Separation equipment and process for water washing and alkali washing liquid of dinitrate product

Abstract

The invention relates to the technical field of separation and purification, and provides dinitrate product water washing and alkali washing liquid separation equipment and technology.The equipment comprises a dinitrate oil separation tank, the dinitrate oil separation tank is connected with a first-stage water washing kettle and a dinitrate waste acid tank through pipelines, the first-stage water washing kettle is connected with a first-stage water washing separation tank through a pipeline, and the second-stage water washing separation tank is connected with a second-stage waste acid tank through a pipeline; the first-stage washing separation tank is respectively connected with a second-stage washing kettle and a wastewater neutralization kettle through pipelines, the second-stage washing kettle is connected with a second-stage washing separation tank through a pipeline, the wastewater neutralization kettle is connected with a washing brine tank through a pipeline, and the second-stage washing separation tank is respectively connected with a second-stage washing wastewater tank and an alkali washing kettle through pipelines; and the alkali washing kettle is connected with an alkali washing separation tank through a pipeline. According to the technical scheme, the problems that existing alkali washing liquid separation equipment usually separates liquid through other technical means, but separated waste liquid is not recycled, certain pollution is caused, and more manpower and material resources are paid for solving the pollution are solved.

Description

Technical Field

[0001] The invention relates to the technical field of separation and purification, and in particular to a dinitro product water washing and alkali washing liquid separation device and process. Background Art

[0002] The main components of the material after the dinitrogen reaction are the acid phase and the mixed liquid phase of dinitrochlorobenzene. Dinitrochlorobenzene needs to be obtained through separation technology, mainly through alkali washing technology to achieve liquid separation, and finally obtain high-quality dinitrochlorobenzene. Dinitrochlorobenzene has a good application in the field of medicine. Dinitrochlorobenzene is a hapten and can be covalently combined with the soluble part of epithelial protein to become a complete antigen; After searching, the application publication number is CN110270290A, which discloses a continuous washing device and a continuous water washing and alkali washing method and its application. Through the device and method of the invention, continuous water washing and alkali washing can be achieved, thereby shortening the production cycle, improving production efficiency, and increasing product yield; However, the above-mentioned existing alkaline washing liquid separation equipment usually separates the liquid through other technical means, but the waste liquid after separation is not recycled and reused, which not only causes certain pollution, but also requires more manpower and material resources to solve the pollution. For this reason, we propose a dinitro product water washing and alkaline washing liquid separation equipment and process. Summary of the invention

[0003] The present invention proposes a dinitrate product water washing and alkali washing liquid separation device and process, which solves the problem mentioned in the background technology that the existing alkali washing liquid separation equipment usually separates the liquid by other technical means, but the separated waste liquid is not recycled and reused, which not only causes certain pollution, but also requires more manpower and material resources to solve the pollution.

[0004] The technical solution of the present invention is as follows: A dinitrate product water washing and alkali washing liquid separation device comprises a dinitrate nitrate oil separation tank, wherein the dinitrate nitrate oil separation tank is respectively connected to a primary water washing kettle and a dinitrate waste acid tank through pipelines, the primary water washing kettle is connected to a primary water washing separation tank through pipelines, the primary water washing separation tank is respectively connected to a secondary water washing kettle and a wastewater neutralization kettle through pipelines, the secondary water washing kettle is connected to a secondary water washing separation tank through pipelines, the wastewater neutralization kettle is connected to a washing brine tank through pipelines, the secondary water washing separation tank is respectively connected to a secondary water washing wastewater tank and an alkali washing kettle through pipelines, the alkali washing kettle is connected to an alkali washing separation tank through pipelines, the alkali washing separation tank is respectively connected to an alkali washing wastewater tank and a dinitrate transfer tank through pipelines, the secondary water washing wastewater tank is connected to the primary water washing kettle through pipelines, and the alkali washing wastewater tank and the secondary water washing kettle are connected through pipelines.

[0005] As a further technical solution of the present invention, the dinitrate nitrate oil separation tank is used to receive the material after the dinitrate reaction is cooled, and the upper layer of the dinitrate nitrate oil separation tank enters the primary water washing kettle, and the lower layer of the material enters the dinitrate waste acid tank; The water washing control temperature of the first-stage water washing kettle is 55°C, and circulating cooling water (green line) is introduced through the coil fixed inside the first-stage water washing kettle - in from the upper left and out from the lower right, and low-pressure steam is introduced into the outer half pipe; The primary water washing separation tank is used to receive the overflow of the primary water washing kettle, and the upper layer of wastewater in the primary water washing separation tank flows to the wastewater neutralization kettle by gravity, and the lower layer flows into the secondary water washing kettle; Steam is introduced into the outer half of the secondary water washing kettle to control the temperature at 55°C to further remove the acid in the material; The secondary water washing separation tank is used to receive the liquid material overflowing from the secondary water washing kettle and perform stratification, the upper layer of material enters the secondary water washing wastewater tank, and the material enters the alkali washing kettle; The alkali washing kettle is temperature controlled by introducing steam through the outer half pipe, so as to further remove acid and water from the material and improve the purity of the product; The alkali washing separation tank is introduced with steam through the outer half pipe to control the temperature, and the upper layer flows by gravity to the alkali washing wastewater tank, and the lower layer flows by gravity into the dinitrate transfer tank; The water jacket in the alkaline washing wastewater tank is used for the secondary washing kettle water washing process; The dinitrate transfer tank is used to store the separated liquid.

[0006] As a further technical solution of the present invention, the material in the dinitrate waste acid tank is used as a raw material for the mononitrate reaction; The wastewater neutralization kettle is used to receive the upper liquid of the primary water washing separation tank and quantitatively add 50% sodium hydroxide for neutralization; The washing brine tank is used to receive the liquid material after neutralization in the wastewater and the liquid material after neutralization in the kettle, and is used as bottom water by pumping sulphur black production; The alkali washing kettle is connected to a soda ash dissolving kettle through a pipeline, and the soda ash dissolving kettle is used to prepare alkali washing water for alkali washing of the alkali washing kettle; The material in the secondary washing wastewater tank is pumped into the primary washing kettle and used as washing water.

[0007] As a further technical solution of the present invention, the dinitro transfer tank is pumped into the dinitrochlorobenzene 95 finished product tank in the tank area or pumped into a crystallizer for crystallization and purification.

[0008] As a further technical solution of the present invention, the dinitrogen nitrate oil separation tank includes an outer shell, a variable frequency air pump and a water pump, two sets of sight glasses are arranged on the surface of the outer shell, a coil is arranged inside the outer shell, a promotion structure is arranged inside the outer shell, and an adjustment structure is connected between the coil and the outer shell.

[0009] As a further technical solution of the present invention, the promoting structure includes a rotating shaft rotatably connected to the axis center of the outer shell, the surface of the rotating shaft is movably sleeved with a rotating part, the surface of the outer shell is connected through a No. 1 sleeve, the interior of the No. 1 sleeve is movably connected with a movable tube, the surface of the outer shell is fixedly connected to a main motor corresponding to the top of the rotating shaft, the surface of the rotating part is rotatably connected with a rotating ring, the lower end of the rotating ring is provided with a connecting hole, the connecting hole is connected to the movable tube and the interior of the rotating part, the surface of the rotating part is fixedly connected with a stirring plate, the surface of the stirring plate is fixedly connected with a one-way ventilation valve, and the surface of the rotating shaft is fixedly connected with a convex strip.

[0010] As a further technical solution of the present invention, the adjustment structure includes an annular tube fixedly connected to both ends of the coil, a No. 2 sleeve is fixedly connected to the surface of the annular tube, an inlet pipe is movably sleeved on the inner side of the upper end of the No. 2 sleeve, a No. 1 plate is fixedly connected to the surface of the No. 2 sleeve, a No. 2 plate is fixedly connected to the surface of the inlet pipe, and a support spring is connected between the No. 2 plate and the No. 1 plate.

[0011] As a further technical solution of the present invention, a rotation connection is formed between the rotating shaft and the outer shell through a bearing, the rotating shaft and the convex strip both penetrate the rotating part, the rotating part slides along the length direction of the rotating shaft, the outer surface of the rotating shaft is kept stable by a bracket near the lower end, the outer diameter of the movable tube is equal to the inner diameter of the No. 1 sleeve, the movable tube and the No. 1 sleeve are in a sliding connection, the main motor is a variable frequency motor, the output end of the variable frequency air pump is connected to the top of the No. 1 sleeve, the rotating part is driven to rotate together with the stirring plate through the rotation of the rotating shaft, the stirring plate is connected to the interior of the rotating part, the airflow direction of the one-way vent valve is from the inside of the stirring plate to the outside of the one-way vent valve, the movable tube and the rotating ring are fixedly connected, and the rotating ring and the rotating part are rotationally connected.

[0012] As a further technical solution of the present invention, the inlet pipe is used to pass hot water, and the surface of the ring pipe corresponding to the lower end of the coil is also connected to a group for connecting to a drainage pipe for drainage. The structure of the connection between the drainage pipe and the ring pipe is the same as the structure of the connection between the inlet pipe and the ring pipe. The upper and lower ends of the support spring are fixedly connected to the No. 2 plate and the No. 1 plate respectively. The No. 2 sleeve slides up and down along the inlet pipe, and the downward movement of the ring pipe together with the coil is realized by the hot water impacting the conical plate.

[0013] The present invention also includes a dinitrate product water washing and alkali washing liquid separation equipment treatment process, the treatment process comprises the following steps: S1. After the dinitration reaction is completed and cooled, the material flows into the dinitrification oil separation tank by gravity using the potential difference of the equipment, and is continuously layered under normal pressure. The acid phase in the lower layer is dinitrification waste acid, the main components of which are sulfuric acid and a small amount of nitric acid. It flows into the dinitrification waste acid tank by gravity using the potential difference of the equipment, and is used as the raw material for the mononitrification reaction; The main components of the organic phase in the upper layer are dinitrochlorobenzene and a small amount of sulfuric acid and nitric acid, which enter the primary water washing kettle. The primary water washing kettle can be introduced into the circulating water through the coil or the steam through the outer half pipe to control the temperature between 46℃-85℃ to remove the acid in the material; S2. The primary washing kettle is charged with 1 ton of dinitrate and 1 ton of water, and the material is washed at the primary level. At this time, the wash water is the secondary wash wastewater; After washing in the primary washing kettle, the material overflows to the primary washing separation tank. When entering this step, steam can be introduced through the outer half pipe to control the temperature between 46°C and 85°C to prevent the material from crystallizing. The material is continuously stratified in the primary washing separation tank. After stratification, the upper aqueous phase is acidic wastewater, which flows into the wastewater neutralization kettle by potential difference. 50% sodium hydroxide is quantitatively added to the wastewater neutralization kettle at the same time until the amount of sodium hydroxide added makes the pH value of the neutralized wastewater between 6 and 12. The neutralized wastewater contains 6% sodium nitrate and about 2% sodium sulfate. Then it enters the washing brine tank and is pumped out to sulfide black production as bottom water; The lower organic phase in the primary water washing separation tank is mainly composed of dinitrochlorobenzene and trace amounts of sulfuric acid and nitric acid. It enters the secondary water washing kettle and is washed again after steam is introduced through the outer half pipe to control the temperature between 46°C and 85°C. At this time, this part of the washing water is alkaline washing wastewater, which is used to further remove the acid in the material; After that, the materials in the secondary water washing kettle overflow to the secondary water washing separation tank. The temperature can be controlled between 46℃ and 85℃ by introducing steam through the outer half pipe. The materials are continuously stratified in the secondary water washing separation tank. After stratification, the upper water phase is acid-containing wastewater, which flows into the secondary water washing wastewater tank by gravity and is pumped into the primary water washing kettle for use as water for washing. The main components of the lower organic phase are dinitrochlorobenzene and trace amounts of sulfuric acid and nitric acid. It enters the soda ash dissolution kettle and introduces steam through the outer half pipe to control the temperature between 30℃-60℃ for further deacidification treatment to further remove the acid and water in the material and improve the purity of the product.

[0014] S3. The material in the soda ash dissolving kettle is a sodium carbonate solution of about 15%. First, 99.5% solid powdered sodium carbonate is quantitatively added to the outlet of the soda ash dissolving kettle, and the pH is controlled at 7-11. At the same time, a certain amount of fresh water is metered and pumped in, and the stirring system is turned on. The solid sodium carbonate is dissolved at about 40°C and normal pressure. After the dissolution, the sodium carbonate solution is pumped into the alkali washing kettle for use as alkali washing water, and two soda ash dissolving kettles are used alternately as storage tanks; S4. Steam is introduced into the soda ash dissolution kettle to heat and dissolve, and the temperature is controlled at 30°C-60°C; S5. After the alkali washing water in the soda ash dissolving kettle is pumped into the alkali washing kettle, the alkali washing is maintained under normal pressure stirring conditions, and the feed liquid overflows into the alkali washing separation tank for automatic stratification. During the stratification process, steam is introduced through an external accompanying pipe to control the temperature to 46°C-85°C. After stratification, the upper aqueous phase is the alkali washing wastewater, which flows into the alkali washing wastewater tank by gravity and is transported to the secondary water washing kettle water washing process by a pump; The lower organic phase is 95% of 2,4-dinitrochlorobenzene, and the remaining 5% is a mixture of 2,6-dinitrochlorobenzene, 3,5-dinitrochlorobenzene and a small amount of water, which flows into the dinitro transfer tank by gravity. The dinitro transfer tank is heated at 55℃-60℃ by steam introduced through an external coil. Finally, it is pumped into the dinitrochlorobenzene 95 finished product tank in the tank area or pumped into a crystallizer for crystallization and purification to complete separation and purification.

[0015] The working principle and beneficial effects of the present invention are: The four-stage water washing separation in the equipment of the present invention can make the liquid material be fully washed with water to achieve efficient separation. At the same time, the waste generated in the water washing process can be recycled and reused, or used for subsequent processing in other production. While achieving efficient water washing and separation, the generation of waste can be greatly reduced and the waste can be recycled.

[0016] The separation and treatment process provided in the method of the present invention can effectively improve the purity of the feed liquid during the separation process, thereby being able to meet the subsequent high-quality purification needs of different users. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] The present invention will be further described in detail below in conjunction with the accompanying drawings and specific embodiments.

[0018] Figure 1 It is a flow chart of the equipment of the present invention; Figure 2 It is a structural diagram of the dinitro nitrate oil separation tank of the present invention; Figure 3 It is a schematic diagram of the local structure of the promoting structure of the present invention; Figure 4 For the present invention Figure 3 Schematic diagram of the local structure; Figure 5 It is a schematic diagram of a partial structure of a rotating member cut away in the present invention; Figure 6 It is a schematic diagram of the local structure of the coil of the present invention; Figure 7 It is a schematic diagram of the local structure of the regulating structure of the present invention; Figure 8 For the present invention Figure 7 Schematic diagram of the cutaway partial structure.

[0019] In the figure: 1. Dinitrate nitrate oil separation tank; 2. Primary water washing kettle; 3. Dinitrate waste acid tank; 4. Primary water washing separation tank; 5. Secondary water washing kettle; 6. Wastewater neutralization kettle; 7. Secondary water washing separation tank; 8. Washing brine tank; 9. Secondary water washing wastewater tank; 10. Alkali washing kettle; 11. Alkali washing separation tank; 12. Soda ash dissolving kettle; 13. Alkali washing wastewater tank; 14. Dinitrate transfer tank; 15. Shell; 16. Frequency conversion air pump; 17. Water pump; 18. Sight glass; 19. Coil; 20. Promotion structure; 201. Rotating shaft; 202. Rotating member; 203. No. 1 sleeve; 204. Main motor; 205. Movable tube; 206. Rotating ring; 207. Connecting hole; 208. Stirring plate; 209. One-way vent valve; 210. Raised strip; 21. Adjusting structure; 211. Ring pipe; 212. No. 2 casing; 213. Inlet pipe; 214. No. 1 plate; 215. No. 2 plate; 216. Support spring; 217. Conical plate. DETAILED DESCRIPTION

[0020] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention. Example 1

[0021] like Figure 1 As shown, this embodiment proposes a dinitrate product water washing and alkali washing liquid separation equipment, including a dinitrate nitrate oil separation tank 1, the dinitrate nitrate oil separation tank 1 is connected to a primary water washing kettle 2 and a dinitrate waste acid tank 3 through pipelines, the primary water washing kettle 2 is connected to a primary water washing separation tank 4 through pipelines, the primary water washing separation tank 4 is connected to a secondary water washing kettle 5 and a wastewater neutralization kettle 6 through pipelines, the secondary water washing kettle 5 is connected to a secondary water washing separation tank 7 through pipelines, the wastewater neutralization kettle 6 is connected to a washing brine tank 8 through pipelines, the secondary water washing separation tank 7 is connected to a secondary water washing wastewater tank 9 and an alkali washing kettle 10 through pipelines, the alkali washing kettle 10 is connected to an alkali washing separation tank 11 through pipelines, the alkali washing separation tank 11 is connected to an alkali washing wastewater tank 13 and a dinitrate transfer tank 14 through pipelines, the secondary water washing wastewater tank 9 is connected to the primary water washing kettle 2 through pipelines, and the alkali washing wastewater tank 13 is connected to the secondary water washing kettle 5 through pipelines.

[0022] The dinitrate nitrate oil separation tank 1 is used to receive the material after the dinitrate reaction is cooled, and the upper layer of the dinitrate nitrate oil separation tank 1 enters the primary water washing kettle 2, and the lower layer of the material enters the dinitrate waste acid tank 3; the water washing control temperature of the primary water washing kettle 2 is 55°C, and the circulating cooling water green line-in the upper left and out the lower right is introduced through the coil 19 fixedly arranged inside the primary water washing kettle 2, and low-pressure steam is introduced into the outer half pipe; the primary water washing separation tank 4 is used to receive the overflow of the primary water washing kettle 2, and the upper layer of waste water inside the primary water washing separation tank 4 flows by gravity to the wastewater neutralization kettle 6, and the lower layer flows into the secondary water washing kettle 5; the steam is introduced into the outer half pipe of the secondary water washing kettle 5 to control the temperature The temperature of the alkali washing separation tank is 55°C, which is used to further remove the acid in the material; the secondary water washing separation tank 7 is used to receive the liquid material overflowing from the secondary water washing kettle 5 and to separate them into layers. The upper layer of the material enters the secondary water washing wastewater tank 9, and the material enters the alkali washing kettle 10; the alkali washing kettle 10 is introduced with steam through the outer half pipe to control the temperature, which is used to further remove the acid and water in the material and improve the purity of the product; the alkali washing separation tank 11 is introduced with steam through the outer half pipe to control the temperature, and the upper layer flows by gravity to the alkali washing wastewater tank 13, and the lower layer flows by gravity into the dinitrate transfer tank 14; the water jacket in the alkali washing wastewater tank 13 is used for the water washing process of the secondary water washing kettle 5; the dinitrate transfer tank 14 is used to store the separated liquid.

[0023] The material in the dinitrate waste acid tank 3 is used as the raw material for the mononitrate reaction; the wastewater neutralization kettle 6 is used to receive the upper liquid of the primary water washing separation tank 4 and quantitatively add 50% sodium hydroxide for neutralization; the washing brine tank 8 is used to receive the liquid material after neutralization in the wastewater neutralization kettle 6, and pumps it into sulfide black production as bottom water; the alkali washing kettle 10 is connected to the soda ash dissolving kettle 12 through a pipeline, and the soda ash dissolving kettle 12 is used to prepare alkali washing water for alkali washing of the alkali washing kettle 10; the material in the secondary water washing wastewater tank 9 is pumped into the primary water washing kettle 2 and used as washing water.

[0024] The dinitro transfer tank 14 is pumped into the dinitrochlorobenzene 95 finished product tank in the tank area or into the crystallizer for crystallization and purification.

[0025] In this embodiment, the liquid material can be fully washed with water to achieve efficient separation. At the same time, the waste generated during the washing process can be recycled and reused, or used for subsequent processing in other production. While efficient washing and separation, the generation of waste can be greatly reduced and the waste can be recycled. Example 2

[0026] like Figure 2~Figure 5 As shown, on the basis of Example 1, a dinitrogen nitrate oil separation tank 1 is proposed, which includes a shell 15, a variable frequency air pump 16 and a water pump 17. Two sets of sight glasses 18 are arranged on the surface of the shell 15, a coil 19 is arranged inside the shell 15, a promotion structure 20 is arranged inside the shell 15, and an adjustment structure 21 is connected between the coil 19 and the shell 15.

[0027] The promoting structure 20 includes a rotating shaft 201 rotatably connected to the axis center of the outer shell 15, a rotating part 202 is movably sleeved on the surface of the rotating shaft 201, a No. 1 sleeve 203 is penetrated and connected to the surface of the outer shell 15, and a movable tube 205 is movably connected inside the No. 1 sleeve 203, a main motor 204 is fixedly connected to the top of the rotating shaft 201 on the surface of the outer shell 15, a rotating ring 206 is rotatably connected to the surface of the rotating part 202, a connecting hole 207 is opened at the lower end of the rotating ring 206, the connecting hole 207 is connected to the movable tube 205 and the inside of the rotating part 202, a stirring plate 208 is fixedly connected to the surface of the rotating part 202, a one-way air valve 209 is fixedly connected to the surface of the stirring plate 208, and a convex strip 210 is fixedly connected to the surface of the rotating shaft 201.

[0028] The rotating shaft 201 and the housing 15 are rotatably connected by a bearing. The rotating shaft 201 and the convex strip 210 are both inserted into the rotating member 202. The rotating member 202 slides along the length direction of the rotating shaft 201. The outer surface of the rotating shaft 201 is kept stable by a bracket near the lower end. The outer diameter of the movable tube 205 is equal to the inner diameter of the No. 1 sleeve 203. The movable tube 205 and the No. 1 sleeve 203 are slidably connected. The main motor 204 is a variable frequency motor. The output end of the variable frequency air pump 16 is connected to the top of the No. 1 sleeve 203. The rotating member 202 is driven to rotate together with the stirring plate 208 through the rotation of the rotating shaft 201. The stirring plate 208 is connected to the inside of the rotating member 202. The airflow direction of the one-way vent valve 209 is from the inside of the stirring plate 208 to the outside of the one-way vent valve 209. The movable tube 205 and the rotating ring 206 are fixedly connected, and the rotating ring 206 and the rotating member 202 are rotatably connected.

[0029] In this embodiment, during the use of the dinitrate nitrate oil separation tank 1, the interior of the shell 15 is automatically and continuously stratified. The main motor 204 can drive the rotating shaft 201 together with the convex strip 210 to rotate clockwise. The rotation of the rotating shaft 201 can drive the rotating member 202 to rotate accordingly. The rotating member 202 drives the stirring plate 208 to rotate accordingly, thereby mixing and stirring the liquid inside the dinitrate nitrate oil separation tank 1. At the same time, under the rotation of the stirring plate 208, the water flow will be blown downward, and the rotating member 202 will be pushed upward along the rotating shaft 201 in the opposite direction, so that different areas inside the shell 15 can be stirred, thereby quickly promoting the generation of stratification. During the rotation of the rotating member 202, the rotating ring 206 does not rotate, and the rotating member 202 and the rotating ring 206 rotate relative to each other. During the upward movement of the rotating member 202, the rotating ring 206 will follow the upward movement, and the movable tube 205 will be pushed upward by the rotating ring 206. During this process, the variable frequency air pump 16 injects air into the top of the No. 1 sleeve 203, and the airflow is filled into the rotating ring 206 through the movable tube 205, and then enters the rotating member 202, and then enters the inside of the stirring plate 208 through the rotating member 202, and finally blows out through the one-way vent valve 209. An appropriate amount of bubbles can quickly promote the rapid stratification of the liquid inside the shell 15. It should be noted that during use, gas can be discharged through the exhaust hole. At the same time, the rotating shaft 201 is driven to rotate so that the rotating ring 206 and the lower end of the No. 1 sleeve 203 are moved to the maximum distance, and the rotating shaft 201 can be driven to rotate in the reverse direction by the main motor 204 to realize the downward movement of the rotating member 202. The frequency of the main motor 204 can also be adjusted as needed to realize the adjustment of the rotation height of the rotating member 202. At the same time, when not in use, the stirring plate 208 together with the rotating member 202 and other components can be naturally dropped to the lowest end, and the rotating member 202 can be supported by the bracket of the lower end positioning rotating shaft 201; It should be noted that during use, the structure for stirring to promote stratification and the structure for introducing airflow to promote stratification can be operated separately as needed. Stirring can be performed separately, ventilation can be performed separately, or ventilation can be performed while stirring according to user needs to promote stratification. Example 3

[0030] like Figure 6~Figure 8 As shown, on the basis of Example 2, it is further proposed that the adjustment structure 21 includes an annular tube 211 fixedly connected to the two ends of the coil 19, a No. 2 sleeve 212 is fixedly connected to the surface of the annular tube 211, an inlet pipe 213 is movably sleeved on the inner side of the upper end of the No. 2 sleeve 212, a No. 1 plate 214 is fixedly connected to the surface of the No. 2 sleeve 212, a No. 2 plate 215 is fixedly connected to the surface of the inlet pipe 213, and a support spring 216 is connected between the No. 2 plate 215 and the No. 1 plate 214.

[0031] The inlet pipe 213 is used to introduce hot water. The surface of the ring pipe 211 corresponding to the lower end of the coil 19 is also connected with a group for connecting to the drainage pipe for drainage. The structure of the connection between the drainage pipe and the ring pipe 211 is the same as the structure of the connection between the inlet pipe 213 and the ring pipe 211. The upper and lower ends of the support spring 216 are fixedly connected to the second plate 215 and the first plate 214 respectively. The second sleeve 212 slides up and down along the inlet pipe 213, and the hot water impacts the conical plate 217 to realize the downward movement of the ring pipe 211 together with the coil 19.

[0032] In this embodiment, during use, the water pump 17 can inject hot water of the required temperature into the interior of the inlet pipe 213, enter the interior of the No. 2 casing 212 through the inlet pipe 213, and finally enter the interior of the coil 19 through the ring pipe 211 to adjust the temperature. In this process, the hot water will first impact the conical plate 217, thereby pushing the conical plate 217 to connect the No. 2 casing 212 to move downward, and the No. 2 casing 212, the ring pipe 211 and the coil 19 will move downward for a distance, so that the feed liquid in different areas is heated. With the function of the stirring part of the promotion structure 20, the heating can be quickly uniformed, and then the temperature of the liquid inside the shell 15 can be quickly uniformed. At the same time, the working frequency of the water pump 17 can be adjusted as needed, so that hot water flows at different speeds inside the second casing 212. Due to the different impact forces of the hot water flow on the conical plate 217, the downward movement distance of the second casing 212, the annular tube 211 and the coil 19 can be adjusted to better heat the liquid inside the outer shell 15 and achieve a better temperature control effect.

[0033] It should be noted that when hot water is no longer injected into the inlet pipe 213, the support spring 216 can play a reset role, driving the coil 19 to move to the initial position.

[0034] The present invention also proposes a dinitro product water washing and alkali washing liquid separation equipment treatment process, the treatment process comprises the following steps: S1. After the dinitration reaction is completed and cooled, the material flows into the dinitrification oil separation tank 1 by gravity using the potential difference of the equipment, and is continuously layered under normal pressure conditions, wherein the acid phase of the lower layer is dinitrification waste acid, the main components of which are sulfuric acid and a small amount of nitric acid, and flows into the dinitrification waste acid tank 3 by gravity using the potential difference of the equipment, and is used as a raw material for the mononitrification reaction; The main components of the organic phase in the upper layer are dinitrochlorobenzene and a small amount of sulfuric acid and nitric acid, which enter the primary water washing kettle 2. The primary water washing kettle 2 can be introduced with circulating water through the coil 19 or steam through the outer half pipe to control the temperature between 46°C and 85°C to remove the acid in the material; S2. The primary washing tank 2 is metered to add 1 ton of dinitrate to 1 ton of water for primary washing of the material, at which time the portion of the wash water is the secondary wash wastewater; After washing in the primary washing kettle 2, the material overflows to the primary washing separation tank 4. When entering this step, steam can be introduced through the outer half pipe to control the temperature between 46°C and 85°C to prevent the material from crystallizing. The material is continuously stratified in the primary washing separation tank 4. After stratification, the upper aqueous phase is acidic wastewater, which flows into the wastewater neutralization kettle 6 by potential difference. 50% sodium hydroxide is quantitatively added to the wastewater neutralization kettle 6 at the same time until the amount of sodium hydroxide added makes the pH value of the neutralized wastewater between 6 and 12. The neutralized wastewater contains 6% sodium nitrate and about 2% sodium sulfate. Then it enters the washing brine tank 8 and is pumped out to the sulfide black production as bottom water; The lower organic phase in the primary water washing separation tank 4 is mainly composed of dinitrochlorobenzene and trace amounts of sulfuric acid and nitric acid. It enters the secondary water washing kettle 5 and is washed again after steam is introduced through the outer half pipe to control the temperature between 46°C and 85°C. At this time, this part of the washing water is alkaline washing wastewater, which is used to further remove the acid in the material; After that, the material of the secondary water washing kettle 5 overflows to the secondary water washing separation tank 7. The temperature is controlled between 46°C and 85°C by introducing steam through the outer half pipe. The material is continuously stratified in the secondary water washing separation tank 7. After stratification, the upper aqueous phase is acid-containing wastewater, which flows into the secondary water washing wastewater tank 9 by gravity and is pumped into the primary water washing kettle 2 for use as water for washing. The lower organic phase, whose main components are dinitrochlorobenzene and trace amounts of sulfuric acid and nitric acid, enters the soda ash dissolution kettle 12, where steam is introduced through the outer half pipe to control the temperature between 30°C and 60°C for further deacidification treatment to further remove the acid and water in the material and improve the purity of the product.

[0035] S3. The material in the soda ash dissolving kettle 12 is about 15% sodium carbonate solution. First, 99.5% solid powdered sodium carbonate is quantitatively added to the outlet of the soda ash dissolving kettle 12, and the pH is controlled at 7-11. At the same time, a certain amount of fresh water is pumped in and the stirring system is turned on. The solid sodium carbonate is dissolved at about 40°C and normal pressure. After the dissolution, the sodium carbonate solution is pumped into the alkali washing kettle 10 as alkali washing water, and the two soda ash dissolving kettles 12 are used alternately as storage tanks; S4. Soda ash dissolution kettle 12 is heated to dissolve by steam, and the temperature is controlled at 30 ℃ -60 ℃; S5. After the alkali washing water in the soda ash dissolving kettle 12 is pumped into the alkali washing kettle 10, the alkali washing is maintained under normal pressure stirring conditions, and the feed liquid overflows into the alkali washing separation tank 11 for automatic stratification. During the stratification process, steam is introduced through an external accompanying pipe to control the temperature to 46°C-85°C. After stratification, the upper aqueous phase is the alkali washing wastewater, which flows into the alkali washing wastewater tank 13 by gravity and is transported to the secondary water washing kettle 5 by a pump for water washing process; The lower organic phase is 95% of 2,4-dinitrochlorobenzene, and the remaining 5% is a mixture of 2,6-dinitrochlorobenzene, 3,5-dinitrochlorobenzene and a small amount of water, which flows into the dinitro transfer tank 14 by gravity. The dinitro transfer tank 14 is heated at 55°C-60°C by steam through the external coil 19, and is finally pumped into the dinitrochlorobenzene 95 finished product tank in the tank area or pumped into a crystallizer for crystallization and purification, completing separation and purification.

[0036] The above are only preferred embodiments of the present invention and are not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. A dinitrogen product water washing and alkali washing liquid separation equipment, characterized in that: The invention comprises a dinitrate nitrate oil separation tank (1), wherein the dinitrate nitrate oil separation tank (1) is connected to a primary water washing kettle (2) and a dinitrate waste acid tank (3) through pipelines, the primary water washing kettle (2) is connected to a primary water washing separation tank (4) through pipelines, the primary water washing separation tank (4) is connected to a secondary water washing kettle (5) and a wastewater neutralization kettle (6) through pipelines, the secondary water washing kettle (5) is connected to a secondary water washing separation tank (7) through pipelines, and the wastewater neutralization kettle (6) is connected to a washing brine through pipelines. The secondary water washing separation tank (7) is connected to the secondary water washing wastewater tank (9) and the alkali washing kettle (10) through pipelines, the alkali washing kettle (10) is connected to the alkali washing separation tank (11) through pipelines, the alkali washing separation tank (11) is connected to the alkali washing wastewater tank (13) and the dinitrate transfer tank (14) through pipelines, the secondary water washing wastewater tank (9) is connected to the primary water washing kettle (2) through pipelines, and the alkali washing wastewater tank (13) is connected to the secondary water washing kettle (5) through pipelines.

2. The dinitro product water washing and alkali washing liquid separation equipment according to claim 1 is characterized in that: The dinitrate nitrate oil separation tank (1) is used to receive the material after the dinitrate reaction is cooled, and the upper layer of the dinitrate nitrate oil separation tank (1) enters the primary water washing kettle (2), and the lower layer of the material enters the dinitrate waste acid tank (3); The water washing control temperature of the primary water washing kettle (2) is 55° C., and circulating cooling water (green line) is introduced through the coil (19) fixedly arranged inside the primary water washing kettle (2) - in from the upper left and out from the lower right, and low-pressure steam is introduced into the outer half pipe; The primary water washing separation tank (4) is used to receive the overflow of the primary water washing kettle (2), and the upper layer of wastewater in the primary water washing separation tank (4) flows by gravity to the wastewater neutralization kettle (6), and the lower layer flows into the secondary water washing kettle (5); Steam is introduced into the outer half of the secondary water washing kettle (5) to control the temperature at 55°C, so as to further remove the acid in the material; The secondary water washing separation tank (7) is used to receive the liquid material overflowing from the secondary water washing kettle (5) and to separate the liquid material into layers, with the upper layer of the liquid material entering the secondary water washing wastewater tank (9) and the liquid material entering the alkali washing kettle (10); The alkali washing kettle (10) is provided with steam through the outer half pipe to control the temperature, so as to further remove the acid and water in the material and improve the purity of the product; The alkali washing separation tank (11) is supplied with steam through the outer half pipe to control the temperature, and the upper layer flows by gravity to the alkali washing wastewater tank (13), and the lower layer flows by gravity into the dinitrate transfer tank (14); The water jacket in the alkali washing wastewater tank (13) is used for the water washing process of the secondary water washing kettle (5); The dinitrate transfer tank (14) is used to store the separated liquid.

3. The dinitro product water washing and alkali washing liquid separation equipment according to claim 2 is characterized in that: The material in the dinitrate waste acid tank (3) is used as a raw material for the mononitrate reaction; The wastewater neutralization kettle (6) is used to receive the upper layer liquid of the primary water washing separation tank (4) and quantitatively add 50% sodium hydroxide for neutralization; The washing brine tank (8) is used to receive the liquid material after neutralization in the wastewater neutralization kettle (6) and pump it to produce sulfide black as bottom water; The alkali washing kettle (10) is connected to a soda ash dissolving kettle (12) via a pipeline, and the soda ash dissolving kettle (12) is used to prepare alkali washing water for alkali washing of the alkali washing kettle (10); The material in the secondary washing wastewater tank (9) is pumped into the primary washing kettle (2) to be used as washing water.

4. The dinitro product water washing and alkali washing liquid separation equipment according to claim 3 is characterized in that: The dinitro transfer tank (14) is pumped into the dinitrochlorobenzene 95 finished product tank in the tank area or into a crystallizer for crystallization and purification.

5. The dinitro product water washing and alkali washing liquid separation equipment according to claim 1 is characterized in that: The dinitrate and nitrate oil separation tank (1) comprises a shell (15), a variable frequency air pump (16) and a water pump (17); two sets of sight glasses (18) are arranged on the surface of the shell (15); a coil (19) is arranged inside the shell (15); a promotion structure (20) is arranged inside the shell (15); an adjustment structure (21) is connected between the coil (19) and the shell (15); and an exhaust hole is arranged on the surface of the shell (15).

6. The dinitro product water washing and alkali washing liquid separation equipment according to claim 5, characterized in that: The promotion structure (20) comprises a rotating shaft (201) rotatably connected to the axis of the outer shell (15); a rotating member (202) is movably sleeved on the surface of the rotating shaft (201); a first sleeve (203) is connected through the surface of the outer shell (15); a movable tube (205) is movably connected inside the first sleeve (203); a main motor (204) is fixedly connected to the top of the rotating shaft (201) on the surface of the outer shell (15); a rotating ring (206) is rotatably connected to the surface of the rotating member (202); a connecting hole (207) is provided at the lower end of the rotating ring (206); the connecting hole (207) is connected to the movable tube (205) and the inside of the rotating member (202); a stirring plate (208) is fixedly connected to the surface of the rotating member (202); a one-way vent valve (209) is fixedly connected to the surface of the stirring plate (208); and a convex strip (210) is fixedly connected to the surface of the rotating shaft (201).

7. The dinitrogen product water washing and alkali washing liquid separation equipment according to claim 5, characterized in that: The regulating structure (21) comprises an annular tube (211) fixedly connected to both ends of the coil (19); a second sleeve (212) is fixedly connected to the surface of the annular tube (211); an inlet pipe (213) is movably sleeved on the inner side of the upper end of the second sleeve (212); a first plate (214) is fixedly connected to the surface of the second sleeve (212); a second plate (215) is fixedly connected to the surface of the inlet pipe (213); and a support spring (216) is connected between the second plate (215) and the first plate (214).

8. The dinitro product water washing and alkali washing liquid separation equipment according to claim 6 is characterized in that: The rotating shaft (201) and the housing (15) are rotatably connected via a bearing. The rotating shaft (201) and the convex strip (210) both penetrate the rotating member (202). The rotating member (202) slides along the length direction of the rotating shaft (201). The outer surface of the rotating shaft (201) is kept stable near the lower end by a bracket. The outer diameter of the movable tube (205) is equal to the inner diameter of the first sleeve (203). The movable tube (205) and the first sleeve (203) are slidably connected. The main motor (204) is a variable frequency motor. The output end of the variable frequency air pump (16) is connected to the top end of the No. 1 sleeve (203), and the rotating member (202) is driven to rotate together with the stirring plate (208) through the rotation of the rotating shaft (201). The stirring plate (208) is connected to the inside of the rotating member (202), and the air flow direction of the one-way ventilation valve (209) is from the inside of the stirring plate (208) to the outside of the one-way ventilation valve (209). The movable tube (205) and the rotating ring (206) are fixedly connected, and the rotating ring (206) and the rotating member (202) are rotatably connected.

9. The dinitro product water washing and alkali washing liquid separation equipment according to claim 7, characterized in that: The inlet pipe (213) is used to pass hot water. The surface of the annular pipe (211) corresponding to the lower end of the coil (19) is also connected with a group of pipes for connecting to a drainage pipe for drainage. The structure of the connection between the drainage pipe and the annular pipe (211) is the same as the structure of the connection between the inlet pipe (213) and the annular pipe (211). The upper and lower ends of the support spring (216) are fixedly connected to the second plate (215) and the first plate (214) respectively. The second sleeve (212) slides up and down along the inlet pipe (213), and the hot water impacts the conical plate (217) to achieve the downward movement of the annular pipe (211) together with the coil (19).

10. A process for treating a dinitrate product water washing and alkali washing liquid separation equipment, characterized in that: The treatment process includes the following steps: S1. After the dinitration reaction is completed and cooled, the material flows by gravity into the dinitrification oil separation tank (1) by utilizing the potential difference of the equipment, and is continuously layered under normal pressure. The acid phase in the lower layer is dinitrification waste acid, the main components of which are sulfuric acid and a small amount of nitric acid. The material flows by gravity into the dinitrification waste acid tank (3) by utilizing the potential difference of the equipment, and is used as the raw material for the mononitration reaction; The organic phase in the upper layer mainly contains dinitrochlorobenzene and a small amount of sulfuric acid and nitric acid, and enters the primary water washing kettle (2). The primary water washing kettle (2) can be introduced with circulating water through a coil or steam through an outer half pipe to control the temperature between 46°C and 85°C to remove the acid in the material. S2. Adding 1 ton of dinitrate to 1 ton of water in a ratio of 1 ton to the primary washing kettle (2) to wash the material, at which time the wash water is the secondary washing wastewater; After the primary water washing kettle (2) is washed, the material overflows to the primary water washing separation tank (4). When entering this step, steam can be introduced through the outer half pipe to control the temperature between 46°C and 85°C to prevent the material from crystallizing. The material is continuously stratified in the primary water washing separation tank (4). After stratification, the upper aqueous phase is acidic wastewater, which flows into the wastewater neutralization kettle (6) by gravity using the potential difference. 50% sodium hydroxide is quantitatively added to the wastewater neutralization kettle (6) at the same time until the amount of sodium hydroxide added makes the pH value of the neutralized wastewater between 6 and 12. The neutralized wastewater contains 6% sodium nitrate and about 2% sodium sulfate. It then enters the washing brine tank (8) and is pumped out to the sulfide black production as bottom water; The lower organic phase in the primary water washing separation tank (4) mainly contains dinitrochlorobenzene and trace amounts of sulfuric acid and nitric acid. It enters the secondary water washing kettle (5) and is subjected to water washing again after steam is introduced through the outer half pipe to control the temperature at 46°C-85°C. At this time, this part of the water washing water is alkaline washing wastewater, which is used to further remove the acid in the material. Afterwards, the material in the secondary water washing kettle (5) overflows into the secondary water washing separation tank (7) and the temperature is controlled between 46°C and 85°C by introducing steam through the outer half pipe. The material is continuously separated in the secondary water washing separation tank (7). After separation, the upper aqueous phase is acid-containing wastewater, which flows into the secondary water washing wastewater tank (9) by gravity and is then pumped into the primary water washing kettle (2) for use as washing water. The lower organic phase, which mainly contains dinitrochlorobenzene and trace amounts of sulfuric acid and nitric acid, enters the soda ash dissolution kettle (12), where steam is introduced through the outer half pipe to control the temperature between 30°C and 60°C for further deacidification to further remove the acid and water in the material and improve the purity of the product. S3. The material in the soda ash dissolving kettle (12) is a sodium carbonate solution of about 15%. First, 99.5% solid powdered sodium carbonate is quantitatively added to the outlet of the soda ash dissolving kettle (12) to control the pH value at 7-11. At the same time, a certain amount of fresh water is metered and pumped in and the stirring system is turned on. The solid sodium carbonate is dissolved at about 40° C. and normal pressure. After the dissolution is completed, the sodium carbonate solution is pumped into the alkali washing kettle (10) for use as alkali washing water. The two soda ash dissolving kettles (12) are used alternately as storage tanks. S4. Steam is introduced into the soda ash dissolution kettle (12) to heat and dissolve the soda ash, and the temperature is controlled at 30°C-60°C; S5. The alkali washing water in the soda ash dissolving kettle (12) is pumped into the alkali washing kettle (10), and then alkali washing is performed under normal pressure stirring conditions. The feed liquid overflows into the alkali washing separation tank (11) and is automatically stratified. During the stratification process, steam is introduced through an external accompanying pipe to control the temperature to be 46°C-85°C. After stratification, the upper aqueous phase is the alkali washing wastewater, which flows by gravity into the alkali washing wastewater tank (13) and is transported to the secondary water washing kettle (5) for water washing process by a pump; The lower organic phase is 95% of 2,4-dinitrochlorobenzene, and the remaining 5% is a mixture of 2,6-dinitrochlorobenzene, 3,5-dinitrochlorobenzene and a small amount of water, which flows into the dinitro transfer tank (14) by gravity. The dinitro transfer tank (14) is heated at 55°C-60°C by steam introduced through an external coil. Finally, it is pumped into the dinitrochlorobenzene 95 finished product tank in the tank area or pumped into a crystallizer for crystallization and purification, completing separation and purification.

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