes are respectively arranged at the lower ends of the reaction kettle and the reaction liquid receiving kettle, a two-in-one pressure filter is arranged on one side of the dilute nitric acid storage tank, and the discharge pipes are integrally communicated through a pipeline and are communicated with the two-in-one pressure filter through a reaction liquid material transfer. Compared with an intermittent production process, the invention greatly reduces the labor intensity of workers.

Description

Device and method for producing dithianon through continuous kettle type reaction
Technical Field
The invention belongs to a synthesis process of pesticide organic compounds, and particularly relates to a device and a method for producing dithianon through a continuous kettle type reaction.
Background
Dithianon (dithianon) is a fungicide developed by basf european corporation, pure as a dark brown crystalline solid, with the chemical name: 2, 3-dinitrile-1, 4-dithioanthraquinone. Dithianon (dithianon) is widely used at home and abroad as a protective bactericide, for example, dithianon is used for controlling grape downy mildew (Plasmopara vidcola) III in the vast grape growing area of Australian grape wine producing areas, and the action mechanism of dithianon is to inhibit the germination of sporophytes to finally achieve the protective effect. The production method of dithianon adopts batch kettle type production. Need load and auxiliary operation such as unloading in the intermittent type cauldron formula production process, easily cause loss of material and energy, improved manufacturing cost, prolonged production cycle, and product quality is difficult for stably. The intermittent kettle type production is easy to cause volatilization of toxic, inflammable and explosive solvents, and has certain influence on human health and safe production. The batch kettle type production is not suitable for large-scale production, has the problems of long reaction time, high production cost, serious equipment corrosion, high environmental protection pressure and the like, and has high attention paid to how to simply, efficiently and continuously produce the dithianon.
Disclosure of Invention
In order to solve the technical problems, the invention provides the following technical scheme:
the invention provides a device for producing dithianon by continuous kettle type reaction,
including dilute nitric acid holding vessel, reation kettle includes first reation kettle, second reation kettle, third reation kettle, first reation kettle, second reation kettle, third reation kettle turn right from a left side and highly dwindle setting in proper order, first reation kettle's upper end with dilute nitric acid holding vessel changes the material pump through the pipeline intercommunication through dilute nitric acid, first reation kettle's top down sets gradually from last has the compound to add feed bin, first air lock, feeding auger, second air lock, inlet pipe, the compound of cyclizing adds feed bin, first air lock, feeding auger, second air lock, inlet pipe and communicates in proper order, the inlet pipe with first reation kettle intercommunication, first reation kettle, second reation kettle, third reation kettle top all are provided with outlet duct, back flow, first reation kettle, second reation kettle, third reation kettle top correspond respectively and are provided with first reation kettle condenser, second reation kettle, A second reaction kettle condenser and a third reaction kettle condenser, wherein the upper end and the lower end of the first reaction kettle condenser, the second reaction kettle condenser and the third reaction kettle condenser are respectively provided with an air inlet and a discharge hole, the air outlet pipe is communicated with the air inlet, the return pipe is communicated with the discharge hole,
third reation kettle right side is provided with the reaction liquid and receives the cauldron, the reaction liquid is received the cauldron high-end and is less than the third reation kettle sets up, first reation kettle, second reation kettle, third reation kettle, reaction liquid receive the cauldron and loop through the overflow pipe intercommunication, first reation kettle, second reation kettle, third reation kettle, reaction liquid receive the cauldron lower extreme and all are provided with row material pipe, dilute nitric acid holding vessel one side is provided with two and closes a pressure filter, arrange the material pipe through the whole intercommunication of pipeline through reaction liquid material transfer pump with two and close a pressure filter intercommunication.
Preferably, the upper end of the reaction liquid receiving kettle is provided with an exhaust pipe, and the exhaust pipe is communicated with an air inlet of a condenser of the third reaction kettle.
Preferably, the lower extreme lateral wall of first reation kettle condenser, second reation kettle condenser, third reation kettle condenser all is provided with the air duct, the air duct passes through the whole intercommunication of pipeline and carries to the interior processing of tail gas processing apparatus.
Preferably, the first reaction kettle, the second reaction kettle, the third reaction kettle and the reaction liquid receiving kettle are all provided with an outer jacket and a stirring device, and the stirring device can stir materials in the first reaction kettle, the second reaction kettle, the third reaction kettle and the reaction liquid receiving kettle.
Preferably, the dithianon cyclized material and 30% dilute nitric acid are used as raw materials, and the reaction equation is as follows:
Figure BDA0002834905120000021
the method comprises the following steps:
s1: feeding a dithianon cyclized material to a cyclized material feeding bin, continuously feeding the cyclized material into a first reaction kettle through a first air shutting machine, a feeding auger, a second air shutting machine and a feeding pipe, conveying 30% of dilute nitric acid into the first reaction kettle through a dilute nitric acid transferring pump, starting a stirring device to stir the material in the first reaction kettle, and controlling the temperature of the first reaction kettle to be 65-95 ℃;
s2: overflowing the materials in the first reaction kettle into a second reaction kettle through an overflow pipe, starting a stirring device to stir the materials in the second reaction kettle, and controlling the temperature of the second reaction kettle to be 65-95 ℃;
s3: overflowing the materials in the second reaction kettle into a third reaction kettle through an overflow pipe, starting a stirring device to stir the materials in the third reaction kettle, and controlling the temperature of the third reaction kettle to be 65-95 ℃;
s4: in material in the third reation kettle passed through the overflow pipe overflow and gets into reaction liquid and receive the cauldron, it is right to open agitating unit material in the reaction liquid receipt cauldron stirs, treat the material cooling in the reaction liquid receipt cauldron, reaction liquid receives the cauldron and accumulates a quantitative back, first reation kettle, second reation kettle, third reation kettle, the row's of reaction liquid receipt cauldron lower extreme material pipe pass through the whole intercommunication of pipeline and carry to two-in-one filter-press through reaction liquid commentaries on classics material pump, two-in-one filter-press carries out the filter-pressing to inside material, the waste water treatment is gone to the mother liquor, wet material is dried and is got the dithianon anthraquinone finished product.
Preferably, the dithianon cyclized material: the mass ratio of 30% dilute nitric acid is 1: 1.4 to 4.
Preferably, the molar ratio of the dithianon cyclized material to 30% diluted nitric acid is 1: 2.05-5.74, the mass flow rate of the dithianon cyclized material is 50-100 kg/h, and the mass flow rate of the 30% dilute nitric acid is 35-400 kg/h.
The invention has the beneficial effects
Compared with the prior art, the invention has the following advantages:
(1) compared with an intermittent production process, the labor intensity of workers is greatly reduced.
(2) The selectivity of the product is obviously improved, the byproducts are obviously reduced, and the three wastes are reduced.
(3) The whole reaction process is a continuous reaction, the process is simple, the reaction conditions are accurately controlled, the corrosion of equipment is low, and the safety is high.
(4) The reaction yield is improved, the yield reaches 98 percent, the product purity is 98 to 99 percent, and the production cost is low.
Drawings
FIG. 1 is a schematic structural diagram of an apparatus for producing dithianon according to the present invention.
Description of reference numerals: 1. a dilute nitric acid storage tank; 2. a first reaction kettle; 3. a second reaction kettle; 4. a third reaction kettle; 5. a dilute nitric acid transfer pump; 6. a cyclized product feeding bin; 7. a first air-turning off machine; 8. feeding the auger; 9. a second air shutter machine; 10. a feed pipe; 11. an air outlet pipe; 12. a return pipe; 13. a first reaction kettle condenser; 14. a second reaction kettle condenser; 15. a third reaction kettle condenser; 16. a reaction liquid receiving kettle; 17. a discharge pipe; 18. a reaction liquid transfer pump; 19. a two-in-one filter press; 20. an exhaust pipe; 21. an air duct; 22. and (4) an overflow pipe.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious 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.
Example 1
The preferred embodiment of the method for producing dithianon by using the continuous kettle type dithianon production device of the invention as shown in the attached figure 1,
as shown in figure 1, the invention provides a device for producing dithianon by continuous tank reaction,
comprises a dilute nitric acid storage tank 1 and a reaction kettle, wherein the reaction kettle comprises a first reaction kettle 2, a second reaction kettle 3 and a third reaction kettle 4, the first reaction kettle 2, the second reaction kettle 3 and the third reaction kettle 4 are sequentially arranged in a descending manner from left to right, the upper end of the first reaction kettle 2 and the dilute nitric acid storage tank 1 are communicated through a pipeline through a dilute nitric acid transfer pump 5, a cyclized substance feeding bin 6, a first air shutoff machine 7, a feeding packing auger 8, a second air shutoff machine 9 and an inlet pipe 10 are sequentially arranged above the first reaction kettle 2 from top to bottom, the cyclized substance feeding bin 6, the first air shutoff machine 7, the feeding packing auger 8, the second air shutoff machine 9 and the inlet pipe 10 are sequentially communicated, the inlet pipe 10 is communicated with the first reaction kettle 2, an outlet pipe 11 and a return pipe 12 are arranged above the first reaction kettle 2, the second reaction kettle 3 and the third reaction kettle 4, a first reaction kettle condenser 13, a second reaction kettle condenser 14 and a third reaction kettle condenser 15 are respectively and correspondingly arranged above the first reaction kettle 2, the second reaction kettle 3 and the third reaction kettle 4, the upper end and the lower end of the first reaction kettle condenser 13, the second reaction kettle condenser 14 and the third reaction kettle condenser 15 are respectively provided with an air inlet and a discharge hole, the air outlet pipe 11 is communicated with the air inlet, the return pipe 12 is communicated with the discharge hole,
a reaction liquid receiving kettle 16 is arranged on the right side of the third reaction kettle 4, the height of the reaction liquid receiving kettle 16 is lower than that of the third reaction kettle 4, the lower ends of the first reaction kettle 2, the second reaction kettle 3, the third reaction kettle 4 and the reaction liquid receiving kettle 16 are communicated through an overflow pipe 22 in sequence, discharge pipes 17 are arranged at the lower ends of the first reaction kettle 2, the second reaction kettle 3, the third reaction kettle 4 and the reaction liquid receiving kettle 16, a two-in-one pressure filter 19 is arranged on one side of the dilute nitric acid storage tank 1, the discharge pipes 17 are communicated with the two-in-one pressure filter 19 through a reaction liquid transferring pump 18 through a pipeline, an exhaust pipe 20 is arranged at the upper end of the reaction liquid receiving kettle 16, and the exhaust pipe 20 is communicated with an air inlet of a third reaction kettle condenser 15,
the side walls of the lower ends of the first reaction kettle condenser 13, the second reaction kettle condenser 14 and the third reaction kettle condenser 15 are respectively provided with an air duct 21, the air ducts 21 are integrally communicated through pipelines and are conveyed to a tail gas treatment device for treatment,
the first reaction kettle 2, the second reaction kettle 3, the third reaction kettle 4 and the reaction liquid receiving kettle 16 are all provided with an outer jacket and a stirring device, the stirring device can stir the materials in the first reaction kettle 2, the second reaction kettle 3, the third reaction kettle 4 and the reaction liquid receiving kettle 16,
the method is characterized in that a dithianon cyclized material and 30% dilute nitric acid are used as raw materials, and the reaction equation is as follows:
Figure BDA0002834905120000051
the method comprises the following steps:
s1: the method comprises the following steps of (1) feeding a dithianon cyclized material to a cyclized material feeding bin 6, continuously feeding the cyclized material into a first reaction kettle 2 through a first air-lock valve 7, a feeding auger 8, a second air-lock valve 9 and a feeding pipe 10, conveying 30% of dilute nitric acid into the first reaction kettle 2 through a dilute nitric acid transfer pump 5, starting a stirring device to stir the material in the first reaction kettle 2, and controlling the temperature of the first reaction kettle 2 to be 65-95 ℃;
s2: overflowing the materials in the first reaction kettle 2 into a second reaction kettle 3 through an overflow pipe 22, starting a stirring device to stir the materials in the second reaction kettle 3, and controlling the temperature of the second reaction kettle 3 to be 65-95 ℃;
s3: the materials in the second reaction kettle 3 overflow through an overflow pipe 22 and enter a third reaction kettle 4, a stirring device is started to stir the materials in the third reaction kettle 4, and the temperature of the third reaction kettle 4 is controlled to be 65-95 ℃;
s4: in material in the third reation kettle 4 overflowed through overflow pipe 22 and got into reaction liquid and receive cauldron 16, it was right to open agitating unit material in reaction liquid received cauldron 16 stirs, wait that the material cooling in the reaction liquid received cauldron 16, reaction liquid received cauldron 16 and accumulated a quantitative back, first reation kettle 2, second reation kettle 3, third reation kettle 4, the row's of reaction liquid material pipe 17 of receiving the cauldron 16 lower extreme communicate through the pipeline is whole to be carried to two unification pressure filters 19 through reaction liquid material transfer pump 18, two unification pressure filters 19 carry out the filter-pressing to the internal material, the waste water treatment is removed to the mother liquor, wet material is dried and is got the dithianon anthraquinone finished product.
Example 2
The method comprises the steps of feeding a dithianon cyclized material into a cyclized material feeding bin 6, controlling the feeding speed of the dithianon cyclized material to be 100kg/h through a first air-lock valve 7, a feeding auger 8 and a second air-lock valve 9, continuously feeding the dithianon cyclized material into a first reaction kettle 2, controlling the feeding speed of 30% of dilute nitric acid to be 145kg/h through a dilute nitric acid transfer pump 5, controlling the feeding speed of the dilute nitric acid to be 145kg/h through a mass flow meter and a feeding adjusting valve, pumping the dilute nitric acid to the first reaction kettle 2, starting stirring, controlling the temperature of the reaction kettle to be 80-85 ℃, and overflowing the material into a second; controlling the temperature of the second reaction kettle 3 to be 80-85 ℃, and enabling the reacted materials to overflow into the third reaction kettle 4 through an overflow pipe 22; controlling the temperature of the third reaction kettle 4 to be 80-85 ℃, and enabling the reacted materials to overflow through an overflow pipe 22 and enter a reaction liquid receiving kettle 16 to be cooled to 30 ℃; after the reaction liquid receiving kettle 16 accumulates to a certain amount, the first reaction kettle 2, the second reaction kettle 3, the third reaction kettle 4 and a discharge pipe 17 at the lower end of the reaction liquid receiving kettle 16 are integrally communicated through pipelines and are conveyed to a two-in-one filter press 19 through a reaction liquid transfer pump 18, the two-in-one filter press 19 carries out filter pressing on internal materials, mother liquid is subjected to wastewater treatment, wet materials are dried to obtain a dithianon finished product, the content of the dithianon product is 98.5%, and the yield is 98.7%.
Example 3
The preferred embodiment of the method for producing dithianon by using the continuous kettle type dithianon production device disclosed by the invention and shown in the attached figure 1 sequentially comprises the following steps:
the method comprises the steps of feeding a dithianon cyclized material into a cyclized material feeding bin 6, controlling the feeding speed of the dithianon cyclized material to be 90kg/h through a first air-lock valve 7, a feeding auger 8 and a second air-lock valve 9, continuously feeding the dithianon cyclized material into a first reaction kettle 2, controlling the feeding speed of 30% of dilute nitric acid to be 140kg/h through a dilute nitric acid transfer pump 5, controlling the feeding speed of the dilute nitric acid to be 140kg/h through a mass flow meter and a feeding adjusting valve, pumping the dilute nitric acid to the first reaction kettle 2, starting stirring, controlling the temperature of the reaction kettle to be 80-85 ℃, and overflowing the material into a second; controlling the temperature of the second reaction kettle 3 to be 80-85 ℃, and enabling the reacted materials to overflow into the third reaction kettle 4 through an overflow pipe 22; controlling the temperature of the third reaction kettle 4 to be 80-85 ℃, and enabling the reacted materials to overflow through an overflow pipe 22 and enter a reaction liquid receiving kettle 16 to be cooled to 30 ℃; after the reaction liquid receiving kettle 16 accumulates to a certain amount, the first reaction kettle 2, the second reaction kettle 3, the third reaction kettle 4 and a discharge pipe 17 at the lower end of the reaction liquid receiving kettle 16 are integrally communicated through pipelines and are conveyed to a two-in-one filter press 19 through a reaction liquid transfer pump 18, the two-in-one filter press 19 carries out filter pressing on internal materials, mother liquid is subjected to wastewater treatment, wet materials are dried to obtain a dithianon finished product, the content of the dithianon product is 98.3%, and the yield is 98.5%.
Example 4
The preferred embodiment of the method for producing dithianon by using the continuous kettle type dithianon production device disclosed by the invention and shown in the attached figure 1 sequentially comprises the following steps:
the method comprises the steps of feeding a dithianon cyclized material into a cyclized material feeding bin 6, controlling the feeding speed of the dithianon cyclized material to be 80kg/h through a first air-lock valve 7, a feeding auger 8 and a second air-lock valve 9, continuously feeding the dithianon cyclized material into a first reaction kettle 2, controlling the feeding speed of 30% of dilute nitric acid to be 120kg/h through a mass flow meter and a feeding adjusting valve, pumping the dilute nitric acid to the first reaction kettle 2, starting stirring, controlling the temperature of the reaction kettle to be 80-85 ℃, and overflowing the material into a second reaction kettle 3 through an overflow pipe 22; controlling the temperature of the second reaction kettle 3 to be 80-85 ℃, and enabling the reacted materials to overflow into the third reaction kettle 4 through an overflow pipe 22; controlling the temperature of the third reaction kettle 4 to be 80-85 ℃, and enabling the reacted materials to overflow through an overflow pipe 22 and enter a reaction liquid receiving kettle 16 to be cooled to 30 ℃; after the reaction liquid receiving kettle 16 accumulates to a certain amount, the first reaction kettle 2, the second reaction kettle 3, the third reaction kettle 4 and a discharge pipe 17 at the lower end of the reaction liquid receiving kettle 16 are integrally communicated through pipelines and are conveyed to a two-in-one filter press 19 through a reaction liquid transfer pump 18, the two-in-one filter press 19 carries out filter pressing on internal materials, mother liquid is subjected to wastewater treatment, wet materials are dried to obtain a dithianon finished product, the content of the dithianon product is 98.8%, and the yield is 98.9%.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments or portions thereof without departing from the spirit and scope of the invention.

Claims (7)

1. A device for producing dithianon by continuous kettle type reaction, which is characterized in that,
comprises a dilute nitric acid storage tank (1) and a reaction kettle, wherein the reaction kettle comprises a first reaction kettle (2), a second reaction kettle (3) and a third reaction kettle (4), the first reaction kettle (2), the second reaction kettle (3) and the third reaction kettle (4) are sequentially arranged in a descending manner from left to right, the upper end of the first reaction kettle (2) is communicated with the dilute nitric acid storage tank (1) through a pipeline through a dilute nitric acid transfer pump (5), a cyclic compound feeding bin (6), a first air shutoff machine (7), a feeding packing auger (8), a second air shutoff machine (9) and an inlet pipe (10) are sequentially arranged above the first reaction kettle (2) from top to bottom, the cyclic compound feeding bin (6), the first air shutoff machine (7), the feeding packing auger (8), the second air shutoff machine (9) and the inlet pipe (10) are sequentially communicated, the inlet pipe (10) is communicated with the first reaction kettle (2), an air outlet pipe (11) and a return pipe (12) are respectively arranged above the first reaction kettle (2), the second reaction kettle (3) and the third reaction kettle (4), a first reaction kettle condenser (13), a second reaction kettle condenser (14) and a third reaction kettle condenser (15) are respectively and correspondingly arranged above the first reaction kettle (2), the second reaction kettle (3) and the third reaction kettle (4), the upper end and the lower end of the first reaction kettle condenser (13), the second reaction kettle condenser (14) and the third reaction kettle condenser (15) are respectively provided with an air inlet and a discharge port, the air outlet pipe (11) is communicated with the air inlet, the return pipe (12) is communicated with the discharge port,
third reation kettle (4) right side is provided with the reactant liquid and receives cauldron (16), the reactant liquid is received cauldron (16) high-end and is less than third reation kettle (4) setting, first reation kettle (2), second reation kettle (3), third reation kettle (4), reactant liquid receive cauldron (16) and loop through overflow pipe (22) intercommunication, first reation kettle (2), second reation kettle (3), third reation kettle (4), reactant liquid receive cauldron (16) lower extreme and all are provided with row material pipe (17), dilute nitric acid holding vessel (1) one side is provided with two and closes a pressure filter, arrange material pipe (17) through the whole intercommunication of pipeline through reactant liquid material transfer pump (18) with two close a pressure filter (19) intercommunication.
2. The apparatus for producing dithianon by continuous tank reaction according to claim 1,
an exhaust pipe (20) is arranged at the upper end of the reaction liquid receiving kettle (16), and the exhaust pipe (20) is communicated with an air inlet of the third reaction kettle condenser (15).
3. The apparatus for producing dithianon by continuous tank reaction according to claim 1,
the lower extreme lateral wall of first reation kettle condenser (13), second reation kettle condenser (14), third reation kettle condenser (15) all is provided with air duct (21), air duct (21) are through the whole intercommunication of pipeline and carry to the interior processing of tail gas processing apparatus.
4. The apparatus for producing dithianon by continuous tank reaction according to claim 1,
the first reaction kettle (2), the second reaction kettle (3), the third reaction kettle (4) and the reaction liquid receiving kettle (16) are all provided with an outer jacket and a stirring device, and the stirring device can stir materials in the first reaction kettle (2), the second reaction kettle (3), the third reaction kettle (4) and the reaction liquid receiving kettle (16).
5. A method for producing dithianon by continuous kettle type reaction is characterized in that,
the method is characterized in that a dithianon cyclized material and 30% dilute nitric acid are used as raw materials, and the reaction equation is as follows:
Figure FDA0002834905110000021
the method comprises the following steps:
s1: the method comprises the following steps of (1) feeding a dithianon cyclized material to a cyclized material feeding bin (6), continuously feeding the cyclized material into a first reaction kettle (2) through a first air-lock valve (7), a feeding packing auger (8), a second air-lock valve (9) and a feeding pipe (10), conveying 30% of dilute nitric acid into the first reaction kettle (2) through a dilute nitric acid transfer pump (5), starting a stirring device to stir the material in the first reaction kettle (2), and controlling the temperature of the first reaction kettle (2) to be 65-95 ℃;
s2: overflowing the materials in the first reaction kettle (2) into a second reaction kettle (3) through an overflow pipe (22), starting a stirring device to stir the materials in the second reaction kettle (3), and controlling the temperature of the second reaction kettle (3) to be 65-95 ℃;
s3: overflowing the materials in the second reaction kettle (3) into a third reaction kettle (4) through an overflow pipe (22), starting a stirring device to stir the materials in the third reaction kettle (4), and controlling the temperature of the third reaction kettle (4) to be 65-95 ℃;
s4: materials in the third reaction kettle (4) overflow through an overflow pipe (22) and enter a reaction liquid receiving kettle (16), a stirring device is started to stir the materials in the reaction liquid receiving kettle (16), the reaction liquid is cooled and cooled, the reaction liquid receiving kettle (16) accumulates to a certain amount, a discharge pipe (17) at the lower end of the first reaction kettle (2), a second reaction kettle (3), the third reaction kettle (4) and the reaction liquid receiving kettle (16) is communicated with a material transferring pump (18) through a whole pipeline and conveyed to a two-in-one filter press (19), the two-in-one filter press (19) performs filter pressing on the internal materials, mother liquid is treated by waste water, and wet materials are dried to obtain a finished product of dithianon.
6. The continuous tank reaction process for producing dithianon according to claim 5,
the dithianon cyclized material comprises the following components: the mass ratio of 30% dilute nitric acid is 1: 1.4 to 4.
7. The continuous tank reaction process for producing dithianon according to claim 6,
the molar ratio of the dithianon cyclized material to 30% dilute nitric acid is 1: 2.05-5.74, the mass flow rate of the dithianon cyclized material is 50-100 kg/h, and the mass flow rate of the 30% dilute nitric acid is 35-400 kg/h.
CN202011474736.4A 2020-12-14 2020-12-14 Device and method for producing dithianon through continuous kettle type reaction Pending CN112500391A (en)

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