A method for treating wastewater containing sodium 5-sulfonate of phthalic acid

Abstract

The present invention belongs to the technical field of chemical wastewater sewage treatment, and proposes a wastewater treatment method containing sodium 5-sulfonate of phthalic acid, including process steps: rectification dealcoholization process, extraction and stripping process, concentration and crystallization process, centrifugal dehydration process, primary refining process, primary filtering process, primary crystallization process, primary centrifugal process, secondary refining process, secondary filtering process, secondary crystallization process, secondary centrifugal process and crushing and drying process, the primary refining process and the secondary refining process are respectively refined by refining kettle to the solid components produced in the centrifugal dehydration process and the primary centrifugal process, and the refining kettle includes kettle body, wall sleeve, stirring device and activated carbon supply and recovery device, and the activated carbon supply and recovery device is used to provide activated carbon to the refining kettle and recover activated carbon from the refining kettle. The present invention is reasonably designed, reasonably designed, can effectively improve the recovery quality of SIPA and can realize flexible recovery of activated carbon, and is suitable for large-scale promotion.

Description

Technical Field

[0001] The invention belongs to the technical field of chemical wastewater and sewage treatment, and in particular relates to a method for treating wastewater containing sodium 5-sulfonate of phthalic acid. Background Art

[0002] Sodium 5-sulfophthalate (SIPM) uses isophthalic acid sulfonation, esterification, and salt-forming processes to produce three monomers. The measured isophthalic acid and fuming sulfuric acid are put into the sulfonation reactor, and the sulfonation reaction is carried out at a certain temperature. The qualified sulfonated material is moved to the esterification reactor, and an appropriate amount of methanol is added for esterification. Under the condition of ensuring the esterification rate, the esterified material is moved to the salt-forming reactor for salting. After the salt-forming material is filtered, it is refined and impurities are removed, the refined liquid is finely filtered, cooled and crystallized, and dehydrated to obtain wet-based SIPM, which is then dried to obtain a powdered finished product, which is weighed, packaged, and put into storage.

[0003] Sodium 5-sulfoisophthalic acid (SIPA) has two fewer methyl groups than sodium dimethyl ester 5-sulfoisophthalic acid (SIPM). The direct preparation method of sodium 5-sulfoisophthalic acid is, for example, a production process of sodium 5-sulfoisophthalic acid disclosed in patent CN202211637981.1, which mainly uses isophthalic acid as a raw material, and after sulfonation, it is directly obtained by neutralization and refining without the need for an esterification step. One of the indirect preparation methods of sodium 5-sulfoisophthalic acid is, for example, a method for extracting sodium 5-sulfoisophthalic acid from sodium 5-sulfoisophthalic acid wastewater disclosed in CN201510448496.3, which is a method for recovering sodium 5-sulfoisophthalic acid from wastewater of a direct preparation process. Another indirect preparation method of sodium 5-sulfoisophthalate is a method for comprehensive treatment of production wastewater of three monomers, such as the method disclosed in CN201110378414.4, which takes the production wastewater of three monomers as the treatment object, and undergoes a process of distillation dealcoholization process, extraction process, back extraction process, concentration and dehydration process, hot melt fine filtration process, dehydration and crystallization process, and crushing and drying process, in which an alcohol-acid mixed solvent is added in the extraction process; liquid alkali and pure water are added in the back extraction process; sulfuric acid, activated carbon and pure water are added in the hot melt fine filtration process; under the process conditions of temperature, moisture and time corresponding to the process, the finished product of sodium 5-sulfoisophthalate is finally prepared.

[0004] At present, for the indirect production process of SIPA, such as the method disclosed in CN201110378414.4 for comprehensive treatment of production wastewater using three monomers, there are still some problems in its actual production application. For example, firstly, the purity of SIPA after the filtrate is dehydrated and crystallized is insufficient, and if it is directly subjected to the drying process, it will also affect the factory quality of the finished product; secondly, in the hot melt fine filtration process (V), the activated carbon added to the hot melt kettle plays a decolorizing role, and it needs to be filtered out of the mother liquor / filtrate in the subsequent fine filtration and filtration steps. Since the activated carbon is recyclable, this process, like some other processes, is not conducive to the recovery of activated carbon. In many cases, it is transferred to the hazardous waste treatment center and treated as waste residue, resulting in a waste of resources. Summary of the invention

[0005] In view of the technical problems existing in the above-mentioned SIPA production process, the present invention proposes a method for treating wastewater containing sodium 5-sulfonate of phthalic acid, which has a reasonable design, can effectively improve the recovery quality of SIPA and can realize flexible recovery of activated carbon.

[0006] In order to achieve the above-mentioned purpose, the technical scheme adopted by the present invention is as follows: a method for treating wastewater containing sodium 5-sulfonate of phthalic acid provided by the present invention comprises process steps: a distillation dealcoholization process, an extraction and stripping process, a concentration and crystallization process, a centrifugal dehydration process, a primary refining process, a primary filtration process, a primary crystallization process and a pulverizing and drying process, wherein the primary crystallization process and the pulverizing and drying process further comprise a primary centrifugal process, a secondary refining process, a secondary filtration process, a secondary crystallization process and a secondary centrifugal process in sequence, the solid components produced in the centrifugal dehydration process, activated carbon and water are added to the primary refining process, the filtrate of the primary filtration process, the mother liquor of the primary centrifugal process and concentrated sulfuric acid are added to the primary crystallization process, and the secondary refining process comprises a primary centrifugal process, a secondary refining process, a secondary filtration process, a secondary crystallization process and a secondary centrifugal process in sequence. The solid components produced in the first centrifugal process, as well as activated carbon and water are added to the preparation process, the mother liquor components produced in the first centrifugal process are added to the extraction and back-extraction process, the mother liquor generated in the second centrifugal process is split and added to the first crystallization process and the second crystallization process, the solid components produced in the second centrifugal process are added to the crushing and drying process, and a refining kettle is used in the first refining process and the second refining process to purify the solid components produced in the centrifugal dehydration process and the first centrifugal process respectively, the refining kettle comprises a kettle body, a wall sleeve, a stirring device and an activated carbon supply and recovery device, the activated carbon supply and recovery device is used to provide activated carbon to the refining kettle and recover activated carbon from the refining kettle, and the activated carbon used in the refining kettle is a column block elastic structure.

[0007] Preferably, the activated carbon supply and recovery device includes a supply component and a recovery component, the supply component includes a supply pipe arranged on the kettle body and extending obliquely toward the inside of the kettle body, a supply core is arranged in the supply pipe, at least two trajectories are arranged on the supply core, the trajectories are used to install activated carbon bombs, and a loading cylinder for top-loading activated carbon bombs is arranged on the outside of the supply pipe.

[0008] Preferably, the stirring device includes a stirring motor, a stirring shaft and a stirring component, the stirring shaft is a hollow structure and a liftable core shaft is arranged inside, the stirring component includes a pipe sleeve that is transmission-connected to the core shaft, the pipe sleeve is provided with a plurality of stirring rods distributed in a circular array, the stirring rod includes a vertical section and an inclined section, the inclined section is provided with at least two clamping rods for connecting the trajectory, and a clamping opening is provided on the top of the clamping rod.

[0009] Preferably, the side of the core shaft is provided with radial shafts and transmission keys spaced apart in upper and lower directions, the stirring shaft is provided with a first key-shaped hole and a second key-shaped hole for lifting and lowering cooperation of the radial shaft and the transmission key, a balancing spring and a lifting plate are respectively provided above and below the radial shaft, and a lifting cylinder is provided at the driving end of the lifting plate.

[0010] Preferably, the stirring rod and the clamping rod are both hollow structures and are interconnected to form a pressure chamber. The head end of the pressure chamber is located at the top of the stirring rod and is provided with a piston assembly that cooperates with the stirring rod. A rotating joint is provided on the top of the piston assembly, and the top of the rotating joint is connected to the top center of the kettle body.

[0011] Preferably, a plug is provided at the end of the pressure chamber, and the plug is provided on the handlebar, with the end on the handlebar facing downward.

[0012] Preferably, a supply clamp is provided inside the supply tube at the top of the supply core, the supply clamp is a double-layer structure and is provided with a plurality of clamping openings for installing activated carbon bombs, a gear ring is sleeved on the supply clamp, a gear shaft meshing with the gear ring is provided on the transmission side of the gear ring, and a stepping motor is provided at the shaft end of the gear shaft.

[0013] Preferably, the activated carbon bomb includes a carbon block, an embedded tube is arranged in the center of the carbon block, end pieces are arranged at both ends of the embedded tube, the end pieces include a threaded tube spirally matched with the embedded tube, an end plate matched with the end of the carbon block is arranged at one end of the threaded tube, a protective sheet extending toward the side direction of the carbon block is arranged on the end plate, and a guide shell is arranged at the other end of the threaded tube, and the guide shell is a metal hemispherical shell.

[0014] Preferably, the recovery component includes a skirt plate arranged inside the kettle body, the plate edge of the skirt plate faces downward and is provided with a plurality of evenly distributed magnetic columns, the skirt plate and the top surface of the wall sleeve constitute a recovery groove with a trapezoidal cross-section, the recovery groove is provided with a fixed stop block and a booster block movable along the circumferential direction of the recovery groove, one end of the booster block is provided with a notch for cooperating with the activated carbon bomb, both ends of the booster block are provided with a driving rope, the power end of the driving rope is provided with a pulley mechanism, the pulley mechanism is arranged on the outside of the kettle body, the kettle body is provided with a recovery pipe at a position corresponding to the fixed stop block, and the side of the recovery pipe is provided with a guide hole for movable sealing cooperation with the driving rope.

[0015] Preferably, the protective sheet is made of metal and has a V-shaped cross section.

[0016] Compared with the prior art, the advantages and positive effects of the present invention are:

[0017] 1. The present invention provides a method for treating wastewater containing sodium 5-sulfophthalate, which uses a primary centrifugation process, a secondary refining process, a secondary filtration process, a secondary crystallization process and a secondary centrifugation process to further treat the solid component, and distinguishes the timing of adding concentrated sulfuric acid from that of adding activated carbon and water, and adds concentrated sulfuric acid in the primary crystallization process, which is beneficial to improving the purity of the final separated product, thereby achieving the treatment of SIPM process wastewater and effectively recovering high-quality SIPA.

[0018] 2. The present invention provides a method for treating wastewater containing sodium 5-sulfonate of phthalic acid. On the basis of using activated carbon to achieve decolorization in the refining kettle in the primary refining process and the secondary refining process, a fixed shape is adopted as the basic shape, and an activated carbon supply and recovery device is provided. With the cooperation of a stirring device, the activated carbon can be recovered in situ, which reduces the amount of activated carbon added in the subsequent filtration step and improves the filtration efficiency. On the other hand, it is also convenient for the reuse of the activated carbon.

[0019] 3. The present invention has a reasonable design, can effectively improve the recovery quality of SIPA and can realize flexible recovery of activated carbon, and is suitable for large-scale promotion. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the following briefly introduces the drawings required for use in the description of the embodiments. Obviously, the drawings described below are some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without creative work.

[0021] Figure 1 A process diagram of a method for treating wastewater containing sodium 5-sulfonate of phthalic acid provided in an embodiment;

[0022] Figure 2 It is the front view of the refining kettle;

[0023] Figure 3 It is the axonometric diagram of the refining kettle in the primary refining process and the secondary refining process;

[0024] Figure 4 for Figure 2 The cross-sectional view of the middle refining kettle in the GG direction;

[0025] Figure 5 It is an axonometric view of the stirring device;

[0026] Figure 6 This is a partial exploded view of the recovered parts;

[0027] Figure 7 This is the front view of the activated carbon bomb;

[0028] Figure 8 It is the cross-sectional view of the activated carbon bomb in the EE direction;

[0029] Fig. 9 It is the cross-sectional view of the activated carbon bomb in the FF direction;

[0030] Fig.10 for Figure 4 A magnified schematic diagram of the structure in the middle;

[0031] In the above figures, 1, kettle body; 2, wall sleeve; 3, stirring device; 31, stirring motor; 32, stirring shaft; 33, stirring component; 331, pipe sleeve; 332, stirring rod; 333, clamping rod; 334, clamping mouth; 34, mandrel; 35, radial shaft; 36, transmission key; 37, balance spring; 38, lifting plate; 39, lifting cylinder; 310, pressure chamber; 311, piston assembly; 312, rotary joint; 313, plug; 314, elbow; 4, activated carbon supply and recovery device; 41, supply component; 411, supply pipe; 412, supply core; 4 13. trajectory; 414. supply clamp; 415. clamping port; 416. gear ring; 417. gear shaft; 418. stepper motor; 42. recovery component; 421. skirt; 422. magnetic column; 423. recovery groove; 424. fixed stopper; 425. booster block; 426. notch; 427. drive rope; 428. pulley mechanism; 429. recovery tube; 4210. guide hole; 43. activated carbon bomb; 431. carbon block; 432. embedded tube; 433. end piece; 4331. threaded tube; 4332. end plate; 4333. protective sheet; 4334. guide shell. DETAILED DESCRIPTION

[0032] In order to more clearly understand the above-mentioned objects, features and advantages of the present invention, the present invention is further described below in conjunction with the accompanying drawings and embodiments. It should be noted that the embodiments of the present application and the features in the embodiments can be combined with each other without conflict. For the convenience of description, if the words "upper", "lower", "left" and "right" appear below, they only indicate that the upper, lower, left and right directions are consistent with the accompanying drawings themselves, and do not limit the structure.

[0033] In the following description, many specific details are set forth to facilitate a full understanding of the present invention. However, the present invention may also be implemented in other ways than those described herein. Therefore, the present invention is not limited to the specific embodiments of the following disclosure.

[0034] Examples, such as Figure 1-Figure 10 As shown, the present invention provides a method for treating wastewater containing sodium 5-sulfophthalate, comprising process steps: a rectification and dealcoholization process, an extraction and stripping process, a concentration and crystallization process, a centrifugal dehydration process, a primary refining process, a primary filtration process, a primary crystallization process, a primary centrifugation process, a secondary refining process, a secondary filtration process, a secondary crystallization process, a secondary centrifugation process and a crushing and drying process. In the primary refining process, solid components, activated carbon and water produced in the centrifugal dehydration process are added, the filtrate of the primary filtration process, the mother liquor of the primary centrifugation process and concentrated sulfuric acid are added to the primary crystallization process, the solid components, activated carbon and water produced in the primary centrifugation process are added to the secondary refining process, the mother liquor components produced in the primary centrifugation process are added to the extraction and stripping process, the mother liquor produced in the secondary centrifugation process is split and added to the primary crystallization process and the secondary crystallization process, and the solid components produced in the secondary centrifugation process are added to the crushing and drying process.

[0035] More specifically, in the distillation dealcoholization process, SIPM process wastewater is stored in a wastewater storage tank, 5% methanol wastewater is pumped into the preheater, and after being preheated by the tower bottom residual liquid and steam condensate, it enters the distillation tower from the middle of the tower, and after being heated by the reboiler, the methanol vapor enters the condenser from the top of the tower, and is cooled by circulating water to become methanol liquid, and enters the receiving tank, part of which is returned to the distillation tower as reflux liquid, and part of which is extracted and enters the methanol storage tank. The tower bottom residual liquid becomes dealcoholization wastewater with an alcohol content of less than 0.1%. After the raw material is cooled, it is pumped to the residual liquid storage tank, and finally pumped into the wastewater treatment workshop for recovery of sodium 5-sulfonate of isophthalic acid. The wastewater components after methanol distillation are sodium sulfate, water, sodium 5-sulfonate of dimethyl isophthalate, sodium 5-sulfonate of isophthalic acid, and isophthalic acid.

[0036] Furthermore, in the recovery process of sodium 5-sulfonate of phthalic acid, the dealcoholization wastewater of the distillation dealcoholization process enters the dealcoholization wastewater storage tank; it is pumped to the extraction and stripping process, and enters the extraction kettle after metering, and the metered extractant is added for extraction. The raffinate is the water phase, which enters the raffinate tank, is pumped for treatment, and is discharged after meeting the standards; the metered liquid alkali is added to the extraction kettle for stripping, and after the stripping is completed, the material enters the stripping liquid storage tank; the material in the stripping liquid storage tank is pumped into the concentration and crystallization kettle supporting the concentration and crystallization process, the liquid alkali is added, steam is heated, the vacuum is turned on, the removed water enters the receiving tank in the process, and finally enters the process water tank for circulation. After dehydration, turn off the steam, pass circulating water to cool down, and the crude product crystallizes out; unload the crystal liquid into the centrifuge supporting the centrifugal dehydration process for centrifugation, and the centrifuged mother liquor enters the sodium salt mother liquor tank for recycling; the centrifuged crude product is sent to the primary refining process, and activated carbon and process water are added to the refining kettle in the primary refining process for mixed decolorization; the solid hot solution after the primary refining is pumped to the primary filtration process, and the primary filtration process is equipped with a filter, and the filtered solid waste residue is sent to the hazardous waste treatment center; the filtrate enters the primary crystallization process, and the primary crystallization process is equipped with a concentrated crystallization kettle, and the measured sulfuric acid and secondary mother liquor are added. After mixing, steam is passed to heat Heat, open the vacuum, the removed water enters the receiving tank in this process, and finally enters the process water tank for recycling. After the dehydration is completed, the steam is turned off, the circulating water is passed for cooling, and the crude product is crystallized and precipitated; the primary crystal liquid is sent to the primary centrifugation process, the primary centrifugation process is equipped with a centrifuge for centrifugal operation, the centrifuged mother liquor enters the primary mother liquor pool, and is pumped into the extraction kettle for recycling; the crude product after centrifugation is sent to the secondary refining process, the secondary refining process is equipped with a refining kettle, and activated carbon and process water are added for mixed decolorization; the hot solution / solid component after decolorization is sent to the secondary filtration process, the secondary filtration process is equipped with a filter for filtration operation; the filtrate of the secondary filtration process is added Enter the secondary crystallization process, the secondary crystallization process is equipped with a secondary concentration crystallization kettle, steam heating, open the vacuum, the removed water enters the receiving tank equipped with this process, and finally enters the process water tank for recycling. After dehydration, turn off the steam, pass circulating water for cooling, and the crude product crystallizes out; the secondary crystallization liquid is unloaded into the secondary centrifugation process, the centrifuge in the secondary centrifugation process performs centrifugal operation, part of the centrifuged mother liquor enters the secondary mother liquor pool, and another part is pumped into the primary concentration crystallization kettle for recycling; the products produced in the secondary centrifugation process are sent to the crushing and drying process, the crushing and drying process is equipped with a crusher for crushing operation, and then sent to the vacuum dryer for drying and packaging and storage.

[0037] In the process steps provided by the present invention, a primary centrifugation process, a secondary refining process, a secondary filtration process, a secondary crystallization process and a secondary centrifugation process are used to further process the hot solution / solid components, which increases the number of refining, crystallization and filtration times, increases the extraction steps of SIPA, and is beneficial to improving the purity of the final separated product. Furthermore, the timing of adding concentrated sulfuric acid is different from that of adding activated carbon and water. Activated carbon and water are added to the refining kettle in the refining step, while concentrated sulfuric acid is added to the primary crystallization process, which can effectively ensure the decolorization quality of the activated carbon for the material and is beneficial to improving the saturated crystallinity of SIPA. In this way, the wastewater treatment process provided by the present invention not only realizes the treatment of SIPM process wastewater, but also effectively recovers high-quality SIPA.

[0038] In the present invention, the amount of activated carbon put into the primary refining process and the secondary refining process is 2% to 5% of the dehydrated material. In order to improve the recovery rate of activated carbon in the present method, the present invention adopts a refining kettle in the primary refining process and the secondary refining process to purify the solid components produced in the centrifugal dehydration process and the primary centrifugal process respectively. The refining kettle includes a kettle body 1, a wall sleeve 2, a stirring device 3 and an activated carbon supply and recovery device 4. The activated carbon supply and recovery device 4 is used to provide activated carbon to the refining kettle and recover activated carbon from the refining kettle. The activated carbon used in the refining kettle is a column block elastic structure. The basic shape of the activated carbon put into the refining kettle adopts a fixed shape, and the input and recovery are completed by the matching activated carbon supply and recovery device 4, and the full contact with the material in the refining kettle is completed with the cooperation of the stirring device 3. On the basis of achieving decolorization of the activated carbon, on the one hand, the amount of activated carbon in the subsequent filtration step is reduced, the filtration load is reduced, and the filtration efficiency is improved. On the other hand, it is also convenient to reuse the activated carbon. Regarding the methods of reusing activated carbon, high-temperature steam method, exposure method, electric heating regeneration method and chemical oxidation regeneration method can be used.

[0039] like Figure 2 , Figure 3 , Figure 4 and Figure 6 As shown, the activated carbon supply and recovery device 4 provided by the present invention includes a supply component 41 and a recovery component 42. The supply component 41 includes a supply pipe 411 arranged on the kettle body 1 and extending obliquely toward the inside of the kettle body 1. A supply core 412 is arranged in the supply pipe 411. At least two ballistics 413 are arranged on the supply core 412. The ballistics 413 are used to install activated carbon bombs 43. The outside of the supply pipe 411 is provided with a loading cylinder for loading the activated carbon bombs 43. The loading cylinders are installed in pairs on the frame system of the workshop, with their telescopic ends facing the supply component 41. The supply component 41 provides a plurality of activated carbon bombs 43. The loading cylinder pushes the activated carbon bombs 43 into the kettle body 1 along the ballistics 413 through the telescopic action.

[0040] like Figure 4 and Figure 5 As shown, in cooperation with the supply component 41, the stirring device 3 provided by the present invention includes a stirring motor 31, a stirring shaft 32 and a stirring component 33. The stirring shaft 32 is a hollow structure and a liftable core shaft 34 is arranged inside. The stirring component 33 includes a pipe sleeve 331 which is transmission-connected to the core shaft 34. The pipe sleeve 331 is provided with a plurality of stirring rods 332 distributed in a circular array. The stirring rod 332 includes a vertical section and an inclined section. The inclined section is provided with at least two clamping rods 333 for connecting with the trajectory 413. The top of the clamping rod 333 is provided with a clamping opening 334. Among them, the core shaft 34 can make the stirring rod 332 rise and fall by lifting and lowering, and the rising action of the stirring rod 332 can be connected to the loading action of the loading cylinder. After the clamping port 334 is aligned with the trajectory 413, the loading cylinder pushes the activated carbon bomb 43 into the clamping port 334, and the two trajectories 413 simultaneously load the activated carbon bomb 43 into the ends of the two clamping rods 333; further, the stirring motor 31 rotates in a stepping mode, and each clamping rod 333 is connected to the supply component 41 in an orderly manner through step adjustment, so that all clamping rods 333 are equipped with activated carbon bombs 43. Regarding the stirring device 3, the activated carbon bomb 43 has a certain axial length, which can form a stirring arm of a certain length with the clamping rod 333, which not only extends the actual stirring range of the stirring device 3, but also can complete contact with the material during the continuous stirring process, thereby achieving the purpose of decolorization.

[0041] like Figure 5 and Fig.10 As shown, in order to improve the automation of the activated carbon supply in the refining kettle, the side of the core shaft 34 provided by the present invention is provided with radial shafts 35 and transmission keys 36 spaced apart from each other, and the stirring shaft 32 is provided with a first key-shaped hole and a second key-shaped hole for lifting and lowering cooperation of the radial shaft 35 and the transmission key 36. The transmission key 36 connects the core shaft 34 and the sleeve 331, and a fixing screw can be installed on the side of the sleeve 331 to make the core shaft 34 and the sleeve 331 have synchronous action, and a balance spring 37 and a lifting plate 38 are respectively provided above and below the radial shaft 35, and a lifting cylinder 39 is provided at the driving end of the lifting plate 38. In this way, the lifting cylinder 39 can drive the lifting plate 38 to move up and down through the telescopic action. If the lifting plate 38 moves up, the radial shaft 35, the core shaft 34 and the sleeve 331 can also move up. The radial shaft 35 moves up along the first key-shaped hole, and the core shaft 34 and the sleeve 331 move up along the direction of the transmission key 36 and the second key-shaped hole. When the lifting plate 38 is passively lowered, the core shaft 34 moves down under the pressure of gravity and the balance spring 37 on the radial shaft 35, so that the stirring rod 332 and the clamping rod 333 are reset, thereby realizing the automatic lifting and lowering of the clamping rod 333, and then realizing the automatic loading action of the activated carbon bomb 43.

[0042] like Figure 4 , Figure 5 and Fig.10 As shown, in order to improve the stability of the activated carbon bomb 43 on the clamping rod 333, the stirring rod 332 and the clamping rod 333 provided by the present invention are both hollow structures and are interconnected to form a pressure chamber 310. The head end of the pressure chamber 310 is located at the top of the stirring rod 332 and is provided with a piston assembly 311 that cooperates with the stirring rod 332 for insertion and extraction. The piston assembly 311 includes a piston and a piston rod. A rotary joint 312 is provided on the top of the piston rod. The top of the rotary joint 312 is connected to the top center of the kettle body 1. The activated carbon bomb 43 is loaded to the clamping port 334 through the top of the loading cylinder. The clamping port 334 is in the ascending position. The actual working length of the pressure chamber 310 is small, and the pressure of the pressure chamber 310 is basically the same as the pressure in the kettle body 1. During the resetting process of the stirring component 33, the vertical distance of the piston in the pressure chamber 310 is pulled apart, the actual working length of the pressure chamber 310 is lengthened, and negative pressure is formed in the pressure chamber 310, thereby sucking the activated carbon bomb 43 into the clamping port 334, ensuring the stability of the activated carbon bomb 43 in synchronous rotation with the stirring rod 332 and the clamping rod 333. During the continuous stirring process of the pipe sleeve 331 of the stirring device 3 driven by the stirring motor 31, the stirring shaft 32 and the core shaft 34, the piston assembly 311 always maintains a corresponding high horizontal position through the rotary joint 312, thereby ensuring the stability of the synchronous movement of the activated carbon bomb 43 and the clamping rod 333.

[0043] Furthermore, the present invention provides a plug 313 at the end of the pressure chamber 310. The plug 313 can be connected to the end of the stirring rod 332 by a threaded connection and serves as the blocking end of the pressure chamber 310. The plug 313 is arranged on a curved handle 314, and the end of the curved handle 314 faces downward. The curved handle 314 can serve as a lever structure for installing the plug 313, and can also serve as a part of the stirring arm of the stirring device 3, thereby improving the refining effect of the material in the refining kettle.

[0044] like Figure 4 and Figure 6As shown, considering that the number of clamping rods 333 designed for the stirring device 3 is relatively large, generally 6 stirring rods 332 and at least 12 clamping rods 333 are set. Based on the 12 clamping rods 333, in addition to the activated carbon bombs 43 originally assembled on the clamping rods 333, the number of activated carbon bombs 43 in the trajectory 413 is at most 4 to 8. Therefore, in order to fully supply the activated carbon bombs 43 corresponding to each clamping rod 333 during the replacement cycle, the present invention is provided with a supply clamp 414 at the top of the supply core 412 inside the supply pipe 411, and a sufficient number of activated carbon bombs 43 are pre-loaded through the supply clamp 414. Specifically, the supply clamp 414 provided by the present invention is a double-layer structure and a plurality of clamping ports 415 for installing the activated carbon bombs 43 are provided on the supply clamp 414. There are at least 6 activated carbon bombs 43 in a single layer and at least 12 in two layers. In addition to the preset spatial position in the trajectory 413, the supply quantity of the supply component 41 is sufficient. In order to load the activated carbon bomb 43 of the clamping port 415 into the trajectory 413, the present invention is provided with a ring gear 416 on the supply clamp 414, and the transmission side of the ring gear 416 is provided with a gear shaft 417 meshing with it, and the shaft end of the gear shaft 417 is provided with a stepping motor 418. The stepping motor 418 drives the gear shaft 417 and the ring gear 416 to generate stepping rotation through stepping action, so that the clamping port 415 is aligned with the corresponding empty trajectory 413. Under the action of the loading cylinder, the activated carbon bombs 43 can be put into place one after another, and then the action of successively equipping the stirring device 3 with the activated carbon bombs 43 can be completed. In order to ensure the controllability of the pressure inside the kettle body 1, the refining pressure is generally around 0.3 MPa. The present invention provides a sealing end cover at the end of the supply pipe 411, and a through hole that can cooperate with the telescopic rod of the cylinder is opened on the sealing end cover. During the time period when the activated carbon bomb 43 is not replenished, the sealing end cover and the telescopic rod maintain a movable seal, thereby ensuring that the pressure inside the kettle body 1 meets the pressure conditions of the refining process.

[0045] like Figure 4 , Figure 7-Figure 9As shown, in order to improve the matching performance between the activated carbon bomb 43 and the supply component 41 and the recovery component 42, the activated carbon bomb 43 provided by the present invention includes a carbon block 431, an embedded tube 432 is arranged at the center of the carbon block 431, and end pieces 433 are arranged at both ends of the activated carbon bomb 43, and the end pieces 433 include a threaded tube 4331 spirally matched with the embedded tube 432, an end plate 4332 matched with the end of the carbon block 431 is arranged at one end of the threaded tube 4331, a protective sheet 4333 extending toward the side direction of the carbon block 431 is arranged on the end plate 4332, and a guide shell 4334 is arranged at the other end of the threaded tube 4331, and the guide shell 4334 is a metal hemispherical shell. Among them, the carbon block 431 is the main decolorizing material, the embedded tube 432 can serve as the internal support of the activated carbon bomb 43 to improve the structural strength of the activated carbon bomb 43, and the end piece 433 can form a clamping relationship with the carbon block 431, so that the activated carbon bomb 43 remains a relatively independent component with a certain degree of anti-collision. The guide shell 4334 can form a relatively sealed assembly relationship with the clamping port 334, which is convenient for the piston assembly 311 and the pressure chamber 310 to cooperate with each other to complete the suction and ejection action of the activated carbon bomb 43.

[0046] Regarding the recycling component 42, Figure 2-4 As shown, the recovery component 42 provided by the present invention includes a skirt plate 421 arranged inside the kettle body 1, the plate edge of the skirt plate 421 faces downward and is provided with a plurality of evenly distributed magnetic columns 422, the skirt plate 421 and the top surface of the wall sleeve 2 form a recovery groove 423 with a trapezoidal cross section, the recovery groove 423 is provided with a fixed stopper 424 and a booster block 425 movable along the circumferential direction of the recovery groove 423, one end of the booster block 425 is provided with a notch 426 for cooperating with the activated carbon bomb 43, and both ends of the booster block 425 are provided with a driving Rope 427, the driving rope 427 is arranged near the inner top edge of the recovery groove 423 to avoid the pushed path of the activated carbon bomb 43 in the recovery groove 423 as much as possible; further, the power end of the driving rope 427 is provided with a pulley mechanism 4228, the pulley mechanism 428 includes a pulley and a driving motor, the pulley mechanism is arranged on the outside of the kettle body 1, and the kettle body 1 is provided with a recovery pipe 429 at a position corresponding to the fixed stopper 424, and the side of the recovery pipe 429 is provided with a guide hole 4210 for movable sealing cooperation with the driving rope 427.

[0047] The working principle of the recovery component 42 is that before and after the rising action of the stirring component 33 is completely completed, the activated carbon bomb 43 is pushed out of the clamping port 334 by the pressure in the pressure chamber 310, and the material in the kettle body 1 acts as a buffer. The activated carbon bomb 43 rises to the vicinity of the skirt plate 421 under the action of buoyancy, and the magnetic column 422 attracts the activated carbon bomb 43 through attraction. The cylindrical surface of the magnetic column 422 contacts the shell edge of the guide shell 4334 in a point-line manner. Under the action of magnetic attraction, gravity and buoyancy, the activated carbon bomb 43 enters The recovery groove 423 is located in the moving direction of the booster block 425; the driving rope 427 can be driven to move by starting the pulley mechanism, and the booster block 425 can squeeze the activated carbon bomb 43 into its slot 426, and continuously push other activated carbon bombs 43 to move toward the fixed block 424, until the activated carbon bomb 43 is guided to the recovery pipe by the fixed block 424, and the recovery pipe can be connected to the recovery manipulator or recovery bin of the workshop to recover the extruded activated carbon bomb 43, thereby realizing the automatic recovery of the activated carbon bomb 43. In the recovery process, the activated carbon bomb 43 can be directly processed together with the end piece 433, or the end piece 433 can be removed and all carbon blocks 431 can be regenerated by high-temperature steam method / electric heating regeneration method and other regeneration processing operations.

[0048] like Fig. 9 As shown, in order to improve the recovery efficiency of the activated carbon bomb 43, the protective sheet 4333 provided by the present invention is made of metal and has a V-shaped cross-section. In this way, when the activated carbon bomb 43 is ejected to the surface of the material, the magnetic column 422 and the protective sheet 4333 of the activated carbon bomb 43 can be magnetically attracted, and the magnetic attraction node is a line contact pair. Under the influence of gravity and magnetic attraction, the activated carbon bomb 43 can move along the V-shaped surface and deviate to the inner side of the recovery groove 423. In this way, the coordination effect of the booster block 425 and the activated carbon bomb 43 on the recovery path can be improved, thereby improving the recovery efficiency of the refining kettle for activated carbon.

[0049] The above description is only a preferred embodiment of the present invention and does not limit the present invention in other forms. Any technician familiar with the profession may use the technical content disclosed above to change or modify it into an equivalent embodiment with equivalent changes and apply it to other fields. However, any simple modification, equivalent change and modification made to the above embodiment based on the technical essence of the present invention without departing from the content of the technical solution of the present invention still falls within the protection scope of the technical solution of the present invention.

Claims

1. A method for treating wastewater containing sodium 5-sulfophthalate, comprising the steps of: a rectification and dealcoholization process, an extraction and stripping process, a concentration and crystallization process, a centrifugal dehydration process, a primary refining process, a primary filtration process, a primary crystallization process and a pulverization and drying process, characterized in that: The process between the primary crystallization process and the pulverizing and drying process also includes a primary centrifugation process, a secondary refining process, a secondary filtration process, a secondary crystallization process and a secondary centrifugation process in sequence. The solid components generated in the centrifugal dehydration process, activated carbon and water are added to the primary refining process. The filtrate of the primary filtration process, the mother liquor of the primary centrifugation process and concentrated sulfuric acid are added to the primary crystallization process. The solid components generated in the primary centrifugation process, activated carbon and water are added to the secondary refining process. The mother liquor components generated in the primary centrifugation process are added to the extraction and back-extraction process. The mother liquor generated in the secondary centrifugation process is divided and added to the primary crystallization process and the secondary crystallization process. The solid components generated in the secondary centrifugation process are added to the pulverizing and drying process. In the primary refining process and the secondary refining process, a refining kettle is used to purify the solid components generated in the centrifugal dehydration process and the primary centrifugation process respectively. The refining kettle includes a kettle body, a wall sleeve, a stirring device and an activated carbon supply and recovery device. The activated carbon supply and recovery device is used to provide activated carbon to the refining kettle and recover activated carbon from the refining kettle. The activated carbon used in the refining kettle is a column block elastic structure.

2. The method for treating wastewater containing sodium 5-sulfophthalate according to claim 1, characterized in that: The activated carbon supply and recovery device includes a supply component and a recovery component. The supply component includes a supply pipe arranged on the kettle body and extending obliquely toward the inside of the kettle body. A supply core is arranged in the supply pipe. At least two ballistics are arranged on the supply core. The ballistics are used to install activated carbon bombs. A loading cylinder for top loading activated carbon bombs is arranged on the outside of the supply pipe.

3. A method for treating wastewater containing sodium 5-sulfophthalate according to claim 2, characterized in that: The stirring device includes a stirring motor, a stirring shaft and a stirring component. The stirring shaft is a hollow structure and a liftable core shaft is arranged inside. The stirring component includes a pipe sleeve that is transmission-connected to the core shaft. The pipe sleeve is provided with a plurality of stirring rods distributed in a circular array. The stirring rod includes a vertical section and an inclined section. The inclined section is provided with at least two clamping rods for connecting the trajectory, and a clamping opening is provided on the top of the clamping rod.

4. The method for treating wastewater containing sodium 5-sulfophthalate according to claim 3, characterized in that: The side of the core shaft is provided with radial shafts and transmission keys spaced apart in upper and lower directions, the stirring shaft is provided with a first key-shaped hole and a second key-shaped hole for lifting and lowering cooperation between the radial shaft and the transmission key, a balancing spring and a lifting plate are respectively provided above and below the radial shaft, and a lifting cylinder is provided at the driving end of the lifting plate.

5. The method for treating wastewater containing sodium 5-sulfonate of phthalic acid according to claim 4, characterized in that: The stirring rod and the clamping rod are both hollow structures and are interconnected to form a pressure chamber. The head end of the pressure chamber is located at the top of the stirring rod and is provided with a piston assembly that cooperates with the stirring rod. A rotating joint is provided on the top of the piston assembly, and the top of the rotating joint is connected to the top center of the kettle body.

6. The method for treating wastewater containing sodium 5-sulfonate of phthalic acid according to claim 5, characterized in that: A plug is arranged at the end of the pressure chamber, and the plug is arranged on a curved handle, with the end on the curved handle facing downward.

7. A method for treating wastewater containing sodium 5-sulfophthalate according to any one of claims 2 to 6, characterized in that: A supply clamp at the top of the supply core is arranged inside the supply tube, the supply clamp is a double-layer structure and is provided with a plurality of clamping openings for installing activated carbon bombs, a gear ring is sleeved on the supply clamp, a gear shaft meshing with the gear ring is arranged on the transmission side of the gear ring, and a stepping motor is arranged at the shaft end of the gear shaft.

8. The method for treating wastewater containing sodium 5-sulfophthalate according to claim 2, characterized in that: The activated carbon bomb includes a carbon block, an embedded tube is arranged at the center of the carbon block, and end pieces are arranged at both ends of the embedded tube. The end pieces include a threaded tube that is spirally matched with the embedded tube, an end plate that is matched with the end of the carbon block is arranged at one end of the threaded tube, and a protective sheet extending toward the side direction of the carbon block is arranged on the end plate. A guide shell is arranged at the other end of the threaded tube, and the guide shell is a metal hemispherical shell.

9. The method for treating wastewater containing sodium 5-sulfophthalate according to claim 8, characterized in that: The recovery component includes a skirt plate arranged inside the kettle body, the plate edge of the skirt plate faces downward and is provided with a plurality of evenly distributed magnetic columns, the skirt plate and the top surface of the wall sleeve form a recovery groove with a trapezoidal cross-section, a fixed stopper and a booster block movable along the circumferential direction of the recovery groove are arranged in the recovery groove, one end of the booster block is provided with a notch for cooperating with the activated carbon bomb, both ends of the booster block are provided with a driving rope, the power end of the driving rope is provided with a pulley mechanism, and the pulley mechanism is arranged on the outside of the kettle body, the kettle body is provided with a recovery pipe at a position corresponding to the fixed stopper, and the side of the recovery pipe is provided with a guide hole for movable sealing cooperation with the driving rope.

10. The method for treating wastewater containing sodium 5-sulfophthalate according to claim 9, characterized in that: The protective sheet is made of metal and has a V-shaped cross section.

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