CN113908786A

CN113908786A - 2B acid crude production system

Info

Publication number: CN113908786A
Application number: CN202111316885.2A
Authority: CN
Inventors: 王慧; 俞卫祥; 许青山; 张玉超; 顾国萍
Original assignee: ZHEJIANG YOULIAN CHEMICAL INDUSTRY CO LTD; Jiaxing University
Current assignee: ZHEJIANG YOULIAN CHEMICAL INDUSTRY CO LTD; Jiaxing University
Priority date: 2021-11-09
Filing date: 2021-11-09
Publication date: 2022-01-11

Abstract

The invention discloses a 2B acid crude product production system which comprises a heating and stirring reaction kettle, a fractionating column, a vertical shell-and-tube condenser, a horizontal shell-and-tube condenser, a sulfuric acid liquid distribution structure and a water separator, wherein a solvent backflow port is arranged at the upper part of the outer wall surface of the heating and stirring reaction kettle, the fractionating column is arranged at the top of the heating and stirring reaction kettle, the inlet and the outlet of the vertical shell-and-tube condenser are respectively connected with the outlet of the fractionating column and the inlet of the horizontal shell-and-tube condenser, a water separator liquid inlet and a water separator balance port are arranged at the top of the water separator, the outlet of the horizontal condenser is connected with a water separator liquid inlet, the water separator balance port is connected with a balance port of the horizontal condenser, a solvent discharge port is arranged at the bottom of the water separator, a water discharge port is arranged at the upper part of the outer wall surface of the water separator, and the solvent discharge port is connected with the solvent backflow port; the sulfuric acid liquid distribution structure is arranged above the inside of the heating and stirring reaction kettle and is connected with a sulfuric acid feeding pipe. The invention has simple equipment and very convenient operation, is beneficial to shortening the production period and can reduce the production cost.

Description

2B acid crude production system

Technical Field

The invention relates to the technical field of 2B acid production, in particular to a 2B acid crude product production system.

Background

The 2B acid with the chemical name of 4-amino-2-chlorotoluene-5-sulfonic acid is an important organic pigment intermediate and is mainly used for synthesizing organic pigments such as fast scarlet BBN, fast scarlet BBS, fast scarlet MGP, fast scarlet F5R, fast scarlet 2BL and the like.

The 2B acid is produced by sulfonating 4-amino-2-chloroaniline 2B oil, and the traditional synthesis process mainly comprises a liquid phase method and a solid phase method. In the solid phase method, because sulfuric acid and 2B oil cannot be completely and uniformly mixed, the 2B oil is not completely reacted, the raw material carbonization phenomenon is very serious, the yield of the 2B acid is low, a sulfonated product is refined by alkali dissolution, decoloration, filtration, acid precipitation crystallization, dehydration, drying and other processes, and the purity requirement of the 2B acid product can be met. The production process of 2B acids is therefore gradually replaced entirely by liquid phase processes.

For example, application publication No.: CN109180537A, Chinese patent application publication No. 2019, 1, 11, discloses a method for preparing 3-chloro-p-toluidine-6-sulfonic acid by a liquid-phase baking method, wherein the method specifically discloses process equipment for preparing 3-chloro-p-toluidine-6-sulfonic acid, which comprises a sulfonation kettle, a baking kettle, a water separator, a condenser, a receiving tank and other equipment, in the preparation method, 2B oil and a dispersing agent are put into the sulfonation kettle to be uniformly mixed, concentrated sulfuric acid is added dropwise to react to form salt, and finally the material is transferred into the baking kettle to be subjected to high-temperature transposition, dehydration and sulfonation; the preparation method has the following defects: (1) the sulfonation kettle and the baking kettle are both conventional vertical jacket stirring kettles, and the problems of uneven material mixing and heating exist during use, so that the product purity and yield are influenced; (2) sulfonation and baking are carried out in different reaction kettles, and materials are required to be transferred for dehydration and transposition after the sulfonation reaction is salified, so that the operation is complicated, and the production period is not shortened; (3) by adopting the traditional water separator, the dripping condensate can cause impact and disturbance on the boundary liquid level in the water separator, so that the water separating effect of the water separator is poor.

Disclosure of Invention

The invention aims to solve the technical problems of the existing equipment for producing 2B acid, and provides a 2B acid crude product production system which is simple in equipment, convenient to operate, uniform in material mixing and heating, good in solvent and water separation effect and capable of reducing production cost.

In order to achieve the purpose, the invention adopts the following technical scheme: A2B acid crude product production system comprises a heating and stirring reaction kettle, a fractionating column, a vertical shell and tube condenser, a horizontal shell and tube condenser, a sulfuric acid cloth liquid structure and a water separator, wherein a reaction kettle gas phase discharge port is arranged at the top of the heating and stirring reaction kettle, a solvent backflow port is arranged at the upper part of the outer wall surface of the heating and stirring reaction kettle, a reaction kettle discharge port is arranged at the bottom of the heating and stirring reaction kettle, a water separator liquid inlet and a water separator balance port are arranged at the top of the water separator, a solvent discharging port is arranged at the bottom of the water separator, a water outlet is arranged at the upper part of the outer wall surface of the water separator, a lower end inlet of the fractionating column is connected with the reaction kettle gas phase discharge port, an upper end outlet of the fractionating column is connected with an inlet of the vertical shell and tube condenser, an outlet of the vertical shell and tube condenser is connected with an inlet of the horizontal condenser, an outlet of the horizontal condenser is connected with the water separator liquid inlet, the solvent discharging port is connected with the solvent backflow port, the balance port of the water separator is connected with the balance port of the horizontal condenser; the sulfuric acid liquid distribution structure is arranged above the interior of the heating and stirring reaction kettle and is connected with a sulfuric acid feeding pipe. The 2B acid crude product production system is used for producing 2B acid by a liquid phase sulfonation method; the invention only adopts a heating and stirring reaction kettle as a reaction vessel, has simple structure, can finish salification and dehydration transposition (sulfonation) in the heating and stirring reaction kettle, has simple equipment and very convenient operation, is beneficial to shortening the production period, can obtain the 2B acid crude product by pumping and filtering the reaction product, has low energy consumption, can recycle the solvent and can reduce the production cost; the solvent used in the present invention has a density and a boiling point higher than those of water, and includes, but is not limited to, 1,3, 5-trichlorobenzene, 1, 4-dichlorobenzene, etc.

Preferably, the heating and stirring reaction kettle comprises a kettle body, a jacket and a stirring device, wherein the stirring device comprises a motor, a stirring shaft and a stirring paddle, the jacket is arranged outside the kettle body, a heat conduction oil cavity is formed in a space between the jacket and the kettle body, an oil inlet is formed in the bottom of the jacket, an oil return port is formed in the upper portion of the jacket, the motor is fixed to the top of the kettle body, the stirring shaft is located in the kettle body, the stirring shaft is connected with a rotating shaft of the motor, and the stirring paddle is arranged on the lower portion of the stirring shaft. The invention takes heat conducting oil as a heating medium, can lead the heat conducting oil with different temperatures into the heat conducting oil cavity according to actual needs, is convenient to operate, and can adopt other heating modes including but not limited to steam and the like.

Preferably, the cauldron internal fixation has a section of thick bamboo of blockking, block a section of thick bamboo be located the stirring rake outside and with the coaxial setting of (mixing) shaft, the clearance that blocks between a section of thick bamboo and the cauldron internal wall forms baffling passageway, blocks to be equipped with a plurality of draft tubes along circumference interval on the section of thick bamboo, the draft tube is the round platform form, and the outer end opening diameter of draft tube is less than the inner opening diameter of draft tube. The material that blocks in the section of thick bamboo can be under the effect of stirring rake and to blocking a section of thick bamboo inner wall motion, can return to again along baffling the passageway from the draft tube after flowing out in, change the flow direction of material and form the sinuous flow, eliminate material layering phenomenon, still make the material form radial and ascending continuous circulation of axial simultaneously, be favorable to strengthening the mixing strength of material, make the material be heated and mix more evenly.

Preferably, the inner wall of the kettle body is provided with an annular arc guide plate at a position corresponding to the outer end opening of the guide cylinder, and the convex arc surface of the arc guide plate faces the guide cylinder. The arc-shaped guide plate plays a role in guiding flow, and materials flowing out of the guide cylinder can be guided to the upper side and the lower side of the deflection channel along the convex arc surface of the arc-shaped guide plate, so that the rebound and backflow of the materials are reduced.

Preferably, the inner wall of the kettle body is located at a position above the isolation cylinder, an annular baffle is arranged at a position above the isolation cylinder, the annular baffle is arranged in a downward inclined mode, an upper circulation port is formed in a gap between the upper end of the isolation cylinder and the annular baffle, a lower circulation port is formed in a gap between the lower end of the isolation cylinder and the kettle body, an annular guide folded plate bent downwards is arranged on the inner wall surface of the annular baffle, and the end portion of the annular guide folded plate is located in the isolation cylinder. When the stirring paddle is used for stirring, materials in the baffling channel can rise along the inner wall of the kettle body, so that the liquid level at the inner wall of the kettle body rises, the materials in the kettle body are in a state of being low in the middle and high around, and the materials are not uniformly mixed and heated.

As preferred, the annular baffle top is located to sulphuric acid cloth liquid structure, and sulphuric acid cloth liquid structure includes that the annular divides liquid pipe and dropping liquid pipe, the (mixing) shaft passes the annular and divides the liquid pipe, sulphuric acid inlet pipe and annular divide the liquid pipe to link to each other, the dropping liquid pipe is fixed in annular branch liquid pipe bottom and is divided the liquid pipe with the annular and be linked together along circumference interval. In the invention, the sulfuric acid is dripped into the material through the sulfuric acid liquid distribution structure, compared with the traditional single-tube feeding, the dripping of the sulfuric acid is more dispersed and uniform, the generation of a large amount of byproducts caused by local overheating of the material can be avoided, and the reaction of the 2B oil is more complete.

Preferably, the fractionating column comprises a liquid removing section and a fractionating section, the liquid removing section and the fractionating section are sequentially connected from bottom to top, a lower end inlet of the liquid removing section is connected with a gas phase discharge port of the reaction kettle, an upper end outlet of the liquid removing section is connected with a lower end inlet of the fractionating section, gas-liquid separation folded plates are fixed in the liquid removing section, the gas-liquid separation folded plates are longitudinally arranged at intervals, a bent gas channel is formed in a gap between the gas-liquid separation folded plates, an upper end outlet of the fractionating section is connected with an inlet of the vertical shell-tube condenser, a grid is fixed at the upper part in the fractionating section, a perforated plate is fixed at the lower part in the fractionating section, and a filler is filled between the grid and the perforated plate. The fractionating column comprises a liquid removing section and a fractionating section, wherein a gas-liquid separation folded plate is arranged in the liquid removing section, after a gas-phase material impacts the gas-liquid separation folded plate, the gas-liquid separation folded plate can capture and gather liquid drops in the rising gas-phase material, the working pressure of the fractionating section is favorably reduced, the situation that the rising gas-phase material directly impacts the fractionating section to influence the gas-liquid separation effect of the fractionating section can be avoided, in addition, a liquid phase flowing down from the fractionating section can flow down along the gas-liquid separation folded plate, and a gas phase can rise along a gas channel, so that the gas-liquid separation is realized.

Preferably, the perforated plate is provided with a gas lift pipe, the upper end of the gas lift pipe is closed, the lower end of the gas lift pipe is open and is communicated with the liquid removing section, and the outer circumferential surface of the gas lift pipe is provided with a plurality of gas outlet holes at intervals along the circumferential direction. Adopt the gas-lift pipe can effectively avoid the venthole to block up, can also make gas, liquid branch way and go simultaneously, the gaseous phase comes out from the gas-lift pipe, and the liquid phase then leaves from the aperture on the trompil board, and the gas-liquid looks mutual noninterference is favorable to improving the fractionation effect.

As preferred, the water knockout drum includes a jar body, the setting of water knockout drum inlet and water knockout drum balance mouth is at a jar body top, solvent discharge mouth sets up in the water knockout drum bottom, and internal baffle and lower baffle of being equipped with of jar, go up and be equipped with an isolation section of thick bamboo between baffle and the lower baffle, go up the space between baffle and the jar body top and form the surge chamber, the space between isolation section of thick bamboo and last baffle, lower baffle, the jar body forms the speed reduction chamber, and the space in the isolation section of thick bamboo forms the separation chamber, and the space between lower baffle and the jar body bottom forms the solvent chamber, the outlet sets up on separation chamber upper portion, goes up the baffle and is close to the edge and is equipped with the through-hole of a plurality of intercommunication surge chambers and speed reduction chamber along the circumference interval, is equipped with the discharge orifice along the circumference interval on the outer periphery of an isolation section of thick bamboo, and lies in the part of separation chamber bottom on the lower baffle and is equipped with the solvent hole of intercommunication separation chamber and solvent chamber. The structure of the water distributor is improved, and a plurality of independent functional spaces are formed in the water distributor through the upper partition plate, the lower partition plate and the partition cylinder; the condensate enters the separation chamber for layering after passing through the buffer chamber and the deceleration chamber, and the flow velocity of the condensate entering the separation chamber can be reduced through the deceleration and slow flow effects of the buffer chamber and the deceleration chamber, so that the impact and disturbance of the condensate on the boundary liquid surface in the separation chamber can be greatly reduced, and the separation efficiency and the separation effect can be improved; the water with lower density rises to the upper layer of the separation chamber and is discharged through the water outlet, the solvent with higher density is settled to the lower layer of the separation chamber and is discharged from the solvent discharge port and reflows to the kettle body; the solvent discharging port is arranged at the bottom of the water separator (solvent chamber) and can prevent the water on the upper layer from flowing back into the kettle body.

Preferably, an anti-impact funnel is arranged in the buffer chamber, and a liquid outlet pipe is connected to an outlet at the bottom of the anti-impact funnel; a circular truncated cone-shaped separating cylinder is arranged above the overflowing hole in the separating chamber, an overflow groove is formed in the space between the separating cylinder and the separating cylinder, and the water outlet is formed in the wall of the overflow groove; and a solvent settling hopper fixedly connected with the bottom surface of the lower isolation plate is arranged at the lower side of the solvent hole. The anti-impact funnel plays a role in buffering and concentrating condensate, the condensate is left from the liquid outlet pipe after being concentrated in the anti-impact funnel, and the falling condensate can be prevented from directly impacting the condensate in the water separator, so that impact and disturbance are reduced; the separating cylinder can prolong the separation and sedimentation time of water and the solvent, is beneficial to improving the separation effect, can reduce the entrainment of the solvent in water, and avoids the loss and waste of the solvent caused by the discharge of the solvent along with water; the sedimentation funnel plays a role in further concentrating and settling the solvent, so that the solvent in the solvent chamber is not easy to return to the separation chamber again when water is difficult to enter the solvent chamber, and the separation effect is ensured.

Therefore, the invention has the following beneficial effects:

(1) only one heating and stirring reaction kettle is used as a reaction container, the structure is simple, salification and dehydration transposition (sulfonation) are completed in the heating and stirring reaction kettle, the equipment is simple, the operation is very convenient, the production period is favorably shortened, and the 2B acid crude product can be obtained by pumping and filtering the reaction product, so that the energy consumption is low, the solvent can be recycled, and the production cost can be reduced;

(2) the kettle body structure of the heating and stirring reaction kettle is improved, so that materials in the kettle body can form continuous circulation in the radial direction and the axial direction, the material layering phenomenon is eliminated, the mixing strength of the materials is greatly enhanced, and the materials in the kettle body are heated and mixed more uniformly;

(3) the structure of the water separator is improved, a plurality of independent functional spaces are formed in the water separator through the upper partition plate, the lower partition plate and the partition cylinder, the impact and disturbance of condensate on a boundary liquid level can be greatly reduced, the entrainment of a solvent in water and the entrainment of water in the solvent can be reduced, and the separation efficiency and the separation effect are good;

(4) sulfuric acid is dripped into the material through a sulfuric acid cloth liquid structure, and compared with the traditional single tube feeding, the sulfuric acid dripping is more dispersed and uniform, so that a large amount of byproducts generated due to local overheating of the material can be avoided, and meanwhile, the 2B oil reaction is more complete.

Drawings

Fig. 1 is a schematic illustration of a connection according to the present invention.

FIG. 2 is a schematic diagram of a heated stirred tank reactor.

Fig. 3 is a top view of a sulfuric acid cloth fluid structure.

FIG. 4 is a schematic view of an internal structure of a fractionating column.

Figure 5 is a cross-sectional view of the water separator.

In the figure: a heating and stirring reaction kettle 1, a fractionating column 2, a vertical shell-and-tube condenser 3, a horizontal shell-and-tube condenser 4, a water separator 5, a gas phase discharge port 6 of the reaction kettle, a solvent return port 7, a discharge port 8 of the reaction kettle, a water separator liquid inlet 9, a water separator balance port 10, a solvent discharge port 11, a water discharge port 12, a sulfuric acid feed pipe 13, a kettle body 14, a jacket 15, a motor 16, a stirring shaft 17, a stirring paddle 18, a heat conducting oil cavity 19, an oil inlet 20, an oil return port 21, a blocking cylinder 22, a baffling channel 23, a guide cylinder 24, an arc-shaped guide plate 25, an annular baffle plate 26, an upper flow port 27, a lower flow port 28, an annular guide folded plate 29, an annular liquid dividing pipe 30, a liquid dropping pipe 31, a liquid removing section 32, a fractionating section 33, a gas-liquid separation folded plate 34, a gas channel 35, a grating 36, a perforated plate 37, a filler 38, a riser 39, a gas outlet 40, a tank body 41, an upper partition plate 42, a lower partition plate 43, an isolation cylinder 44, buffer chamber 45, speed reduction chamber 46, separation chamber 47, solvent chamber 48, through-hole 49, overflowing hole 50, solvent hole 51, anti-impact funnel 52, liquid outlet pipe 53, separation cylinder 54, overflow tank 55, solvent settling hopper 56, 2B oil storage tank 57, solvent storage tank 58, sulfuric acid metering tank 59, 2B oil inlet 60 and solvent inlet 61.

Detailed Description

The invention is further described with reference to the following figures and detailed description.

As shown in figure 1, a 2B acid crude product production system comprises a heating and stirring reaction kettle 1, a fractionating column 2, a vertical shell-tube condenser 3, a horizontal shell-tube condenser 4, a sulfuric acid liquid distribution structure, a water separator 5, a 2B oil storage tank 57, a solvent storage tank 58 and a sulfuric acid metering tank 59, wherein the heating and stirring reaction kettle comprises a kettle body 14, a jacket 15 and a stirring device (shown in figure 2), the top of the kettle body is provided with a gas phase discharge port 6 of the reaction kettle, a 2B oil inlet 60 and a solvent inlet 61, the 2B oil inlet is connected with the 2B oil storage tank through a pump and a pipeline, the solvent inlet is connected with the solvent storage tank through a pump and a pipeline, the upper part of the outer wall surface of the heating and stirring reaction kettle is provided with a solvent return port 7, the bottom of the heating and stirring reaction kettle is provided with a discharge port 8 of the reaction kettle, the stirring device comprises a motor 16, a stirring shaft 17 and a stirring paddle 18, the jacket is arranged outside the kettle body, a space between the jacket and the kettle body forms a heat conduction oil cavity 19, an oil inlet 20 is formed in the bottom of the jacket, an oil return port 21 is formed in the upper portion of the jacket, the motor is fixed to the top of the kettle body, the stirring shaft is located in the kettle body and connected with a rotating shaft of the motor, the stirring paddle is arranged on the lower portion of the stirring shaft, a blocking cylinder 22 is fixed in the kettle body and located outside the stirring paddle and coaxially arranged with the stirring shaft, a baffling channel 23 is formed in a gap between the blocking cylinder and the inner wall of the kettle body, a plurality of guide cylinders 24 are circumferentially arranged on the blocking cylinder at intervals, the guide cylinders are circular truncated cone-shaped, the diameter of outer end openings of the guide cylinders is smaller than that of inner end openings of the guide cylinders, annular arc-shaped guide plates 25 are arranged on the inner wall of the kettle body at positions corresponding to the outer end openings of the guide cylinders, and convex arc surfaces of the arc-shaped guide plates face the guide cylinders; an annular baffle 26 is arranged on the inner wall of the kettle body above the blocking cylinder, the annular baffle is arranged in a downward inclined mode, an upper circulation port 27 is formed in a gap between the upper end of the blocking cylinder and the annular baffle, a lower circulation port 28 is formed in a gap between the lower end of the blocking cylinder and the kettle body, an annular guide folded plate 29 bent downwards is arranged on the inner wall surface of the annular baffle, and the end portion of the annular guide folded plate is located in the blocking cylinder; the sulfuric acid liquid distribution structure is arranged above the annular baffle plate and comprises an annular liquid distribution pipe 30 and a liquid dropping pipe 31 (shown in figure 3), the stirring shaft penetrates through the annular liquid distribution pipe, the sulfuric acid feeding pipe is connected with the annular liquid distribution pipe, the liquid dropping pipes are fixed at the bottom of the annular liquid distribution pipe at intervals along the circumferential direction and are communicated with the annular liquid distribution pipe, the annular liquid distribution pipe is connected with a sulfuric acid feeding pipe 13, and the sulfuric acid feeding pipe is connected with a sulfuric acid metering tank 59 through a pipeline; the fractionating column comprises a liquid removing section 32 and a fractionating section 33, the liquid removing section and the fractionating section are sequentially connected from bottom to top, a lower end inlet of the liquid removing section is connected with a gas phase discharge port of the reaction kettle, an upper end outlet of the liquid removing section is connected with a lower end inlet of the fractionating section, a gas-liquid separation folded plate 34 (shown in figure 4) is fixed in the liquid removing section, the gas-liquid separation folded plate is longitudinally arranged at intervals, a bent gas channel 35 is formed in a gap between the gas-liquid separation folded plates, a grating 36 is fixed at the upper part in the fractionating section, a perforated plate 37 is fixed at the lower part in the fractionating section, a filler 38 is filled between the grating and the perforated plate, a gas rising pipe 39 is arranged on the perforated plate, the upper end of the gas rising pipe is closed, the lower end of the gas rising pipe is open and communicated with the liquid removing section, and a plurality of gas outlet holes 40 are circumferentially arranged on the outer circumferential surface of the gas rising pipe at intervals; an outlet at the upper end of the fractionation section is connected with an inlet of a vertical shell-and-tube condenser, and an outlet of the vertical shell-and-tube condenser is connected with an inlet of a horizontal condenser; the water separator comprises a tank body 41 (shown in figure 5), a water separator liquid inlet 9 and a water separator balance port 10 are arranged at the top of the tank body, a solvent discharging port 11 is arranged at the bottom of the tank body, the water separator balance port is connected with a balance port of a horizontal condenser through a pipeline, the solvent discharging port is connected with a solvent return port through a pipeline, an outlet of the horizontal condenser is connected with a water separator liquid inlet, an upper partition plate 42 and a lower partition plate 43 are arranged in the tank body, an isolation cylinder 44 is arranged between the upper partition plate and the lower partition plate, a buffer chamber 45 is formed in the space between the upper partition plate and the top of the tank body, an anti-impact funnel 52 is arranged in the buffer chamber, a liquid outlet pipe 53 is connected with the outlet at the bottom of the anti-impact funnel, a speed reduction chamber 46 is formed in the spaces between the isolation cylinder and the upper partition plate, the lower partition plate and the tank body, a separation chamber 47 is formed in the space in the isolation cylinder, a separation cylinder 54 in a truncated cone shape is arranged above an overflowing hole, and an overflow trough 55 is formed in the space between the separation cylinder, the wall of the overflow groove is provided with a water outlet 12, the space between the lower clapboard and the bottom of the tank body forms a solvent chamber 48, the water outlet is arranged at the upper part of the separation chamber, the edge of the upper clapboard close to the upper clapboard is provided with a plurality of through holes 49 which are communicated with the buffer chamber and the speed reduction chamber at intervals along the circumferential direction, the outer circumferential surface of the isolation cylinder is provided with overflowing holes 50 at intervals along the circumferential direction, the part of the lower clapboard at the bottom of the separation chamber is provided with solvent holes 51 which are communicated with the separation chamber and the solvent chamber, and the lower side of the solvent holes is provided with a solvent settling hopper 56 which is fixedly connected with the bottom surface of the lower clapboard.

The operation process of the invention is as follows: pumping a solvent and 2B oil into a kettle body of a heating and stirring reaction kettle, starting a stirring device and cooling water of a vertical shell-and-tube condenser and a horizontal shell-and-tube condenser, gradually dripping concentrated sulfuric acid (98%) into the kettle body, introducing heat conduction oil into a heat conduction oil cavity after the concentrated sulfuric acid is dripped, slowly heating to a required salt forming temperature (about 90 ℃), heating to a sulfonation temperature (200-210 ℃) after reacting for a period of time, carrying out heat preservation reaction, discharging the solvent at the bottom in a water separator from a solvent discharge port, returning the solvent to the kettle body through a solvent return port, and timely discharging water in a water collection tank in the water separator; after the reaction is carried out for a certain time under the condition of heat preservation, the reaction is stopped, the temperature is reduced (below 50 ℃), and the reactants in the kettle are discharged from a discharge hole of the reaction kettle and then are filtered, so as to obtain the crude product of the 2B acid.

The above-described embodiments are only preferred embodiments of the present invention, and are not intended to limit the present invention in any way, and other variations and modifications may be made without departing from the spirit of the invention as set forth in the claims.

Claims

1. A2B acid crude product production system is characterized by comprising a heating and stirring reaction kettle (1), a fractionating column (2), a vertical shell-and-tube condenser (3), a horizontal shell-and-tube condenser (4), a sulfuric acid liquid distribution structure and a water distributor (5), wherein a reaction kettle gas-phase discharge port (6) is arranged at the top of the heating and stirring reaction kettle, a solvent return port (7) is arranged at the upper part of the outer wall surface of the heating and stirring reaction kettle, a reaction kettle discharge port (8) is arranged at the bottom of the heating and stirring reaction kettle, a water distributor liquid inlet (9) and a water distributor balance port (10) are arranged at the top of the water distributor, a solvent discharge port (11) is arranged at the bottom of the water distributor, a water outlet (12) is arranged at the upper part of the outer wall surface of the water distributor, the inlet at the lower end of the fractionating column is connected with the reaction kettle gas-phase discharge port, the outlet at the upper end of the fractionating column is connected with the inlet of the vertical shell-and-tube condenser, the outlet of the vertical shell-and-tube condenser is connected with the inlet of the horizontal condenser, the outlet of the horizontal condenser is connected with the liquid inlet of the water separator, the solvent discharging port is connected with the solvent backflow port, and the balance port of the water separator is connected with the balance port of the horizontal condenser; the sulfuric acid liquid distribution structure is arranged above the interior of the heating and stirring reaction kettle and is connected with a sulfuric acid feeding pipe (13).

2. The crude 2B acid production system according to claim 1, wherein the heating and stirring reaction kettle comprises a kettle body (14), a jacket (15) and a stirring device, the stirring device comprises a motor (16), a stirring shaft (17) and a stirring paddle (18), the jacket is arranged outside the kettle body, a heat conducting oil cavity (19) is formed in a space between the jacket and the kettle body, an oil inlet (20) is formed in the bottom of the jacket, an oil return opening (21) is formed in the upper portion of the jacket, the motor is fixed to the top of the kettle body, the stirring shaft is located in the kettle body, the stirring shaft is connected with a rotating shaft of the motor, and the stirring paddle is arranged at the lower portion of the stirring shaft.

3. The 2B acid crude product production system according to claim 2, wherein a blocking cylinder (22) is fixed in the kettle body, the blocking cylinder is positioned outside the stirring paddle and is coaxially arranged with the stirring shaft, a baffling channel (23) is formed in a gap between the blocking cylinder and the inner wall of the kettle body, a plurality of guide cylinders (24) are arranged on the blocking cylinder at intervals along the circumferential direction, the guide cylinders are in a circular truncated cone shape, and the opening diameter of the outer ends of the guide cylinders is smaller than that of the inner ends of the guide cylinders.

4. The crude 2B acid production system according to claim 3, wherein an annular arc-shaped guide plate (25) is arranged on the inner wall of the kettle body at a position corresponding to the outer end opening of the guide cylinder, and the convex arc surface of the arc-shaped guide plate faces the guide cylinder.

5. The 2B acid crude product production system according to claim 3 or 4, wherein an annular baffle (26) is arranged on the inner wall of the kettle body at a position above the blocking cylinder, the annular baffle is arranged in a downward inclined manner, an upper circulation port (27) is formed in a gap between the upper end of the blocking cylinder and the annular baffle, a lower circulation port (28) is formed in a gap between the lower end of the blocking cylinder and the kettle body, an annular guide folded plate (29) bent downwards is arranged on the inner wall surface of the annular baffle, and the end part of the annular guide folded plate is positioned in the blocking cylinder.

6. The crude 2B acid production system according to claim 2, wherein the sulfuric acid distribution structure is arranged above the annular baffle, the sulfuric acid distribution structure comprises an annular liquid distribution pipe (30) and a liquid dropping pipe (31), the stirring shaft penetrates through the annular liquid distribution pipe, the sulfuric acid feeding pipe is connected with the annular liquid distribution pipe, and the liquid dropping pipe is fixed at the bottom of the annular liquid distribution pipe along the circumferential direction at intervals and is communicated with the annular liquid distribution pipe.

7. The crude 2B acid production system according to claim 1, wherein the fractionating column comprises a liquid removing section (32) and a fractionating section (33), the liquid removing section and the fractionating section are sequentially connected from bottom to top, a lower inlet of the liquid removing section is connected with a gas phase discharge port of the reaction kettle, an upper outlet of the liquid removing section is connected with a lower inlet of the fractionating section, gas-liquid separating folded plates (34) are fixed in the liquid removing section, the gas-liquid separating folded plates are longitudinally arranged at intervals, a bent gas channel (35) is formed in a gap between the gas-liquid separating folded plates, an upper outlet of the fractionating section is connected with an inlet of the vertical shell-and-tube condenser, a grid (36) is fixed at the upper part in the fractionating section, a perforated plate (37) is fixed at the lower part in the fractionating section, and a filler (38) is filled between the grid and the perforated plate.

8. The crude 2B acid production system according to claim 7, wherein said perforated plate is provided with a gas lift tube (39), the upper end of said gas lift tube is closed, the lower end of said gas lift tube is open and is communicated with the liquid removal section, and the outer circumferential surface of said gas lift tube is provided with a plurality of gas outlets (40) at intervals along the circumferential direction.

9. The crude 2B acid production system according to claim 1, wherein the water separator comprises a tank body (41), the water inlet and the balance port of the water separator are arranged at the top of the tank body, the solvent discharge port is arranged at the bottom of the water separator, an upper partition plate (42) and a lower partition plate (43) are arranged in the tank body, a separation cylinder (44) is arranged between the upper partition plate and the lower partition plate, a buffer chamber (45) is formed in the space between the upper partition plate and the top of the tank body, a speed reduction chamber (46) is formed in the spaces between the separation cylinder and the upper partition plate, between the separation cylinder and the tank body, a separation chamber (47) is formed in the space between the lower partition plate and the bottom of the tank body, a solvent chamber (48) is formed in the space between the lower partition plate and the bottom of the tank body, the water outlet is arranged at the upper part of the separation chamber, and a plurality of through holes (49) communicating the buffer chamber and the speed reduction chamber are arranged at intervals along the circumferential direction near the edge of the upper partition plate, the outer circumference of the isolation cylinder is provided with overflowing holes (50) at intervals along the circumferential direction, and the part of the lower partition plate positioned at the bottom of the separation chamber is provided with solvent holes (51) for communicating the separation chamber and the solvent chamber.

10. The crude 2B acid production system according to claim 9, wherein an anti-impact funnel (52) is arranged in the buffer chamber, and a liquid outlet pipe (53) is connected to an outlet at the bottom of the anti-impact funnel; a separating cylinder (54) in a circular truncated cone shape is arranged above the overflowing hole in the separating chamber, an overflow groove (55) is formed in the space between the separating cylinder and the separating cylinder, and the water outlet is formed in the wall of the overflow groove; and a solvent settling hopper (56) fixedly connected with the bottom surface of the lower isolation plate is arranged at the lower side of the solvent hole.