An industrial impurity removal system and method for the waste liquid of galaxol chlorobenzene rear stage
By designing an industrial impurity removal system that includes stirring, brushing and anti-spinning mechanisms, the problems of chloropropanol entrainment and impurities accumulation in the waste liquid in the back section of Galle Musk chlorobenzene were solved, and efficient chlorobenzene recycling and layered laying were achieved.
Patent Information
- Application Number
- CN202211197549.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2022-09-29
- Publication Date
- 2025-04-01
- Estimated Expiration
- 2042-09-29
AI Technical Summary
The waste liquid of Jiale Musk chlorobenzene is entrained with more chloropropanol, which makes it difficult to recover chlorobenzene, the recovery rate of pure products is low, and the impurities in the reaction kettle are difficult to clean, which affects the efficiency of layered cutting.
An industrial impurity removal system including the main body of the kettle body, the top disk assembly, the chassis and the anti-rotating and anti-rotating mechanism is designed. Through the combination of the stirring mechanism, the brush cleaning mechanism and the scraping mechanism, the up and down stirring of the liquid in the kettle and the inner wall cleaning are achieved. The anti-rotating and anti-rotating mechanism reduces vortex and improves the layered cutting efficiency.
Effectively remove impurities in the kettle, improve the recovery rate of pure chlorobenzene products, improve the efficiency of layering and cutting, ensure that the chlorobenzene content is ≥90%, and the chloropropanol impurity peak is ≤1%.
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Figure CN115626726B_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of impurity removal of galaxol chlorobenzene waste liquid, and in particular to an industrial impurity removal system and method for galaxol chlorobenzene rear-stage waste liquid. Background Art
[0002] Galaxan is a synthetic musk with a molecular weight of 258.4 and a boiling point of 129°C (107Pa). Its chemical name is 1,3,4,6,7,8-hexahydro-4,6,6,7,8,8-hexamethylcyclopenta-γ-2-benzopyran. It can emit a strong and lasting musk aroma, accompanied by a woody aroma during the volatilization process. It is widely used as an auxiliary fragrance in cosmetics, soap flavors and other industries.
[0003] At the back end of the production of galaxol, a certain amount of waste liquid from the bottom of the chlorobenzene tower will be generated. The waste liquid from the bottom of the chlorobenzene tower contains a lot of chloropropanol, which makes it difficult to recover chlorobenzene, the recovery rate of pure chlorobenzene is low, a large amount of impurities overlap with chlorobenzene, and the purity of chlorobenzene after recovery is low. In addition, during the process of recycling chlorobenzene in the reactor, the impurities inside the reactor will remain inside the reactor, and when performing the stratified operation, it is easy for stratified material to be discharged, resulting in excessive vortexes, which directly affects the stratified material discharge. For this reason, we proposed the operation mode of water washing and alkali washing, and optimized the impurity removal system for the situation where the stratification of material discharge is easily affected by vortices.
[0004] Therefore, in view of this, the inventor, with many years of rich experience in design, development and actual production in the relevant industry, has studied and improved the existing structure and deficiencies, and provided an industrial impurity removal system and method for the waste liquid of the latter stage of galaxol chlorobenzene, in order to achieve a more practical purpose. Summary of the invention
[0005] In order to solve the problems mentioned in the above background technology, the present invention provides an industrial impurity removal system and method for the waste liquid of the latter stage of galaxol chlorobenzene.
[0006] In order to achieve the above object, the present invention adopts the following technical solutions:
[0007] An industrial impurity removal system and method for galaxol chlorobenzene rear-stage waste liquid, comprising a kettle body, a top plate assembly, a bottom plate and an anti-rotation feeding mechanism, wherein the top plate assembly, the kettle body, the bottom plate and the anti-rotation feeding mechanism are sealed and sleeved in sequence from top to bottom, a transmission shaft is sleeved on a middle bearing of the bottom surface of the top plate assembly, a stirring mechanism is sleeved on the outer surface of the transmission shaft, a cleaning mechanism is sleeved on the bottom end of the outer surface of the stirring mechanism, a scraping mechanism is provided in the middle of the top surface of the bottom plate, and a support column is provided on the bottom surface of the bottom plate.
[0008] Preferably, the top plate assembly includes a top cover plate, the bottom surface of the top cover plate is sealed with the top surface of the kettle body, the top surface of the top cover plate is mounted with a drive motor, the bottom end of the output end of the drive motor is mounted with the top bearing of the transmission shaft, the right side of the top surface of the top cover plate is connected to a first feed pipe, the right side of the top surface of the top cover plate is connected to a second feed pipe, and the left end of the top surface of the top cover plate is connected to a main feed pipe.
[0009] Preferably, the anti-rotation unloading mechanism includes a positioning sleeve, the top surface of the positioning sleeve is connected to the middle part of the bottom surface of the chassis, the inner cavity sealing sleeve of the positioning sleeve is provided with a unloading tube, the bottom end of the unloading tube is connected to an adjusting tube, the bottom surface of the adjusting tube is connected to an adjusting block, the bottom surface bearing sleeve of the adjusting block is provided with a connecting pipe, the top surface of the unloading tube is provided with an anti-rotation cover, and the top surface of the anti-rotation cover is provided with a sealing top plate.
[0010] Preferably, the stirring mechanism comprises a spiral stirring blade and a sleeve column, the inner cavity of the spiral stirring blade is fixedly sleeved on the outer surface of the transmission shaft, and the sleeve column is sleeved on the outer surface of the spiral stirring blade.
[0011] Preferably, the cleaning mechanism includes a splicing seat, the top end of the splicing seat is fixedly mounted on the bottom end of the transmission shaft, support rods are evenly arranged around the bottom end of the outer surface of the splicing seat, a cleaning plate is arranged at the end of the support rod, and balance rods are evenly arranged around the top end of the outer surface of the splicing seat, and the outer end of the balance rod is connected to the inner side of the cleaning plate.
[0012] Preferably, the scraper mechanism includes a support seat, the bottom surface of the support seat is connected to the middle part of the bottom surface of the chassis inner cavity, a connecting column is provided on the middle bearing sleeve of the top surface of the support seat, an extension rod is provided on the outer surface of the connecting column, and a scraper pushing plate is provided on the bottom surface of the extension rod.
[0013] Preferably, the inner cavity of the spiral stirring blade is provided with a fitting hole, the size and shape of the fitting hole are matched with the size and shape of the transmission shaft, the bottom end of the splicing seat is fixedly mounted on the top surface of the connecting column, the circumferential surface of the support seat is provided with a discharge port, and the top surface of the inner cavity of the support seat is provided with a sealing groove, the size and shape of the sealing groove are matched with the size and shape of the top surface of the sealing top plate.
[0014] Preferably, a sealing limit ring is provided on the inner cavity side wall of the positioning sleeve, the inner diameter size and shape of the sealing limit ring are adapted to the size and shape of the outer surface of the discharge tube, the outer surface of the sealing top plate is provided with a top sealing ring, the top surface of the adjusting tube is provided with a bottom sealing ring located outside the discharge tube, and the middle part of the top surface of the sealing top plate is connected to a liquid guide tube.
[0015] Preferably, the number of the cleaning brush plates is three, and the three cleaning brush plates are evenly distributed in the inner cavity of the kettle body in the circumferential direction. A cleaning brush is provided on the outer surface of the cleaning brush plate, and the end of the cleaning brush is in contact with the inside of the kettle body.
[0016] Preferably, a gap is left between the bottom end of the scraper pushing plate and the bottom surface of the inner cavity of the chassis, and the size of the gap can be adjusted according to the position of the support seat and the connecting column sleeve.
[0017] An industrial impurity removal method for the waste liquid of the rear stage of galaxol chlorobenzene comprises the following steps:
[0018] S1: add 3000kg of chlorobenzene tower bottom waste liquid (chlorobenzene 80%, chloropropanol 10%, methylal and chloropropanol polymer 8%, indane 2%) into the main body of the kettle through the main feeding pipe, turn on the driving motor so that the output shaft of the driving motor can indirectly drive the set column, the cleaning plate and the scraper pushing plate to stir, connect the first feeding pipe with the external steam supply pipeline, and input steam for heating to raise the temperature in the kettle to 60-90°C;
[0019] S2: Connect the second feed pipe to the external pipeline, and slowly and uniformly add 120-200 kg of 98% sulfuric acid into the interior of the kettle body through the second feed pipe to ensure that the interior of the kettle body does not boil violently. The addition needs to be completed within 2-3 hours;
[0020] S3: Turn off the steam input of the first feed pipe, so that the interior of the kettle body is naturally cooled to 40°C, and 400 kg of pure water is added to the interior of the kettle body through the second feed pipe for water washing (to dilute part of the sulfuric acid that does not participate in the reaction), and then stirred for 1 hour, and then left to stand for 1 hour. The mixed liquid is naturally stratified inside the kettle body, and the lower layer of acid water is discharged to the external wastewater tank through the anti-rotation discharge mechanism;
[0021] S4: The chlorobenzene phase obtained in the upper layer inside the kettle body is retained inside the kettle body, and 400 kg of 5% sodium hydroxide solution (neutralized with sulfuric acid to make the reaction liquid alkaline) is added through the second feeding pipe, stirred for 1 hour, allowed to stand for 1 hour for natural stratification, and then the lower alkaline water phase is released through the anti-rotation discharge mechanism to obtain the treated chlorobenzene crude solution. The impurity peak of chloropropanol is ≤1% and the chlorobenzene content is ≥90% after gas chromatography.
[0022] Compared with the prior art, the present invention has the following beneficial effects:
[0023] 1. First of all, through the setting of the cleaning mechanism and the scraping mechanism, the inner wall of the kettle body and the bottom plate can be cleaned to avoid the accumulation of impurities generated by the liquid material during the reaction process on the inner wall of the kettle body and the bottom plate, which will make it impossible to clean up later. In addition, according to the setting shape of the set column and the scraper push plate, the liquid material inside the kettle body can be turned upside down and stirred.
[0024] 2. Secondly, by setting up the anti-rotation discharge mechanism and utilizing the threaded connection between the positioning sleeve and the adjusting sleeve, the use height of the anti-rotation cover can be adjusted relative to the positioning sleeve to avoid excessive vortex when the upper and lower layers of liquid are separated and discharged inside the kettle body, so that the retained available product will not be easily lost.
[0025] In summary, the present invention overcomes the shortcomings of the prior art, has a reasonable design and a compact structure, and utilizes the opposite settings of the stirring rotation directions to allow the liquid material in the kettle to be stirred upside down, and according to the optimization of the discharge end, the vortex of the layered liquid is weakened, and has a high social use value and application prospect. BRIEF DESCRIPTION OF THE DRAWINGS
[0026] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.
[0027] Figure 1 It is a schematic diagram of the overall structure explosion of the present invention.
[0028] Figure 2 It is a schematic diagram of the impurity removal process of the present invention.
[0029] Figure 3 It is a schematic diagram of the overall appearance structure of the present invention.
[0030] Figure 4 It is a structural schematic diagram of the chassis in the present invention.
[0031] Figure 5 It is a structural schematic diagram of the cleaning mechanism in the present invention.
[0032] Figure 6 It is a structural schematic diagram of the stirring mechanism in the present invention.
[0033] Figure 7 It is a structural schematic diagram of the scraping mechanism in the present invention.
[0034] Figure 8It is a schematic structural diagram of the opening stage of the anti-rotation feeding mechanism in the present invention.
[0035] Fig. 9 It is a schematic structural diagram of the closing stage of the anti-rotation feeding mechanism in the present invention.
[0036] Fig.10 It is a schematic diagram of the explosion structure of the anti-rotation feeding mechanism in the present invention.
[0037] In the figure: 1. kettle body; 2. top plate assembly; 201. top cover plate; 202. drive motor; 203. first feed pipe; 204. second feed pipe; 205. main feeding pipe; 3. bottom plate; 301. support column; 4. anti-rotation feeding mechanism; 41. positioning sleeve; 42. feeding tube; 43. adjusting tube; 433. bottom sealing ring; 44. adjusting block; 45. connecting pipe; 46. anti-rotation cover; 47. sealing top plate; 471. liquid guide tube; 5. transmission shaft; 6. stirring mechanism; 61. spiral stirring blade; 62. set column; 7. cleaning mechanism; 71. splicing seat; 72. support rod; 73. balance rod; 74. cleaning plate; 8. scraping mechanism; 81. support seat; 82. connecting column; 83. extension rod; 84. scraping push plate. DETAILED DESCRIPTION
[0038] In order to make the purpose, technical solution and advantages of the embodiments of the present invention clearer, the technical solution in the embodiments of the present invention will be clearly and completely described below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are 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.
[0039] Example 1
[0040] Reference Figure 1 , Figure 3-8 and Fig.10 , an industrial impurity removal system and method for the waste liquid of the rear stage of galaxol chlorobenzene, comprising a kettle body 1, a top plate assembly 2, a bottom plate 3 and an anti-rotation feeding mechanism 4, the top plate assembly 2, the kettle body 1, the bottom plate 3 and the anti-rotation feeding mechanism 4 are sealed and mounted in sequence from top to bottom, so that the inner cavity of the kettle body 1 forms a closed space, which is convenient for stirring and static treatment of raw materials, a transmission shaft 5 is sleeved on the middle bearing of the bottom surface of the top plate assembly 2, and the transmission shaft 5 can be first fixedly sleeved with the bottom end of the output shaft of the driving motor 202, so that the output shaft of the driving motor 202 drives the transmission shaft 5 to rotate, the outer surface of the transmission shaft 5 is fixedly sleeved with a stirring mechanism 6, and the bottom end of the outer surface of the stirring mechanism 6 is fixedly sleeved with a cleaning mechanism 7, the middle part of the top surface of the bottom plate 3 is fixedly bolted with a scraping mechanism 8, and the bottom surface of the bottom plate 3 is fixedly bolted with a support column 301.
[0041] Specifically, the top plate assembly 2 includes a top cover plate 201, the bottom surface of the top cover plate 201 is sealed with the top surface of the kettle body 1, the top surface of the top cover plate 201 is equipped with a drive motor 202, the bottom end of the output end of the drive motor 202 is equipped with the top bearing of the transmission shaft 5, the right side of the top surface of the top cover plate 201 is connected to a first feed pipe 203, the right side of the top surface of the top cover plate 201 is connected to a second feed pipe 204, and the left end of the top surface of the top cover plate 201 is connected to a main feed pipe 205. Through the setting of the top plate assembly 2, a drive source can be provided for the internal components of the kettle body 1, and a sealing effect can be provided for the top surface of the kettle body 1, and materials can be introduced from the first feed pipe 203, the second feed pipe 204 and the main feed pipe 205 into the interior of the kettle body 1 for stirring and static treatment.
[0042] Specifically, the anti-rotation unloading mechanism 4 includes a positioning sleeve 41, the top surface of the positioning sleeve 41 is connected to the middle part of the bottom surface of the chassis 3, the inner cavity sealing sleeve of the positioning sleeve 41 is provided with a unloading tube 42, the bottom end of the unloading tube 42 is connected to an adjusting tube 43, the bottom surface of the adjusting tube 43 is connected to an adjusting block 44, the bottom surface bearing sleeve of the adjusting block 44 is provided with a connecting pipe 45, the top surface of the unloading tube 42 is sleeved with an anti-rotation cover 46, and the top surface of the anti-rotation cover 46 is sleeved with a sealing top plate 47. Through the setting of the anti-rotation unloading mechanism 4, the internal components of the anti-rotation unloading mechanism 4 can be used to reduce the vortex during the unloading process of the material through the connection between the chassis 3 and the anti-rotation unloading mechanism 4, so as to avoid the mixing of the liquid surface in the early static stratification, thereby improving the efficiency of stratified unloading.
[0043] Specifically, the stirring mechanism 6 includes a spiral stirring blade 61 and a sleeve column 62. The inner cavity of the spiral stirring blade 61 is fixedly sleeved on the outer surface of the transmission shaft 5, and the sleeve column 62 is sleeved on the outer surface of the spiral stirring blade 61. Through the setting of the stirring mechanism 6, when the output shaft of the driving motor 202 drives the transmission shaft 5 to rotate, the spiral stirring blade 61 can rotate synchronously with the transmission shaft 5, so that the sleeve column 62 can stir the liquid inside the kettle body 1.
[0044] Specifically, the cleaning mechanism 7 includes a splicing seat 71, the top end of the splicing seat 71 is fixedly sleeved with the bottom end of the transmission shaft 5, the bottom end of the outer surface of the splicing seat 71 is evenly provided with support rods 72 in the circumferential direction, and the end of the support rod 72 is provided with a cleaning plate 74, and the top end of the outer surface of the splicing seat 71 is evenly provided with a balance rod 73 in the circumferential direction, and the outer end of the balance rod 73 is connected to the inner side of the cleaning plate 74. Through the internal component arrangement of the cleaning mechanism 7, a cleaning brush can be arranged on the outer surface of the cleaning plate 74. The cleaning brush is in the shape of a fan and can be directly fixed on the outer surface of the cleaning plate 74, which is convenient for cleaning the inner cavity side wall of the kettle body 1 and can be replaced regularly.
[0045] Specifically, the scraper mechanism 8 includes a support seat 81, the bottom surface of the support seat 81 is connected to the middle part of the bottom surface of the inner cavity of the chassis 3, the bearing sleeve in the middle part of the top surface of the support seat 81 is provided with a connecting column 82, the outer surface of the connecting column 82 is provided with an extension rod 83, and the bottom surface of the extension rod 83 is provided with a scraper pushing plate 84. The internal component arrangement of the scraper mechanism 8 can stir the liquid inside the chassis 3 and prevent impurities from being retained on the bottom surface of the inner cavity of the chassis 3. The scraper pushing plate 84 can contact the impurities attached to the bottom surface of the inner cavity of the chassis 3 to play a cleaning role.
[0046] Specifically, the inner cavity of the spiral stirring blade 61 is provided with a sleeve hole, the size and shape of the sleeve hole are matched with the size and shape of the transmission shaft 5, the bottom end of the splicing seat 71 is fixedly sleeved with the top surface of the connecting column 82, the circumferential surface of the support seat 81 is provided with a discharge port, and the top surface of the inner cavity of the support seat 81 is provided with a sealing groove, the size and shape of the sealing groove are matched with the size and shape of the top surface of the sealing top plate 47. The opening of the sleeve hole enables the spiral stirring blade 61 to be sleeved on the outer surface of the transmission shaft 5, the sleeve of the splicing seat 71 and the connecting column 82 can be installed in a fixed sleeve manner, and the sleeve between the connecting column 82 and the support seat 81 is fixed in the form of an embedded groove, which is convenient for installation and operation, and the opening of the discharge port cooperates with the internal components of the anti-rotation discharge mechanism 4, so that during the liquid discharge process, it can play a certain blocking role and avoid the situation where the discharge vortex is too large.
[0047] Specifically, a sealing limit ring is provided on the side wall of the inner cavity of the positioning sleeve 41, and the inner diameter and shape of the sealing limit ring are adapted to the size and shape of the outer surface of the discharge tube 42. The outer surface of the sealing top plate 47 is provided with a top sealing ring, and the top surface of the adjusting tube 43 is provided with a bottom sealing ring 433 located on the outside of the discharge tube 42. The middle part of the top surface of the sealing top plate 47 is connected to a liquid guide tube 471. The setting of the sealing limit ring and the top sealing ring can seal the connection between the anti-rotation discharge mechanism 4 and the chassis 3 when the internal components of the anti-rotation discharge mechanism 4 are in motion, thereby preventing liquid from flowing out from the connection points between the chassis 3 and the positioning sleeve 41 and the splicing gaps of the internal components of the anti-rotation discharge mechanism 4.
[0048] Specifically, there are three cleaning brush plates 74, which are evenly distributed in the inner cavity of the kettle body 1 in the circumferential direction. A cleaning brush is provided on the outer surface of the cleaning brush plate 74, and the end of the cleaning brush is in contact with the interior of the kettle body 1. The cleaning brush plate 74 is set at an angle interval of 120 degrees, which can maximize the cleaning operation of the inner cavity side wall of the kettle body 1 in cooperation with the cleaning brush. The outer surface of the cleaning brush is provided with bristles, and its inner surface can be tightly fitted with the outer surface of the cleaning brush plate 74, and the two are installed and fixed by bolts. The lightness and size of the cleaning brush need to be compatible with the shape and size of the cleaning brush plate 74.
[0049] Specifically, a gap is left between the bottom end of the scraper pushing plate 84 and the bottom surface of the inner cavity of the chassis 3, and the size of the gap can be adjusted according to the position of the support seat 81 and the connecting column 82. The gap left at the bottom end of the scraper pushing plate 84 prevents the scraper pushing plate 84 from making direct contact with the bottom surface of the inner cavity of the chassis 3, avoids hard collision during rotation, and avoids damage to the scraper pushing plate 84 and the chassis 3.
[0050] Example 2
[0051] Reference Fig. 9 The difference between this embodiment and embodiment 1 is that the fitting position between the positioning sleeve 41 and the discharge tube 42 can be adjusted. According to the corresponding threads on the outer surface of the adjustment tube 43 and the bottom end of the inner side wall of the positioning sleeve 41, it can be adjusted by rotation, so that the top surface of the sealing top plate 47 is separated from the top surface of the inner cavity of the support seat 81, and the top surface height of the liquid guide tube 471 is matched with the height of the bottom surface of the inner cavity of the chassis 3, so that the material liquid inside the kettle body 1 can be directly discharged through the liquid guide tube 471 without passing through the anti-rotation cover 46, so that the anti-rotation discharge mechanism 4 can perform the opening and closing operations of the anti-rotation program. This type of improvement can avoid the interference of the internal components of the anti-rotation discharge mechanism 4 causing the discharge speed to slow down when the kettle body 1 does not need to discharge materials in layers.
[0052] For other structures not described, refer to Example 1.
[0053] Working principle: In the present invention, firstly, the waste liquid at the bottom of the chlorobenzene tower is introduced into the interior of the kettle body 1 from the main feeding pipe 205 through external pumping, and then the driving motor 202 is turned on, so that the output shaft of the driving motor 202 can drive the transmission shaft 5 to rotate, so that the transmission shaft 5 drives the set column 62, the cleaning plate 74 and the scraper pushing plate 84 to rotate synchronously in the same direction, and the heating steam is introduced into the interior of the kettle body 1 through the first feeding pipe 203, so that the temperature inside the kettle body 1 can reach 60-90°C, so that the interior of the kettle body 1 can be stirred and steam heated, and then sulfuric acid is dripped into the interior of the kettle body 1 through the second feeding pipe 204 to ensure that the interior of the kettle body 1 will not boil violently, and the time for dripping sulfuric acid needs to be controlled within 2-3 hours, and then the input of heating steam is closed to allow The internal temperature of the kettle body 1 is controlled at 40°C, and pure water is added to the inside of the kettle body 1 through the second feed pipe 204 for water washing, and stirring is started simultaneously. The stirring time is controlled at 1 hour. After the stirring is completed, the liquid inside the kettle body 1 needs to be left to stand for 1 hour so that the mixed liquid inside the kettle body 1 can be naturally stratified. The waste water in the lower layer of the kettle body 1 is directly discharged through the anti-rotation discharge mechanism 4. In the process of discharging the waste water, the anti-rotation cover 46 needs to be raised to play an anti-rotation role for the discharge of the liquid. The chlorobenzene phase in the upper layer of the kettle body 1 is retained in the kettle body 1, and then sodium hydroxide solution is added. The stirring and standing operations for 1 hour are performed again. The lower layer of alkaline water caused by the stratification of the mixed liquid is directly discharged through the anti-rotation discharge mechanism 4 to obtain the treated chlorobenzene crude solution.
[0054] Example 3
[0055] Reference Figure 2 , an industrial impurity removal method for the waste liquid of galaxol chlorobenzene rear stage, comprising the following steps:
[0056] S1: 3000 kg of chlorobenzene tower bottom waste liquid (chlorobenzene 80%, chloropropanol 10%, methylal and chloropropanol polymer 8%, indane 2%) is added into the kettle body 1 through the main feeding pipe 205, and the driving motor 202 is turned on so that the output shaft of the driving motor 202 can indirectly drive the set column 62, the cleaning plate 74 and the scraper pushing plate 84 to stir, and the first feeding pipe 203 is connected to the external steam supply pipeline, and steam is input for heating to raise the temperature in the kettle to 60-90°C;
[0057] S2: Connect the second feed pipe 204 to the external pipeline, and slowly and uniformly add 120-200 kg of 98% sulfuric acid to the interior of the kettle body 1 through the second feed pipe 204 to ensure that the interior of the kettle body 1 does not boil violently. The addition needs to be completed within 2-3 hours;
[0058] S3: The steam input of the first feed pipe 203 is closed, so that the interior of the kettle body 1 is naturally cooled to 40°C, and 400 kg of pure water is added to the interior of the kettle body 1 through the second feed pipe 204 for water washing (to dilute part of the sulfuric acid that does not participate in the reaction), and then stirred for 1 hour, and then left to stand for 1 hour, and the mixed liquid is naturally stratified inside the kettle body 1, and the lower layer of acid water is discharged to the external wastewater tank through the anti-rotation discharge mechanism 4;
[0059] S4: The chlorobenzene phase obtained in the upper layer inside the kettle body 1 is retained inside the kettle body 1, and 400 kg of 5% sodium hydroxide solution (neutralized with sulfuric acid to make the reaction solution alkaline) is added through the second feed pipe 204, stirred for 1 hour, allowed to stand for 1 hour for natural stratification, and then the lower alkaline water phase is released through the anti-rotation discharge mechanism 4 to obtain the treated chlorobenzene crude solution. The chloropropanol impurity peak is ≤1% and the chlorobenzene content is ≥90% after gas chromatography detection.
[0060] Example 4
[0061] The difference between this embodiment and embodiment 3 is that the temperature of the S1 stage is controlled at 60°C, 200 kg of sulfuric acid with a concentration of 98% is added dropwise in the S2 stage, resulting in the discharge of the lower layer acid water in the S3 stage being about 420 kg, so that the amount of alkaline water in the lower layer in the S4 stage is about 400 kg, the output of crude chlorobenzene is about 2700 kg, and the impurity peak of chloropropanol is 0.6% and the chlorobenzene content is 93% after gas chromatography detection.
[0062] For other steps not described, refer to Example 3.
[0063] Example 5
[0064] The difference between this embodiment and embodiment 3 is that the temperature of the S1 stage is controlled at 60°C, 180 kg of sulfuric acid with a concentration of 98% is added dropwise in the S2 stage, resulting in the discharge of about 410 kg of acid water in the lower layer in the S3 stage, so that the amount of alkaline water in the lower layer in the S4 stage is about 400 kg, the output of crude chlorobenzene is about 2700 kg, and the impurity peak of chloropropanol is 0.8% and the chlorobenzene content is 92% after gas chromatography.
[0065] For other steps not described, refer to Example 3.
[0066] Example 6
[0067] The difference between this embodiment and embodiment 3 is that the temperature of the S1 stage is controlled to 60°C, the content of the chlorobenzene bottom waste liquid pumped into the kettle body 1 in the S1 stage is (chlorobenzene 84%, chloropropanol 8%), 150 kg of sulfuric acid with a concentration of 98% is added dropwise in the S2 stage, resulting in the discharge of the lower layer of acid water in the S3 stage being about 400 kg, so that the amount of alkaline water in the lower layer in the S4 stage is about 400 kg, the output of crude chlorobenzene is about 2700 kg, and the chloropropanol impurity peak is 1% and the chlorobenzene content is 90% as detected by gas chromatography.
[0068] For other steps not described, refer to Example 3.
[0069] It can be seen from Examples 4-6 that, through the concentrated sulfuric acid reaction, the chloropropanol impurities in the chlorobenzene tower bottom waste liquid are significantly eliminated, and the chlorobenzene content is greatly increased, so it can be used as a crude product for distillation.
[0070] In the description of the present invention, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside", "clockwise", "counterclockwise", "axial", "radial", "circumferential" and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the accompanying drawings, and are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the referred device or element must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be understood as limiting the present invention.
[0071] In the present invention, unless otherwise clearly specified and limited, the terms "set", "install", "connect", "connect", "fix" and the like should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral one; it can be a mechanical connection, a direct connection, or an indirect connection through an intermediate medium, it can be the internal connection of two elements or the interaction relationship between two elements. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.
[0072] The control method of the present invention is automatic control through a controller. The control circuit of the controller can be implemented by simple programming by technicians in this field. The provision of power is also common knowledge in this field. The present invention is mainly used to protect mechanical devices, so the present invention will no longer explain the control method and circuit connection in detail.
[0073] The above description is only a preferred specific implementation manner of the present invention, but the protection scope of the present invention is not limited thereto. Any technician familiar with the technical field can make equivalent replacements or changes according to the technical scheme and inventive concept of the present invention within the technical scope disclosed by the present invention, which should be covered by the protection scope of the present invention.
Claims
1. An industrial impurity removal system for the waste liquid of the rear stage of galaxol chlorobenzene, comprising a kettle body (1), a top plate assembly (2), a bottom plate (3) and an anti-rotation feeding mechanism (4), characterized in that: The top plate assembly (2), the kettle body (1), the bottom plate (3) and the anti-rotation discharge mechanism (4) are sealed and sleeved in sequence from top to bottom; a transmission shaft (5) is sleeved on a bearing in the middle of the bottom surface of the top plate assembly (2); a stirring mechanism (6) is sleeved on the outer surface of the transmission shaft (5); a cleaning mechanism (7) is sleeved on the bottom end of the outer surface of the stirring mechanism (6); a scraping mechanism (8) is provided in the middle of the top surface of the bottom plate (3); and a support column (301) is provided on the bottom surface of the bottom plate (3); The anti-rotation material discharge mechanism (4) comprises a positioning sleeve (41), the top surface of the positioning sleeve (41) is connected to the middle part of the bottom surface of the chassis (3), the inner cavity sealing sleeve of the positioning sleeve (41) is provided with a material discharge tube (42), the bottom end of the material discharge tube (42) is connected to an adjustment tube (43), the bottom surface of the adjustment tube (43) is connected to an adjustment block (44), the bottom surface bearing sleeve of the adjustment block (44) is provided with a connecting pipe (45), the top surface of the material discharge tube (42) is provided with an anti-rotation cover (46), and the top surface of the anti-rotation cover (46) is provided with a sealing top plate (47); The inner cavity side wall of the positioning sleeve (41) is provided with a sealing limit ring, the inner diameter size and shape of the sealing limit ring are matched with the size and shape of the outer surface of the material discharge tube (42), the outer surface of the sealing top plate (47) is sleeved with a top sealing ring, the top surface of the adjustment tube (43) is provided with a bottom sealing ring (433) located outside the material discharge tube (42), and the middle part of the top surface of the sealing top plate (47) is connected to a liquid guide tube (471); The fitting position between the positioning sleeve (41) and the discharge tube (42) can be adjusted. According to the corresponding threads formed on the outer surface of the adjustment tube (43) and the bottom end of the inner side wall of the positioning sleeve (41), the adjustment can be made by rotation, so that the top surface of the sealing top plate (47) is separated from the top surface of the inner cavity of the support seat (81), and the height of the top surface of the liquid guide tube (471) is matched with the height of the bottom surface of the inner cavity of the bottom plate (3). The liquid in the kettle body (1) can be directly discharged through the liquid guide tube (471) without passing through the anti-rotation cover (46), so that the anti-rotation discharge mechanism (4) can be turned on and off to perform the anti-rotation program. When the kettle body (1) does not need to discharge materials in layers, the internal components of the anti-rotation discharge mechanism (4) can be prevented from interfering with each other to reduce the discharge speed.
2. The industrial impurity removal system for the waste liquid of the rear stage of galaxol chlorobenzene according to claim 1, characterized in that: The top plate assembly (2) comprises a top cover plate (201), the bottom surface of the top cover plate (201) is sealed with the top surface of the kettle body (1), the top surface of the top cover plate (201) is fitted with a drive motor (202), the bottom end of the output end of the drive motor (202) is fitted with a top bearing of a transmission shaft (5), the right side of the top surface of the top cover plate (201) is connected to a first feed pipe (203), the right side of the top surface of the top cover plate (201) is connected to a second feed pipe (204), and the left end of the top surface of the top cover plate (201) is connected to a main feeding pipe (205).
3. The industrial impurity removal system for the waste liquid of the rear stage of galaxol chlorobenzene according to claim 1, characterized in that: The stirring mechanism (6) comprises a spiral stirring blade (61) and a sleeve column (62); the inner cavity of the spiral stirring blade (61) is fixedly sleeved on the outer surface of the transmission shaft (5); and the sleeve column (62) is sleeved on the outer surface of the spiral stirring blade (61).
4. The industrial impurity removal system for the waste liquid of the rear stage of galaxol chlorobenzene according to claim 3, characterized in that: The cleaning mechanism (7) comprises a splicing seat (71), the top end of the splicing seat (71) is fixedly sleeved with the bottom end of the transmission shaft (5), support rods (72) are evenly arranged in the circumferential direction at the bottom end of the outer surface of the splicing seat (71), and a cleaning plate (74) is arranged at the end of the support rod (72), and a balance rod (73) is evenly arranged in the circumferential direction at the top end of the outer surface of the splicing seat (71), and the outer end of the balance rod (73) is connected to the inner side of the cleaning plate (74).
5. The industrial impurity removal system for the waste liquid of the rear stage of galaxol chlorobenzene according to claim 1, characterized in that: The scraper mechanism (8) comprises a support seat (81), the bottom surface of the support seat (81) is connected to the middle of the bottom surface of the inner cavity of the chassis (3), a bearing sleeve in the middle of the top surface of the support seat (81) is provided with a connecting column (82), an extension rod (83) is provided on the outer surface of the connecting column (82), and a scraper pushing plate (84) is provided on the bottom surface of the extension rod (83).
6. The industrial impurity removal system for the waste liquid of the rear stage of galaxol chlorobenzene according to claim 4, characterized in that: The inner cavity of the spiral stirring blade (61) is provided with a sleeve hole, the size and shape of the sleeve hole are compatible with the size and shape of the transmission shaft (5), the bottom end of the splicing seat (71) is fixedly sleeved with the top surface of the connecting column (82), the circumferential surface of the support seat (81) is provided with a discharge port, and the top surface of the inner cavity of the support seat (81) is provided with a sealing groove, the size and shape of the sealing groove are compatible with the size and shape of the top surface of the sealing top plate (47).
7. The industrial impurity removal system for the waste liquid of the rear stage of galaxol chlorobenzene according to claim 6, characterized in that: The number of the cleaning brush plates (74) is three, and the three cleaning brush plates (74) are evenly distributed in the circumferential direction in the inner cavity of the kettle body (1). Cleaning brushes are provided on the outer surfaces of the cleaning brush plates (74), and the ends of the cleaning brushes are in contact with the interior of the kettle body (1).
8. The industrial impurity removal system for the waste liquid of the rear stage of galaxol chlorobenzene according to claim 5, characterized in that: A gap is provided between the bottom end of the scraper pushing plate (84) and the bottom surface of the inner cavity of the chassis (3), and the size of the gap can be adjusted according to the position of the support seat (81) and the connecting column (82).
9. A method for removing impurities from an industrial impurity removal system of the galaxol chlorobenzene waste liquid of any one of claims 1 to 7, characterized in that: The following steps are involved: S1: 3000 kg of chlorobenzene tower bottom waste liquid (chlorobenzene 80%, chloropropanol 10%, methylal and chloropropanol polymer 8%, indane 2%) is added to the kettle body (1) through the main feeding pipe (205), the driving motor (202) is turned on, so that the output shaft of the driving motor (202) can indirectly drive the set column (62), the cleaning plate (74) and the scraper pushing plate (84) to stir, the first feeding pipe (203) is connected to the external steam supply pipeline, and steam is input for heating to raise the temperature in the kettle to 60-90° C.; S2: connecting the second feed pipe (204) to an external pipeline, and slowly and uniformly dripping 120-200 kg of 98% sulfuric acid into the interior of the kettle body (1) through the second feed pipe (204), ensuring that the interior of the kettle body (1) does not boil violently, and the dripping needs to be completed within 2-3 hours; S3: the steam input of the first feed pipe (203) is closed, so that the interior of the kettle body (1) is naturally cooled to 40°C, 400 kg of pure water is added to the interior of the kettle body (1) through the second feed pipe (204) for water washing (to dilute part of the sulfuric acid that has not participated in the reaction), and then stirred for 1 hour, and then allowed to stand for 1 hour, the mixed liquid is naturally stratified inside the kettle body (1), and the lower layer of acid water is discharged to the external wastewater tank through the anti-rotation discharge mechanism (4); S4: The chlorobenzene phase obtained in the upper layer inside the kettle body (1) is retained inside the kettle body (1), and 400 kg of 5% sodium hydroxide solution (neutralized with sulfuric acid to make the reaction solution alkaline) is added through the second feed pipe (204), stirred for 1 hour, left to stand for 1 hour to naturally separate, and then the lower alkaline water phase is discharged through the anti-rotation discharge mechanism (4) to obtain a treated chlorobenzene crude solution. The chloropropanol impurity peak is ≤1% and the chlorobenzene content is ≥90% as detected by gas chromatography.
Citation Information
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