CN112191196B - Hydrolysis device for preparing paratoluensulfonyl chloride and processing technology - Google Patents
Hydrolysis device for preparing paratoluensulfonyl chloride and processing technology Download PDFInfo
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- CN112191196B CN112191196B CN202010973227.XA CN202010973227A CN112191196B CN 112191196 B CN112191196 B CN 112191196B CN 202010973227 A CN202010973227 A CN 202010973227A CN 112191196 B CN112191196 B CN 112191196B
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- 238000006460 hydrolysis reaction Methods 0.000 title claims abstract description 128
- YYROPELSRYBVMQ-UHFFFAOYSA-N 4-toluenesulfonyl chloride Chemical compound CC1=CC=C(S(Cl)(=O)=O)C=C1 YYROPELSRYBVMQ-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 230000007062 hydrolysis Effects 0.000 title claims abstract description 39
- 238000012545 processing Methods 0.000 title claims abstract description 10
- 238000005516 engineering process Methods 0.000 title claims abstract description 6
- 230000007246 mechanism Effects 0.000 claims abstract description 127
- 238000003756 stirring Methods 0.000 claims abstract description 106
- 230000005540 biological transmission Effects 0.000 claims abstract description 103
- 238000006243 chemical reaction Methods 0.000 claims abstract description 88
- 238000004140 cleaning Methods 0.000 claims abstract description 35
- 239000002904 solvent Substances 0.000 claims abstract description 32
- 239000000203 mixture Substances 0.000 claims abstract description 13
- 238000000926 separation method Methods 0.000 claims abstract description 7
- 238000004090 dissolution Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 90
- 238000000034 method Methods 0.000 claims description 25
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 21
- 230000008569 process Effects 0.000 claims description 19
- 238000002425 crystallisation Methods 0.000 claims description 14
- 230000008025 crystallization Effects 0.000 claims description 14
- 238000005507 spraying Methods 0.000 claims description 13
- 238000004519 manufacturing process Methods 0.000 claims description 11
- KEQGZUUPPQEDPF-UHFFFAOYSA-N 1,3-dichloro-5,5-dimethylimidazolidine-2,4-dione Chemical compound CC1(C)N(Cl)C(=O)N(Cl)C1=O KEQGZUUPPQEDPF-UHFFFAOYSA-N 0.000 claims description 10
- XTHPWXDJESJLNJ-UHFFFAOYSA-N chlorosulfonic acid Substances OS(Cl)(=O)=O XTHPWXDJESJLNJ-UHFFFAOYSA-N 0.000 claims description 10
- 230000001360 synchronised effect Effects 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 9
- 238000003860 storage Methods 0.000 claims description 7
- 239000002351 wastewater Substances 0.000 claims description 5
- 238000004891 communication Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 4
- 230000009467 reduction Effects 0.000 claims description 4
- 238000012546 transfer Methods 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 2
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 11
- 238000010586 diagram Methods 0.000 description 9
- 238000011084 recovery Methods 0.000 description 8
- 238000007599 discharging Methods 0.000 description 7
- 230000001276 controlling effect Effects 0.000 description 6
- 238000005406 washing Methods 0.000 description 5
- 239000000975 dye Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 230000005484 gravity Effects 0.000 description 4
- 230000017525 heat dissipation Effects 0.000 description 4
- 239000007921 spray Substances 0.000 description 4
- 239000003814 drug Substances 0.000 description 3
- 239000000575 pesticide Substances 0.000 description 3
- 239000000376 reactant Substances 0.000 description 3
- 230000009471 action Effects 0.000 description 2
- 239000012043 crude product Substances 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000011010 flushing procedure Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- UWHURBUBIHUHSU-UHFFFAOYSA-N 2-[(4-methoxy-6-methyl-1,3,5-triazin-2-yl)carbamoylsulfamoyl]benzoic acid Chemical compound COC1=NC(C)=NC(NC(=O)NS(=O)(=O)C=2C(=CC=CC=2)C(O)=O)=N1 UWHURBUBIHUHSU-UHFFFAOYSA-N 0.000 description 1
- 239000005578 Mesotrione Substances 0.000 description 1
- 239000005808 Metalaxyl-M Substances 0.000 description 1
- SJEYSFABYSGQBG-UHFFFAOYSA-M Patent blue Chemical compound [Na+].C1=CC(N(CC)CC)=CC=C1C(C=1C(=CC(=CC=1)S([O-])(=O)=O)S([O-])(=O)=O)=C1C=CC(=[N+](CC)CC)C=C1 SJEYSFABYSGQBG-UHFFFAOYSA-M 0.000 description 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- 239000005618 Sulcotrione Substances 0.000 description 1
- 239000000980 acid dye Substances 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000000986 disperse dye Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000011552 falling film Substances 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 239000000543 intermediate Substances 0.000 description 1
- 239000003562 lightweight material Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- KPUREKXXPHOJQT-UHFFFAOYSA-N mesotrione Chemical compound [O-][N+](=O)C1=CC(S(=O)(=O)C)=CC=C1C(=O)C1C(=O)CCCC1=O KPUREKXXPHOJQT-UHFFFAOYSA-N 0.000 description 1
- ZQEIXNIJLIKNTD-GFCCVEGCSA-N metalaxyl-M Chemical compound COCC(=O)N([C@H](C)C(=O)OC)C1=C(C)C=CC=C1C ZQEIXNIJLIKNTD-GFCCVEGCSA-N 0.000 description 1
- FWFGVMYFCODZRD-UHFFFAOYSA-N oxidanium;hydrogen sulfate Chemical compound O.OS(O)(=O)=O FWFGVMYFCODZRD-UHFFFAOYSA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 235000013547 stew Nutrition 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- PQTBTIFWAXVEPB-UHFFFAOYSA-N sulcotrione Chemical compound ClC1=CC(S(=O)(=O)C)=CC=C1C(=O)C1C(=O)CCCC1=O PQTBTIFWAXVEPB-UHFFFAOYSA-N 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
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Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F33/00—Other mixers; Mixing plants; Combinations of mixers
- B01F33/80—Mixing plants; Combinations of mixers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F33/00—Other mixers; Mixing plants; Combinations of mixers
- B01F33/80—Mixing plants; Combinations of mixers
- B01F33/836—Mixing plants; Combinations of mixers combining mixing with other treatments
- B01F33/8362—Mixing plants; Combinations of mixers combining mixing with other treatments with chemical reactions
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/02—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof
- C07C303/04—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof by substitution of hydrogen atoms by sulfo or halosulfonyl groups
- C07C303/08—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof by substitution of hydrogen atoms by sulfo or halosulfonyl groups by reaction with halogenosulfonic acids
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The invention relates to a hydrolysis device for preparing paratoluensulfonyl chloride, which comprises a reaction kettle, a cleaning mechanism, a uniform dripping mechanism, a stirring mechanism and a gasoline transmission mechanism, and also provides a paratoluensulfonyl chloride processing technology, which comprises the following steps: step one, producing tosyl chloride; step two, hydrolysis reaction; step three, adjusting the reaction temperature; step four, dissolution reaction; step five, self-cleaning; step six, standing and separating; the invention solves the technical problems that when solvent gasoline is added and dissolved, stirring is needed, a stirring piece is not beneficial to full layering and later separation of a mixture, the mixture remained on the stirring piece cannot be cleaned and discharged in time, and the precision of the hydrolysis reaction at this time is reduced and the precision of the next hydrolysis reaction is influenced.
Description
Technical Field
The invention relates to the technical field of paratoluensulfonyl chloride, in particular to a hydrolysis device for preparing paratoluensulfonyl chloride and a processing technology.
Background
The p-toluenesulfonyl chloride is used as a fine chemical product, widely applied to the dye, medicine and pesticide industries, and mainly used for manufacturing intermediates of disperse dyes, ice dyes and acid dyes in the dye industry; the preparation method is mainly used for producing sulfa drug metsulfuron and the like in the medical industry; the pesticide industry is mainly used for mesotrione, sulcotrione, metalaxyl-M and the like, and with the continuous development of the dye, medicine and pesticide industries, the international demand for the product is increasing, especially in Europe and America, and the market prospect is wide.
Patent No. CN2015209956449 discloses a refining system of a p-toluenesulfonyl chloride crude product, which comprises a dissolving kettle, a washing kettle, a filter, a crystallization kettle, a centrifugal separator, a dryer and a solvent oil recovery mechanism, wherein the dissolving kettle is connected with the washing kettle through a pipeline; the feeding port of the dissolving kettle is connected with the crude product storage tank, the discharging port of the dissolving kettle is connected with the feeding port of the washing kettle, the discharging port of the washing kettle is connected with the feeding port of the filter, the liquid-phase discharging port of the filter is connected with the crystallization kettle, the discharging port of the crystallization kettle is connected with the centrifugal separator, and the solid-phase discharging port of the centrifugal separator is connected with the dryer; the solvent oil recovery mechanism comprises a first-stage recovery mechanism and a second-stage recovery mechanism which are sequentially connected, wherein a solvent oil recovery storage tank is arranged in each of the first-stage recovery mechanism and the second-stage recovery mechanism, and the solvent oil recovery storage tank is connected with the dissolving kettle.
However, in the in-service use process, the inventor finds that solvent gasoline needs to be stirred when being added into the dissolving work, and then the stirring piece is unfavorable for the mixture to carry out sufficient layering and later stage separation work, and the mixture that remains on the stirring piece can not in time be washed and discharged in addition, influences the problem of the hydrolysis reaction precision next time when reducing this hydrolysis reaction precision.
Disclosure of Invention
Aiming at the defects in the prior art, the driving mechanism is arranged to drive the uniform water dripping mechanism, and the uniform water dripping mechanism finishes the intermittent water dripping work and uniformly falls off in the downward moving process; on the other hand changes the atmospheric pressure below the even mechanism that drips in real time, when pressure is crescent and then make the temperature decline of this reaction space slow, utilize actuating mechanism to generate heat to reation kettle when the during operation heat dissipation gives off simultaneously, make the temperature in the reation kettle descend to 50 ℃ of temperature time lengthening from 70 ℃, and then realize 70 ℃ to 50 ℃ within a range water assurance dropwise add work that finishes, thereby solved solvent gasoline when adding dissolving the work, need stir, and then the stirring piece is unfavorable for the mixture to carry out abundant layering and later stage separation work, the mixture that persists on the stirring piece can't in time wash the discharge in addition, influence the technical problem of next hydrolysis precision when reducing this hydrolysis precision.
Aiming at the technical problems, the technical scheme is as follows: a hydrolysis device for preparing paratoluensulfonyl chloride comprises a reaction kettle, a cleaning mechanism, a uniform dripping mechanism, a stirring mechanism and a gasoline transmission mechanism, wherein the cleaning mechanism, the uniform dripping mechanism and the stirring mechanism are arranged in the reaction kettle and are arranged along the vertical direction, and the gasoline transmission mechanism is arranged outside the reaction kettle and is communicated with the reaction kettle;
the uniform dripping mechanism comprises a water container arranged outside the reaction kettle, a first connecting pipe, a uniform dripping assembly, a driving mechanism and a discontinuous assembly, wherein one end of the first connecting pipe is communicated with the water container, the other end of the first connecting pipe is hermetically connected with the inside of the reaction kettle, the uniform dripping assembly is arranged in the reaction kettle and is communicated with the first connecting pipe, the driving mechanism drives the uniform dripping assembly to lift along the vertical direction and is positioned outside the reaction kettle, the discontinuous assembly is in synchronous transmission with the driving mechanism and controls the discontinuous dripping of water in the water container, and the driving mechanism is used for adjusting the temperature in the reaction kettle;
the stirring mechanism comprises a stirring component arranged on the inner wall of the reaction kettle in a sliding manner, a first transmission component which is driven by the driving mechanism to be in synchronous transmission and is used for driving the stirring component to be in transmission along the vertical direction, and a driving component used for driving the stirring component to rotate circumferentially;
the cleaning mechanism comprises a cleaning component arranged at the upper end of the reaction kettle and positioned above the stirring mechanism and a collecting component arranged outside the reaction kettle;
the gasoline transmission mechanism comprises an oil container and a second transmission assembly, wherein the oil container is communicated with the reaction kettle and the cleaning assembly respectively, and the second transmission assembly is in synchronous transmission with the driving assembly and is used for driving oil in the oil container to enter the reaction kettle.
Preferably, the uniform water dripping assembly comprises a hose which is in sealed communication with the first connecting pipe, a second pressure limiting assembly which is in sealed communication with the lower end of the hose, and a first pressure limiting assembly and a third pressure limiting assembly which are respectively positioned at two sides of the second pressure limiting assembly, the first pressure limiting assembly, the second pressure limiting assembly and the third pressure limiting assembly are in elastic contact and sealed contact with the contact part of the inner wall of the reaction kettle, the first pressure limiting assembly and the third pressure limiting assembly respectively comprise a pressure limiting plate a which is slidably arranged on the inner wall of the reaction kettle and is arranged in a hollow structure, the second pressure limiting assembly comprises a pressure limiting plate b which is hinged with the pressure limiting plate a and is arranged in a hollow structure, a driving shaft a which drives the pressure limiting plate b to rotate and is arranged on the pressure limiting plate a, a first transmission gear which is coaxial with and fixedly connected with the driving shaft a, and a first transmission gear which is meshed with the first transmission gear and is vertically arranged on the inner wall of the reaction kettle The lower end of the pressure limiting plate a is uniformly provided with water outlet holes a, two ends of the pressure limiting plate b are communicated with the two groups of pressure limiting plates a, the lower end of the pressure limiting plate b is uniformly provided with water outlet holes b, the first pressure limiting assembly is vertically provided with a limiting plate a, the upper end of the pressure limiting plate b is provided with a limiting plate b, the limiting plate b and the pressure limiting plate a of the third pressure limiting assembly are in discontinuous lap joint, the lower end of the third pressure limiting assembly is provided with a limiting plate c, the limiting plate c and the lower end of the pressure limiting plate b are in discontinuous lap joint, and the outer circumference formed by the two groups of pressure limiting plates a and the pressure limiting plate b is matched with the inner wall of the reaction kettle;
the intermittent assembly comprises a first linkage rack which is vertically arranged and fixedly connected with the telescopic end of the driving mechanism, a first linkage gear which is meshed with the first linkage rack, a fourth linkage bevel gear which is meshed with the first linkage gear, a fifth linkage bevel gear which is meshed with the fourth linkage bevel gear, a second linkage gear which is synchronously driven by the fifth linkage bevel gear and is arranged in a half-tooth structure, a second linkage rack which is meshed with the second linkage gear and is horizontally driven, and a telescopic spring a which is fixedly connected with the second linkage rack and is slidably arranged on the water container, wherein one end of a water baffle plate on the water container is fixedly connected with the second linkage rack, the other end of the water baffle plate is fixedly connected with the outer wall of the water container, and the telescopic spring a is sleeved outside the second linkage rack.
Preferably, the driving mechanisms are provided with two groups and are respectively connected with the first pressure limiting assembly and the third pressure limiting assembly, each driving mechanism comprises a telescopic cylinder with telescopic ends vertically arranged downwards and installed outside the reaction kettle, a driving rod fixedly connected with the telescopic ends of the telescopic cylinders and vertically arranged, a telescopic spring b sleeved outside the driving rod and a temperature control assembly sleeved outside the reaction kettle, the driving rod is fixedly connected with the upper end of the pressure limiting plate a, one end of the telescopic spring b is fixedly connected with the inner wall of the reaction kettle, and the other end of the telescopic spring b is fixedly connected with the upper end of the pressure limiting plate a;
the temperature control assembly comprises a cover box covered outside the telescopic cylinder, a heat control cavity attached to the outer wall of the reaction kettle, a heat transfer pipe with one end communicated with the inner wall of the cover box and the other end communicated with the heat control cavity, and a third transmission assembly for controlling the opening and closing of the cover box, wherein the third transmission assembly comprises a starting valve for controlling the opening and closing of the opening, a third linkage gear coaxial and synchronously driven with the valve, a linkage rod vertically arranged and fixedly connected with the telescopic end of the telescopic cylinder, a third linkage rack arranged at the upper end of the linkage rod and having a one-way tooth structure, and a fourth linkage rack arranged at the upper end of the linkage rod and having a one-way tooth structure, and the third linkage rack and the fourth linkage rack are both meshed with the third linkage gear and are opposite in one-way transmission direction.
Preferably, the stirring assembly comprises a slider a arranged in a groove b in the inner wall of the reaction kettle in a sliding manner and a stirring shaft rotatably arranged on the slider a, the slider a is arranged in a magnetic structure, two ends of the pressure limiting plate b are provided with stop blocks, the stop blocks are positioned in the pressure limiting plate b, a distance sensor is arranged on the limiting plate c, when the limiting plate c is in contact with the pressure limiting plate b, the stop blocks are ejected outwards and matched to enter the groove b, and when the limiting plate c is not in contact with the pressure limiting plate b, the stop blocks are reset inwards to enter the pressure limiting plate b;
the first transmission assembly comprises a second transmission rack which is fixedly connected with the telescopic end of any telescopic cylinder and is vertically arranged, a second transmission gear which is meshed with the second transmission rack, a third transmission rack which is meshed with the second transmission gear and is arranged opposite to teeth of the second transmission rack, a sliding block b of which the upper end is fixedly connected with the lower end of the third transmission rack, and a telescopic unit b of which the upper end is fixedly connected with the sliding block b and the lower end is fixedly connected with a support frame, the sliding blocks b and the sliding blocks a are arranged in a one-to-one correspondence manner and are magnetically attracted, and the support frame is sleeved on the outer wall of the reaction kettle;
the driving assembly comprises a driving motor, the driving motor is positioned outside the reaction kettle, the rotating end of the driving motor is positioned in the reaction kettle, the rotating end of the driving motor is provided with an elastic ring, and a notch is formed in the elastic ring and the caliber of the notch is smaller than the diameter of the transmission end of the stirring shaft.
Preferably, the cleaning assembly comprises a second connecting pipe arranged in the reaction kettle, a spraying arc plate which is communicated with the second connecting pipe and two ends of which are fixedly arranged on the inner wall of the reaction kettle, and a limiting arc plate which is arranged in a manner of being attached to the lower surface of the spraying arc plate and is rotationally arranged on the reaction kettle through a disc, a third transmission gear and a fourth transmission rack which is meshed with the third transmission gear and is fixedly connected with the upper end of the sliding block a are arranged on the disc, the spraying arc plate is arranged in an eighth structure, and the limiting arc plate is arranged in a half structure;
the collecting assembly comprises a discharge port arranged on the reaction kettle, a valve for controlling the opening and closing of the discharge port, a discharge pipe which is communicated with the discharge port and is obliquely arranged downwards, and a containing container positioned at the output end of the discharge pipe;
the second transmission assembly comprises a first bevel gear, a second bevel gear, a third connecting pipe and a control valve, wherein the first bevel gear is coaxially and fixedly connected with the output end of the driving motor, the second bevel gear is meshed with the first bevel gear, the third connecting pipe is arranged through the oil container, one end of the control valve is arranged on the third connecting pipe, the third connecting pipe is arranged through the third connecting pipe, the other end of the control valve is arranged through the third connecting pipe, the fourth communicating pipe is arranged through the third connecting pipe, one end of the fourth communicating pipe is arranged through the third connecting pipe, the other end of the fourth communicating pipe is arranged through the fifth communicating pipe, the second communicating pipe is arranged through the second connecting pipe, the fourth communicating pipe is arranged through the fifth communicating pipe, and the second bevel gear is synchronously driven through a synchronous belt.
A p-toluenesulfonyl chloride processing technology based on a hydrolysis device for preparing p-toluenesulfonyl chloride comprises the following steps:
step one, producing tosyl chloride, manually selecting a plurality of components of chlorosulfonic acid, adding the chlorosulfonic acid into a 3000L reaction kettle, dropwise adding a plurality of components of toluene into the 3000L reaction kettle under the condition of 30-50 ℃, after dropwise adding, heating and preserving heat;
step two, hydrolysis reaction, namely adding the mixture in the reaction kettle in the step one into the hydrolysis reaction kettle, and starting a driving mechanism to drip water under the condition of negative pressure;
step three, adjusting the reaction temperature, and synchronously with the step two, driving the first pressure limiting assembly and the third pressure limiting assembly to move downwards respectively by the driving mechanism, completing the dripping work and synchronously pressurizing the reaction space, meanwhile, introducing hot gas generated by the driving mechanism to the outer wall of the hydrolysis reaction kettle, and carrying out temperature heat conduction work on the inside of the hydrolysis reaction kettle, so that the cooling speed in the hydrolysis reaction kettle is slowed down in the hydrolysis reaction;
step four, carrying out dissolution reaction, wherein after the water is dripped, a period of time passes, the driving mechanism drives the stirring assembly to descend through the first transmission assembly until the stirring assembly descends to the driving assembly, the driving assembly drives the stirring assembly to rotate, stirring is completed, and then the driving assembly synchronously drives the second transmission assembly to introduce the solvent gasoline in the oil container into the hydrolysis reaction kettle;
step five, self-cleaning, wherein in the process of lifting the stirring assembly, the cleaning assembly finishes the cleaning work of the stirring shaft of the stirring assembly, meanwhile, the solvent gasoline and residues on the stirring shaft are flushed into a limiting arc plate of the stirring assembly below for collection, when a distance sensor on a discharge port on the reaction kettle senses the dripped flushing object, a valve is opened, and the solvent gasoline automatically falls to the discharge port along the limiting arc plate which inclines downwards and is output by means of gravity;
and step six, standing for separation, automatically layering after standing, putting a lower water layer into a wastewater storage tank, adding a solvent layer into a crystallization kettle for cooling crystallization, and keeping centrifugal work after crystallization is finished to obtain a finished product.
Preferably, in the first step, 1.65 tons of chlorosulfonic acid and 510kg of toluene are selected.
Preferably, in the second step, 150kg of water is selected, and the dropwise addition is completed while keeping the temperature below 50 ℃.
Preferably, in the fourth step, solvent gasoline is introduced into the hydrolysis reaction kettle at the temperature of 45 +/-5 ℃, the solvent gasoline is 1500kg, and the mixture is stirred for 30 min.
Preferably, in the sixth step, the standing time is 1-1.2 h, the cooling temperature is 5-10 ℃, and the centrifugal operation is kept for 1-1.5 h.
The invention has the beneficial effects that:
(1) according to the invention, the driving mechanism is arranged to drive the uniform dripping mechanism, and the uniform dripping mechanism completes intermittent dripping work of water and uniform dripping during the downward movement process; on the other hand, the air pressure below the uniform water dripping mechanism is changed in real time, the pressure is gradually increased, the temperature of the reaction space is slowly reduced, and meanwhile, the reaction kettle is heated by using heat emitted by the driving mechanism during heat dissipation during working, so that the time for reducing the temperature in the reaction kettle from 70 ℃ to 50 ℃ is prolonged, the work of ensuring the completion of dripping of water in the range of 70 ℃ to 50 ℃ is further realized, and the working efficiency is high and the automation degree is high;
(2) according to the invention, the uniform dripping mechanism is arranged to be matched with the stirring mechanism for up-and-down switching, when hydrolysis work is carried out in the reaction kettle, the stirring mechanism is lifted and separated from the reaction space, so that water dripped by the uniform dripping mechanism is fully contacted with reactants in the reaction kettle for hydrolysis reaction, and the hydrolysis effect is improved; after the reaction kettle finishes the hydrolysis work, the stirring mechanism is lowered into the reaction space, and the gasoline and the product are fully dissolved through the input of the gasoline, so that the dissolution depth work is improved;
(3) according to the invention, through the temperature control assembly, when the telescopic cylinder works, the heat generated by the telescopic cylinder is fully utilized and transmitted to the outer wall of the reaction kettle, and the outer wall is utilized to conduct heat to the inner wall of the reaction kettle, so that the temperature is regulated and controlled, the temperature cannot be rapidly reduced, the water is favorably dripped at the optimal hydrolysis temperature, and the hydrolysis reaction rate is increased; steam in the lift control cover box that utilizes telescopic cylinder lifts up at telescopic cylinder, and drive cover box is opened, and steam looses fast, and then avoids the temperature to last too high damage that causes the cylinder, energy consumption make full use of, green, recycle.
In conclusion, the device has the advantages of simple structure and full reaction, and is particularly suitable for the technical field of the paratoluensulfonyl chloride.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings described below are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic diagram of a first structure of a hydrolysis device for preparing p-toluenesulfonyl chloride.
FIG. 2 is a second schematic diagram of the structure of a hydrolysis apparatus for preparing p-toluenesulfonyl chloride.
FIG. 3 is a third schematic diagram of the structure of a hydrolysis apparatus for preparing p-toluenesulfonyl chloride.
Fig. 4 is a first structural diagram of the uniform dripping mechanism.
Fig. 5 is a schematic structural diagram of the first transmission assembly.
Fig. 6 is a transmission operation diagram of the driving mechanism.
Fig. 7 is a first schematic view illustrating a driving state of the uniform dripping assembly.
Fig. 8 is a second schematic diagram illustrating a driving state of the uniform water dropping assembly.
Fig. 9 is a third schematic diagram illustrating the driving state of the uniform dripping assembly.
Fig. 10 is a fourth schematic view illustrating a driving state of the uniform dripping assembly.
Fig. 11 is a fifth schematic view illustrating a driving state of the uniform dripping assembly.
Fig. 12 is a sixth schematic view illustrating a driving state of the uniform water dropping unit.
Fig. 13 is a first schematic view of the transmission state of the stirring assembly.
Fig. 14 is a schematic view of a transmission state of the stirring assembly.
Fig. 15 is a third schematic view of the transmission state of the stirring assembly.
Fig. 16 is a schematic view of the transmission state of the drive assembly.
FIG. 17 is a first schematic view of a driving state of the cleaning assembly.
FIG. 18 is a second schematic view of the cleaning assembly in a driving state.
FIG. 19 is a second schematic view of the cleaning assembly in a driving state.
FIG. 20 is a schematic diagram showing the flow structure of p-toluenesulfonyl chloride processing.
Detailed Description
The technical scheme in the embodiment of the invention is clearly and completely explained in the following by combining the drawings.
Example one
As shown in fig. 1 to fig. 3, a hydrolysis device for preparing paratoluensulfonyl chloride comprises a hydrolysis reaction kettle 101, and further comprises a cleaning mechanism 2, a uniform dripping mechanism 3, a stirring mechanism 4 and a gasoline transmission mechanism, wherein the cleaning mechanism 2, the uniform dripping mechanism 3 and the stirring mechanism 4 are arranged in the hydrolysis reaction kettle 101 and are arranged along the vertical direction, and the gasoline transmission mechanism is arranged outside the hydrolysis reaction kettle 101 and is communicated with the hydrolysis reaction kettle 101;
the uniform water dropping mechanism 3 comprises a water container 31 arranged outside the hydrolysis reaction kettle 101, a first connecting pipe 32, one end of which is communicated with the water container 31 and the other end of which is hermetically connected with the inside of the hydrolysis reaction kettle 101, a uniform water dropping component 33, which is arranged inside the hydrolysis reaction kettle 101 and is communicated with the first connecting pipe 32, a driving mechanism 34 and a discontinuous component 35, wherein the driving mechanism 34 drives the uniform water dropping component 33 to lift along the vertical direction and is positioned outside the hydrolysis reaction kettle 101, and the discontinuous component 35 is synchronously driven by the driving mechanism 34 and controls the discontinuous water dropping of the water in the water container 31, and is used for adjusting the temperature inside the hydrolysis reaction kettle 101;
the stirring mechanism 4 comprises a stirring assembly 41 arranged on the inner wall of the hydrolysis reaction kettle 101 in a sliding manner, a first transmission assembly 42 which is driven by the driving mechanism 34 in a synchronous transmission manner and is used for driving the stirring assembly 41 to transmit along the vertical direction, and a driving assembly 43 used for driving the stirring assembly 41 to rotate circumferentially;
the cleaning mechanism 2 comprises a cleaning component 21 arranged at the upper end of the hydrolysis reaction kettle 101 and above the stirring mechanism 4, and a collecting component arranged outside the hydrolysis reaction kettle 101;
the gasoline transmission mechanism comprises an oil container and a second transmission assembly, wherein the oil container is respectively communicated with the hydrolysis reaction kettle 101 and the cleaning assembly 21, and the second transmission assembly is synchronously transmitted with the driving assembly 43 and is used for driving oil in the oil container to enter the hydrolysis reaction kettle 101.
In the conventional process, since the hydrolysis reaction is an endothermic reaction, the hydrolysis speed is reduced along with the rapid reduction of the temperature, in this embodiment, the driving mechanism 34 is arranged to drive the uniform dripping mechanism 3, and the uniform dripping mechanism 3 completes the intermittent dripping work of water and uniformly drops in the process of moving downwards; on the other hand, the air pressure below the uniform water dripping mechanism 3 is changed in real time, the pressure is gradually increased, the temperature of the reaction space is slowly reduced, meanwhile, the reaction kettle is heated by the heat emitted by the driving mechanism 34 during heat dissipation in working, the temperature time of the temperature in the reaction kettle 1 is prolonged from 70 ℃ to 50 ℃, the water is ensured to be dripped in the range of 70 ℃ to 50 ℃, and the automatic water dripping device is high in working efficiency and high in automation degree.
Secondly, the uniform water dripping mechanism 3 is arranged to be matched with the stirring mechanism 4 for up-and-down switching, when hydrolysis work is carried out in the reaction kettle 1, the stirring mechanism 4 is lifted and separated from the reaction space, so that water dripped by the uniform water dripping mechanism 3 is fully contacted with reactants in the reaction kettle 1 for hydrolysis reaction, and the hydrolysis effect work is improved; after the reaction kettle 1 finishes the hydrolysis work, the stirring mechanism 4 descends into the reaction space, and the gasoline and the product are fully dissolved through the input of the gasoline, so that the dissolution depth work is improved.
Thirdly, the stirring mechanism 4 is matched with the cleaning mechanism 2, so that after the stirring mechanism 4 is used for stirring and dissolving the product fully, the product is lifted and conveyed to the upper end of the reaction kettle 1 in time to clean the stirring mechanism 4, on one hand, residual redundant product on the stirring mechanism 4 is washed by gasoline and collected, and the required solvent layer can be extracted while the full utilization rate of raw materials is improved; on the other hand, the stirring mechanism 4 is extracted from the solvent layer and the water layer, so that the production materials are favorably and fully subjected to standing and layering work, and the separation of the solvent and water after layering in the later period is also favorably realized, and the working efficiency is high.
Further, as shown in fig. 7 to 11, the uniform water dripping assembly 33 includes a hose 331 hermetically communicating with the first connection pipe 32, a second pressure limiting assembly 332 communicating with a lower end of the hose 331, and a first pressure limiting assembly 333 and a third pressure limiting assembly 334 respectively located at two sides of the second pressure limiting assembly 332, the first pressure limiting assembly 333, the second pressure limiting assembly 332, and the third pressure limiting assembly 334 are elastically contacted and hermetically contacted with a contact portion of the inner wall of the hydrolysis reaction kettle 101, the first pressure limiting assembly 333 and the third pressure limiting assembly 334 both include a pressure limiting plate a301 slidably disposed on the inner wall of the hydrolysis reaction kettle 101 and configured in a hollow structure, the second pressure limiting assembly 332 includes a pressure limiting plate b302 hinged to the pressure limiting plate a301 and configured in a hollow structure, and a driving shaft a303, a 302 driving the pressure limiting plate b302 to rotate and rotationally disposed on the pressure limiting plate a301, A first transmission gear 304 coaxially and fixedly connected with the driving shaft a303, and a first transmission rack 306 engaged with the first transmission gear 304 and vertically arranged in a groove a305 on the inner wall of the hydrolysis reactor 101, wherein the first transmission rack 306 comprises a first one-way tooth portion 30a and a second one-way tooth portion 30b with opposite teeth, the lower end of the pressure limiting plate a301 is uniformly provided with water outlet holes a335, both ends of the pressure limiting plate b302 are communicated with two groups of pressure limiting plates a301 and the lower end thereof is uniformly provided with water outlet holes b336, the first pressure limiting assembly 333 is vertically provided with a limiting plate a337, the upper end of the pressure limiting plate b302 is provided with a limiting plate b349, the limiting plate b349 is intermittently overlapped with the pressure limiting plate a301 of the third pressure limiting assembly 334, the lower end of the third pressure limiting assembly 334 is provided with a limiting plate c339, and the limiting plate c339 is intermittently overlapped with the lower end of the pressure limiting plate b302, the outer circumference formed by the two groups of pressure limiting plates a301 and b302 is matched with the inner wall of the hydrolysis reaction kettle 101;
the interrupting assembly 35 includes a first linkage rack 351 vertically fixed to the telescopic end of the driving mechanism 34, a first linkage gear 352 engaged with the first linkage rack 351, a fourth linkage bevel gear 357 engaged with the first linkage gear 352, and a fifth linkage bevel gear 358 engaged with the fourth linkage bevel gear 357, a second linkage gear 353 which is synchronously driven with the fifth linkage bevel gear 358 and is arranged in a half-tooth structure, a second linkage rack 354 which is meshed with the second linkage gear 353 and is horizontally driven, a water baffle which is fixedly connected with the second linkage rack 354 and is arranged on the water container 31 in a sliding manner, and an extension spring a356 which has one end fixedly connected with the second linkage rack 354 and the other end fixedly connected with the outer wall of the water container 31, wherein the extension spring a356 is sleeved outside the second linkage rack 354.
In the embodiment, the reaction kettle 1 is divided into an upper layer and a lower layer along the vertical direction by arranging the first pressure limiting component 333, the second pressure limiting component 332 and the third pressure limiting component 334, so that the effect of uniformly dripping water into the reaction kettle while adjusting the air pressure in the reaction kettle 1 in real time is facilitated; in addition, the lifting operation of the stirring mechanism 4 is realized by utilizing the rotation of the second pressure limiting component 332, and the structure is simple and ingenious.
In detail, when the hydrolysis work is performed in the reaction kettle 1, the first pressure limiting component 333, the second pressure limiting component 332 and the third pressure limiting component 334 are in a parallel state, water flows from the pressure limiting plate a301 and the pressure limiting plate b302 in sequence, at the moment, the stopper 414 is ejected outwards and matched to enter the groove b305, further, the first pressure limiting component 333, the second pressure limiting component 332 and the third pressure limiting component 334 are downward and form a sealing work with the inner wall of the reaction kettle 1, and then the first pressure limiting component 333, the second pressure limiting component 332 and the third pressure limiting component 334 move downward to perform a pressurization work; after the hydrolysis operation is completed, when the stirring mechanism 4 descends to the bottom of the reaction kettle, the second pressure limiting assembly 332 is lifted, the first transmission gear 304 is meshed with the first one-way tooth portion 30a, the pressure limiting plate b302 rotates, the opening operation is completed, and the stirring mechanism 4 descends smoothly; on the contrary, after the mixing and dissolving operations are completed, the stirring mechanism 4 is reset to be lifted up, the second pressure limiting assembly 332 is lowered, the first transmission gear 304 is meshed with the first one-way tooth portion 30b, the pressure limiting plate b302 rotates to complete the opening operation, and the stirring mechanism 4 is smoothly lifted up and separated from the bottom of the reaction kettle 1.
It should be noted that, by providing the limiting plate a337, the pressure limiting plate b302 is limited by being turned over, the turned pressure limiting plate b302 automatically falls down under the action of gravity after losing turning power, and the limiting plate b349 performs the limiting operation on the pressure limiting plate b302, so that the pressure limiting plate b302 is kept in a horizontal state.
Secondly, the intermittent assembly 35 is arranged to cooperate with the driving mechanism 34, so as to realize intermittent output of water in the water container 31, specifically, when the driving mechanism 34 descends, the first linkage rack 351 drives the first linkage gear 352 to rotate, the first linkage gear 352 drives the fourth linkage bevel gear 357 to rotate, the fourth linkage bevel gear 357 drives the fifth linkage bevel gear 358 to rotate, the fifth linkage bevel gear 358 drives the second linkage gear 353 to rotate, and the second linkage gear 353 drives the second linkage rack 354 to reciprocate, so as to realize intermittent water outlet work of the water outlet of the water container 31 by the water blocking plate.
Further, as shown in fig. 4 to fig. 6, two sets of driving mechanisms 34 are provided and are respectively connected to the first pressure limiting assembly 333 and the third pressure limiting assembly 334, and each driving mechanism includes a telescopic cylinder 341 with telescopic ends vertically arranged downward and installed outside the hydrolysis reaction kettle 101, a driving rod 342 vertically connected to the telescopic end of the telescopic cylinder 341, a telescopic spring b343 sleeved outside the driving rod 342, and a temperature control assembly 344 sleeved outside the hydrolysis reaction kettle 101, wherein the driving rod 342 is fixedly connected to the upper end of the pressure limiting plate a301, one end of the telescopic spring b343 is fixedly connected to the inner wall of the hydrolysis reaction kettle 101, and the other end of the telescopic spring b343 is fixedly connected to the upper end of the pressure limiting plate a 301;
the temperature control assembly 344 comprises a cover box 345 covering the outside of the telescopic cylinder 341, a heat control cavity 346 attached to the outer wall of the hydrolysis reactor 101, a heat transfer pipe 347 with one end communicated with the inner wall of the cover box 345 and the other end communicated with the heat control cavity 346, and a third transmission assembly 348 for controlling the opening and closing of the cover box 345, the third driving assembly 348 includes a start valve 3481 for controlling opening and closing, a third linkage gear 3482 coaxial with and synchronously driving the start valve 3481, a linkage 3483 vertically connected to the telescopic end of the telescopic cylinder 341, a third linkage rack 3484 with a one-way tooth structure disposed at the upper end of the linkage 3483, and a fourth linkage rack 3485 with a one-way tooth structure disposed at the upper end of the linkage 3483, the third interlocking gear 3484 and the fourth interlocking gear 3485 are both engaged with the third interlocking gear 3482 and have opposite unidirectional transmission directions.
In the embodiment, by providing the driving mechanism 34, on one hand, the driving mechanism 34 is used to drive the second pressure limiting assembly 332 to ascend and descend; on the other hand, the driving mechanism 34 is used for synchronously driving the stirring component 41 and the uniform dripping component 33 to reversely drive through the first transmission component 42, and the two powers are synchronously transmitted to work, so that the additional power is saved and the production cost is reduced.
Secondly, by arranging the temperature control component 344, when the telescopic cylinder 341 works, heat generated by the telescopic cylinder is fully utilized and transmitted to the outer wall of the reaction kettle 1, and then the heat is conducted to the inner wall of the reaction kettle 1 by utilizing the outer wall, so that the temperature is regulated and controlled in the endothermic reaction cooling process, the temperature cannot be rapidly reduced, on one hand, the completion of the dripping of water at the optimal hydrolysis temperature is facilitated, and in addition, the reaction rate of hydrolysis is improved; in addition, when the telescopic cylinder 341 is lifted, the hot air in the cover box 345 is controlled by the lifting of the telescopic cylinder 341 to drive the cover box 345 to be opened, and the hot air is quickly dissipated, so that the damage of the cylinder caused by the continuously overhigh temperature is avoided, and in addition, in the descending process of the telescopic cylinder 341, after the temperature in the cover box 345 is maximally increased to 60-65 ℃, the quick heat dissipation in the resetting of the telescopic cylinder 341 is realized; the energy consumption is fully utilized, and the method is green, environment-friendly and recyclable.
Further, as shown in fig. 13 to 15, the stirring assembly 41 includes a sliding block a412 slidably disposed in a groove b411 of the inner wall of the hydrolysis reactor 101 and a stirring shaft 413 rotatably disposed on the sliding block a412, the sliding block a412 is of a magnetic structure, two ends of the pressure limiting plate b302 are provided with stoppers 414, the stoppers 414 are located in the pressure limiting plate b302, the position limiting plate c339 is provided with a distance sensor, when the position limiting plate c339 is in contact with the pressure limiting plate b302, the stoppers 414 are outwardly ejected and matched into the groove b411, and when the position limiting plate c339 is not in contact with the pressure limiting plate b302, the stoppers 414 are inwardly reset into the pressure limiting plate b 302;
the first transmission assembly 42 comprises a second transmission rack 421 which is fixedly connected with the telescopic end of any one telescopic cylinder 341 and is vertically arranged, a second transmission gear 422 which is meshed with the second transmission rack 421, a third transmission rack 423 which is meshed with the second transmission gear 422 and is arranged opposite to teeth of the second transmission rack 421, a sliding block b424 of which the upper end is fixedly connected with the lower end of the third transmission rack 423, and a telescopic unit b425 of which the upper end is fixedly connected with the sliding block b424 and the lower end is fixedly connected with a support frame 426, the sliding blocks b424 and the sliding blocks a412 are arranged in a one-to-one correspondence manner and are magnetically attracted, and the support frame 426 is sleeved on the outer wall of the hydrolysis reaction kettle 101;
the driving assembly 43 comprises a driving motor 431, the driving motor 431 is located outside the hydrolysis reactor 101, the rotating end of the driving motor 431 is located inside the hydrolysis reactor 101, an elastic ring 432 is arranged at the rotating end of the driving motor 431, a gap 433 is arranged on the elastic ring 432, and the aperture of the gap 433 is smaller than the diameter of the transmission end of the stirring shaft 413.
In this embodiment, the stirring assembly 41 is arranged to cooperate with the first transmission assembly 42, so as to realize the automatic lifting operation of the stirring assembly 41, and simultaneously realize the automatic switching operation of the stirring assembly 41 and the uniform water dripping mechanism 3.
In detail, the second driving rack 421 moves downward under the action of the driving mechanism 34, the second driving rack 421 is engaged with the second driving gear 422, the second driving gear 422 drives the third driving rack 423 to move upward, then the third driving rack 423 drives the sliding block b424 to attract the sliding block a412 to slide upward, and the stopper 414 is located in the pressure limiting plate b302, so that the overturning of the pressure limiting plate b302 is not affected.
It should be noted that the stirring shaft 413 is made of a lightweight material.
In this embodiment, the driving assembly 43 is arranged to further realize the rotation stirring operation of the stirring assembly 41, when the rotation end of the stirring shaft 413 is too hard to be clamped into the elastic ring 432, the sensor on the elastic ring 432 sends a signal to drive the driving motor 431 to rotate, and the rotating driving motor 431 drives the stirring shaft 413 to rotate, so as to complete the mixing operation of the reactant and the gasoline; on the contrary, the rotation time of the driving motor 431 is set to be 30 minutes, after 30 minutes, the driving motor 431 stops working, at the moment, the gap 433 is positioned at the right upper end, the stop position of each time is consistent, after the driving motor 431 stops working, the telescopic cylinder 341 moves downwards again, the synchronous stirring shaft 413 is lifted upwards, and the stirring shaft 413 is separated from the elastic ring 432 too hard.
Further, as shown in fig. 17 to 19, the cleaning assembly 21 includes a second connecting pipe 211 disposed in the hydrolysis reactor 101, a spraying arc plate 212 which is communicated with the second connecting pipe 211 and has two ends fixedly disposed on the inner wall of the hydrolysis reactor 101, and a limiting arc plate 214 which is attached to the lower surface of the spraying arc plate 212 and is rotatably disposed on the hydrolysis reactor 101 through a disc 213, the disc 213 is provided with a third transmission gear 215 and a fourth transmission rack 216 which is engaged with the third transmission gear 215 and is fixedly connected to the upper end of the sliding block a412, the spraying arc plate 212 is disposed in an eighth structure, and the limiting arc plate 214 is disposed in a half structure;
the collecting assembly comprises a discharge port arranged on the hydrolysis reaction kettle 101, a valve for controlling the opening and closing of the discharge port, a discharge pipe which is communicated with the discharge port and is obliquely arranged downwards, and a containing container positioned at the output end of the discharge pipe;
the second transmission assembly include with the coaxial and fixed connection's of driving motor 431 output first awl tooth, with the second awl tooth that first awl tooth meshing set up, with third connecting pipe, the setting that oil container intercommunication set up are in control flap, one end on the third connecting pipe with third connecting pipe intercommunication set up and the other end with the fourth communicating pipe and the one end that hydrolysis reaction cauldron 101 in-connection set up with third connecting pipe intercommunication set up and the other end with the fifth communicating pipe that second connecting pipe 211 intercommunication set up, fourth communicating pipe with the bore of fifth communicating pipe sets up according to the proportion, the second awl tooth passes through hold-in range synchronous drive control flap's on-off work.
In the embodiment, the cleaning component 21 is arranged to be matched with the raised stirring component 41 to drive the spraying arc plate 212 to automatically rotate by 180 degrees, so that on one hand, the rotating spraying arc plate 212 can complete the bearing work of the dripped scoured objects, and simultaneously, the flow guide work is realized; on the other hand, the limit operation of the limit arc plate 214 on the spray arc plate 212 is realized, and the gasoline in the spray arc plate 212 is controlled to be automatically output; on the contrary, in the downward movement process of the stirring shaft, the limiting arc plate 214 is reset, on one hand, the smooth downward movement work of the stirring shaft is facilitated, and on the other hand, the dripping spraying work of gasoline in the spraying arc plate 212 is blocked.
It should be noted that the third transmission gear 215 is clamped and rotated on the support shaft on the reaction kettle 1 through a circular ring, the slider a412 is lifted up, the fourth transmission rack 216 drives the third transmission gear 215 to rotate, the rotating third transmission gear 215 drives the disc 213 to rotate together, the disc 213 drives the limit arc plate 214 to rotate 180 degrees together, the limit arc plate 214 is separated from the spray arc plate 212 after rotating, gasoline in the spray arc plate 212 drips downwards to complete the cleaning work of the stirring shaft 413, meanwhile, the gasoline and residues on the stirring shaft are washed together and enter the limit arc plate 214 below to be collected, when the distance sensor on the discharge port senses the dripped washing object, the valve is opened, and the gasoline automatically falls to the discharge port along the inclined downward limit arc plate 214 by means of gravity and is output.
In this embodiment, collect the subassembly through setting up, the mixture after the cleanness passes through the discharge gate and transmits to the discharging pipe, and rethread discharging pipe gets into to the receiver in, accomplishes the layering work that stews once more, and the solvent layer on upper strata adds the crystallization kettle after mixing with the solvent layer in the reation kettle, and the waste water storage tank is added after the water of lower floor mixes with the water in the reation kettle.
In this embodiment, through setting up second drive assembly, and then realize when stirring subassembly 41 carries out stirring during operation, in the petrol entering reation kettle of synchronous drive oil container, and then realize quantitative oil feed work, the synchronism is high and easily control, on the other hand reduction in production cost.
In detail, the first bevel gear drives the second bevel gear to rotate, the rotating second bevel gear drives the control valve to open, and after the control valve is opened, gasoline in the oil container respectively enters the reaction kettle 1 and the second connecting pipe 211 through the third connecting pipe; in addition, the caliber of the fifth communicating pipe is smaller than that of the fourth communicating pipe, because more gasoline needs to enter the reaction kettle 1, and less gasoline needs to enter the second connecting pipe 211 to clean the stirring shaft 413.
It should be noted that the operation time of the driving motor 431 is 30 minutes, the first 15 minutes is positive rotation, the last 15 minutes is negative rotation, and then the positive rotation and the negative rotation work improves the stirring effect on the one hand, and on the other hand, the control valve is controlled to be opened and closed, so that the quantitative control of the gasoline entering work is realized.
Example two
As shown in fig. 20, a process for processing p-toluenesulfonyl chloride comprises:
step one, producing tosyl chloride, manually selecting a plurality of components of chlorosulfonic acid, adding the chlorosulfonic acid into a 3000L reaction kettle 102, dropwise adding a plurality of components of toluene into the 3000L reaction kettle 102 again under negative pressure in an environment of 30-50 ℃, heating and preserving heat after the dropwise adding is finished;
step two, hydrolysis reaction, namely adding the mixture in the reaction kettle 102 in the step one into a hydrolysis reaction kettle 101, and starting a driving mechanism 34 to drip water under the condition of negative pressure;
step three, adjusting the reaction temperature, and synchronously with the step two, driving the first pressure limiting component 333 and the third pressure limiting component 334 to respectively drive the driving mechanism 34 to move downwards, completing the dripping work and synchronously pressurizing the reaction space, meanwhile, hot gas generated by the driving mechanism 34 is introduced to the outer wall of the hydrolysis reaction kettle 101 to conduct the temperature heat conduction work in the hydrolysis reaction kettle 101, so that the temperature reduction speed in the hydrolysis reaction kettle 101 is slowed down in the hydrolysis reaction;
step four, carrying out dissolution reaction, wherein after the water is dripped, a period of time passes, the driving mechanism 34 drives the stirring assembly 41 to descend through the first transmission assembly 42 until the stirring assembly 41 descends to the driving assembly 43, the driving assembly 43 drives the stirring assembly 41 to rotate, stirring is completed, and then the driving assembly 43 synchronously drives the second transmission assembly to introduce the solvent gasoline in the oil container into the hydrolysis reaction kettle 101;
step five, self-cleaning, in the process of lifting the stirring assembly 41, the cleaning assembly 21 finishes the cleaning work of the stirring shaft 413 of the stirring assembly 41, meanwhile, the solvent gasoline and residues on the stirring shaft 413 are flushed together and enter the limiting arc plate 214 of the stirring assembly 41 below for collection, when a distance sensor on a discharge port on the hydrolysis reaction kettle 101 senses the dripped flushing object, a valve is opened, and the solvent gasoline automatically falls to the discharge port along the limiting arc plate 214 which is inclined downwards and is output by means of gravity;
and step six, standing for separation, automatically layering after standing, putting a lower water layer into a wastewater storage tank 103, adding a solvent layer into a crystallization kettle 104 for cooling crystallization, and keeping centrifugal operation after crystallization is finished to obtain a finished product.
Further, as shown in FIG. 2, in the first step, chlorosulfonic acid is 1.65 tons, and toluene is 510 kg.
Further, as shown in FIG. 2, in the second step, 150kg of water was selected and added dropwise while maintaining at 50 ℃ or lower.
Further, as shown in fig. 2, in the fourth step, solvent gasoline is introduced into the hydrolysis reactor 101 at a temperature of 45 ± 5 ℃, wherein the solvent gasoline is 1500kg, and the mixture is stirred for 30 min.
Further, as shown in FIG. 2, in the sixth step, the standing time is 1h-1.2h, the cooling temperature is 5-10 ℃, and the centrifugal operation is kept for 1h-1.5 h.
Note that p-toluenesulfonyl chloride CH3C6H4SO2CL, has the formula:
NaCL
the production process of the tosyl chloride by the water phase method is researched for years, and through efforts, the clean production process by the water phase method is improved, mainly realizing zero discharge of sewage, absorbing waste gas by adopting a falling film method, adopting a hanging bag type full-closed centrifuge for centrifugation, independently separating each process unit, adopting top air suction negative pressure in a centrifuge room and the like. Greatly reduces the labor intensity, greatly improves the production environment and has no waste water discharge. On the basis, the production process is further researched and implemented by a new process of solvent method production, and the method has the advantages of being cleaner and more environment-friendly, and meanwhile, the product quality is greatly improved under the condition that the production cost is reduced.
The working process comprises the following steps:
the p-toluenesulfonyl chloride is produced through adding chlorosulfonic acid in 1.65 ton in 3000L reactor, dropping toluene in 510kg at 30-50 deg.c and negative pressure, heating to 70 deg.c for 4 hr, adding water in the hydrolysis reactor in 150kg at negative pressure, dropping gasoline in 1500kg at 45 +/-5 deg.c and stirring for 30min, standing for 1 hr for layering, adding water layer to the lower part, adding solvent layer to the crystallizing kettle, cooling to below 10 deg.c for crystallization, and centrifuging after 1 hr to obtain the product.
In the description of the present invention, it is to be understood that the terms "front-back", "left-right", and the like indicate orientations or positional relationships based on those shown in the drawings, and are only for convenience in describing the present invention and simplifying the description, but do not indicate or imply that the referred device or component must have a specific orientation, be constructed in a specific orientation, and be operated, and thus should not be construed as limiting the invention.
Of course, in this disclosure, those skilled in the art will understand that the terms "a" and "an" should be interpreted as "at least one" or "one or more," i.e., in one embodiment, a number of an element may be one, and in another embodiment, a number of the element may be plural, and the terms "a" and "an" should not be interpreted as limiting the number.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily made by those skilled in the art in light of the technical teaching of the present invention should be included within the scope of the present invention. Therefore, the protection scope of the present invention should be subject to the protection scope of the claims.
Claims (9)
1. A hydrolysis device for preparing paratoluensulfonyl chloride comprises a hydrolysis reaction kettle (101), and is characterized by also comprising a cleaning mechanism (2), an even water dripping mechanism (3), a stirring mechanism (4) and a gasoline transmission mechanism, wherein the cleaning mechanism, the even water dripping mechanism and the stirring mechanism are arranged in the hydrolysis reaction kettle (101) and are arranged along the vertical direction, and the gasoline transmission mechanism is arranged outside the hydrolysis reaction kettle (101) and is communicated with the hydrolysis reaction kettle (101);
the uniform water dripping mechanism (3) comprises a water container (31) arranged outside the hydrolysis reaction kettle (101), a first connecting pipe (32) with one end communicated with the water container (31) and the other end hermetically connected with the inside of the hydrolysis reaction kettle (101), a uniform water dripping component (33) arranged in the hydrolysis reaction kettle (101) and communicated with the first connecting pipe (32), a driving mechanism (34) driving the uniform water dripping component (33) to lift along the vertical direction and positioned outside the hydrolysis reaction kettle (101), and an intermittent component (35) synchronously driven by the driving mechanism (34) and controlling water in the water container (31) to drip intermittently, wherein the driving mechanism (34) is used for adjusting the temperature in the hydrolysis reaction kettle (101);
the stirring mechanism (4) comprises a stirring assembly (41) which is arranged on the inner wall of the hydrolysis reaction kettle (101) in a sliding manner, a first transmission assembly (42) which is driven by the driving mechanism (34) in a synchronous transmission manner and is used for driving the stirring assembly (41) to transmit along the vertical direction, and a driving assembly (43) which is used for driving the stirring assembly (41) to rotate circumferentially;
the cleaning mechanism (2) comprises a cleaning component (21) arranged at the upper end of the hydrolysis reaction kettle (101) and above the stirring mechanism (4), and a collecting component arranged outside the hydrolysis reaction kettle (101);
the gasoline transmission mechanism comprises an oil container and a second transmission assembly, wherein the oil container is respectively communicated with the hydrolysis reaction kettle (101) and the cleaning assembly (21), and the second transmission assembly is synchronously transmitted with the driving assembly (43) and is used for driving oil in the oil container to enter the hydrolysis reaction kettle (101);
the uniform water dripping component (33) comprises a hose (331) which is in sealed communication with the first connecting pipe (32), a second pressure limiting component (332) which is in sealed communication with the lower end of the hose (331), and a first pressure limiting component (333) and a third pressure limiting component (334) which are respectively positioned at two sides of the second pressure limiting component (332), wherein the first pressure limiting component (333), the second pressure limiting component (332) and the third pressure limiting component (334) are in elastic contact and sealed contact with the contact part of the inner wall of the hydrolysis reaction kettle (101), the first pressure limiting component (333) and the third pressure limiting component (334) respectively comprise a pressure limiting plate a (301) which is arranged on the inner wall of the hydrolysis reaction kettle (101) in a sliding manner and is arranged in a hollow structure, and the second pressure limiting component (332) comprises a pressure limiting plate b (302) which is hinged with the pressure limiting plate a (301) and is arranged in a hollow structure, The hydrolysis reaction kettle is characterized in that the pressure limiting plate b (302) is driven to rotate and is rotatably arranged on a driving shaft a (303) on the pressure limiting plate a (301), a first transmission gear (304) coaxial with and fixedly connected with the driving shaft a (303) and a first transmission rack (306) meshed with the first transmission gear (304) and vertically arranged in a groove a (305) on the inner wall of the hydrolysis reaction kettle (101), the first transmission rack (306) comprises a first one-way tooth part (30 a) and a second one-way tooth part (30 b) which are oppositely arranged in tooth, water outlet holes a (335) are uniformly formed in the lower end of the pressure limiting plate a (301), two ends of the pressure limiting plate b (302) are communicated with two groups of the pressure limiting plates a (301) and water outlet holes b (336) are uniformly formed in the lower ends of the pressure limiting plate a, and a limiting plate a (337) is vertically arranged on the first pressure limiting assembly (333), a limit plate b (338) is arranged at the upper end of the pressure limit plate b (302), the limit plate b (338) and a limit plate a (301) of the third pressure limit assembly (334) are in discontinuous lap joint, a limit plate c (339) is arranged at the lower end of the third pressure limit assembly (334), the limit plate c (339) and the lower end of the pressure limit plate b (302) are in discontinuous lap joint, and the outer circumference formed by the two groups of pressure limit plates a (301) and b (302) is matched with the inner wall of the hydrolysis reaction kettle (101);
the intermittent assembly (35) comprises a first linkage rack (351) which is fixedly connected with the telescopic end of the driving mechanism (34) and is vertically arranged, a first linkage gear (352) which is meshed with the first linkage rack (351), a fourth linkage bevel gear (357) which is meshed with the first linkage gear (352), a fifth linkage bevel gear (358) which is meshed with the fourth linkage bevel gear (357), a second linkage gear (353) which is synchronously driven with the fifth linkage bevel gear (358) and is arranged in a half-tooth structure, a second linkage rack (354) which is meshed with the second linkage gear (353) and is horizontally driven, a water baffle which is fixedly connected with the second linkage rack (354) and is arranged on the water container (31) in a sliding manner, and a telescopic spring a (356) one end of which is fixedly connected with the second linkage rack (354) and the other end of which is fixedly connected with the outer wall of the water container (31), the expansion spring a (356) is sleeved outside the second linkage rack (354).
2. The hydrolysis apparatus for p-toluenesulfonyl chloride preparation according to claim 1, wherein, the driving mechanisms (34) are arranged in two groups and are respectively connected with the first pressure limiting component (333) and the third pressure limiting component (334), which comprises a telescopic cylinder (341) with a telescopic end arranged vertically downwards and arranged outside a hydrolysis reaction kettle (101), a driving rod (342) fixedly connected with the telescopic end of the telescopic cylinder (341) and arranged vertically, a telescopic spring b (343) sleeved outside the driving rod (342) and a temperature control component (344) sleeved outside the hydrolysis reaction kettle (101), the driving rod (342) is fixedly connected with the upper end of the pressure limiting plate a (301), one end of the telescopic spring b (343) is fixedly connected with the inner wall of the hydrolysis reaction kettle (101) and the other end of the telescopic spring b (343) is fixedly connected with the upper end of the pressure limiting plate a (301);
the temperature control assembly (344) comprises a cover box (345) covered outside the telescopic cylinder (341), a heat control cavity (346) attached to the outer wall of the hydrolysis reaction kettle (101), a heat transfer pipe (347) with one end communicated with the inner wall of the cover box (345) and the other end communicated with the heat control cavity (346), and a third transmission assembly (348) for controlling the opening and closing of the cover box (345), wherein the third transmission assembly (348) comprises a starting valve (3481) for controlling the opening and closing of the opening, a third linkage gear (3482) coaxial and synchronously driven with the starting valve (3481), a linkage rod (3483) vertically connected with the telescopic end of the telescopic cylinder (341), a third linkage rack (3484) arranged at the upper end of the linkage rod (3483) and having a one-way tooth structure, and a fourth linkage rack (3485) arranged at the upper end of the linkage rod (3483) and having a one-way tooth structure, the third linkage rack (3484) and the fourth linkage rack (3485) are both meshed with the third linkage gear (3482) and have opposite unidirectional transmission directions.
3. The hydrolysis apparatus for p-toluenesulfonyl chloride preparation according to claim 2, characterized in that, the stirring assembly (41) comprises a sliding block a (412) which is arranged in a groove b (411) of the inner wall of the hydrolysis reaction kettle (101) in a sliding way and a stirring shaft (413) which is arranged on the sliding block a (412) in a rotating way, the sliding block a (412) is arranged in a magnetic structure, two ends of the pressure limiting plate b (302) are provided with stop blocks (414), the stop block (414) is positioned in the pressure limiting plate b (302), a distance sensor is arranged on the pressure limiting plate c (339), when the limit plate c (339) is contacted with the limit plate b (302), the stop block (414) is ejected outwards to be matched into the groove b (411), when the limiting plate c (339) is not in contact with the limiting plate b (302), the stop block (414) is reset inwards to enter the limiting plate b (302);
the first transmission assembly (42) comprises a second transmission rack (421) which is fixedly connected with the telescopic end of any telescopic cylinder (341) and is vertically arranged, a second transmission gear (422) which is meshed with the second transmission rack (421), a third transmission rack (423) which is meshed with the second transmission gear (422) and is arranged opposite to teeth of the second transmission rack (421), a sliding block b (424) of which the upper end is fixedly connected with the lower end of the third transmission rack (423), and a telescopic unit b (425) of which the upper end is fixedly connected with the sliding block b (424) and the lower end is fixedly connected with a support frame (426), the sliding block b (424) and the sliding block a (412) are arranged in a one-to-one correspondence manner and are arranged in a magnetic attraction manner, and the support frame (426) is sleeved on the outer wall of the hydrolysis reaction kettle (101);
drive assembly (43) includes driving motor (431), driving motor (431) are located hydrolysis reaction cauldron (101) are outer and its rotation end is located hydrolysis reaction cauldron (101) are interior, driving motor (431) rotate the end and be provided with elastic ring (432), be provided with breach (433) and this breach (433) bore is less than on elastic ring (432) the transmission end diameter of (mixing) shaft (413).
4. The hydrolysis apparatus for p-toluenesulfonyl chloride preparation according to claim 3, wherein, the cleaning component (21) comprises a second connecting pipe (211) arranged in the hydrolysis reaction kettle (101), a spraying arc plate (212) which is communicated with the second connecting pipe (211) and two ends of which are fixedly arranged on the inner wall of the hydrolysis reaction kettle (101), and a limiting arc plate (214) which is jointed with the lower surface of the spraying arc plate (212) and is rotationally arranged on the hydrolysis reaction kettle (101) through a disc (213), a third transmission gear (215) and a fourth transmission rack (216) which is meshed with the third transmission gear (215) and is fixedly connected with the upper end of the sliding block a (412) are arranged on the circular disc (213), the spraying arc plate (212) is arranged in an eighth structure, and the limiting arc plate (214) is arranged in a half structure;
the collecting assembly comprises a discharge hole formed in the hydrolysis reaction kettle (101), a valve for controlling the opening and closing of the discharge hole, a discharge pipe communicated with the discharge hole and arranged obliquely downwards, and a containing container positioned at the output end of the discharge pipe;
the second transmission assembly include with the coaxial and fixed connection's of driving motor (431) output first awl tooth, with second awl tooth that first awl tooth meshing set up, with third connecting pipe, the setting that oil container intercommunication set up are in control flap, one end on the third connecting pipe with third connecting pipe intercommunication set up and the other end with fourth communicating pipe and one end that hydrolysis reaction cauldron (101) in-connection set up with third connecting pipe intercommunication set up and the other end with the fifth communicating pipe that second connecting pipe (211) intercommunication set up, fourth communicating pipe with the bore of fifth communicating pipe sets up according to the proportion, the second awl tooth passes through hold-in range synchronous drive control flap's on-off work.
5. A p-toluenesulfonyl chloride processing process based on a hydrolysis device for preparing p-toluenesulfonyl chloride described in claims 1 to 4, comprising:
step one, tosyl chloride production, namely manually selecting a plurality of components of chlorosulfonic acid, adding the chlorosulfonic acid into a 3000L reaction kettle (102), dropwise adding a plurality of components of toluene into the 3000L reaction kettle (102) again under negative pressure in an environment of 30-50 ℃, heating and preserving heat after dropwise adding is finished;
step two, hydrolysis reaction, namely adding the mixture in the reaction kettle (102) in the step one into a hydrolysis reaction kettle (101), and starting a driving mechanism (34) to drip water under the condition of negative pressure;
step three, adjusting the reaction temperature, and synchronously with the step two, driving the first pressure limiting assembly (333) and the third pressure limiting assembly (334) to respectively drive the driving mechanism (34) to move downwards, completing the water dripping work and synchronously pressurizing the reaction space, meanwhile, hot air generated by the driving mechanism (34) is introduced to the outer wall of the hydrolysis reaction kettle (101) to conduct the temperature heat conduction work in the hydrolysis reaction kettle (101), so that the temperature reduction speed in the hydrolysis reaction kettle (101) is slowed down in the hydrolysis reaction;
step four, carrying out dissolution reaction, wherein after water is dropwise added for a period of time, the driving mechanism (34) drives the stirring assembly (41) to descend through the first transmission assembly (42) until the stirring assembly descends to the driving assembly (43), the driving assembly (43) drives the stirring assembly (41) to rotate, stirring work is completed, and then the driving assembly (43) synchronously drives the second transmission assembly to introduce solvent gasoline in the oil container into the hydrolysis reaction kettle (101);
step five, self-cleaning, wherein in the lifting process of the stirring assembly (41), the cleaning assembly (21) finishes the cleaning work of the stirring shaft (413) of the stirring assembly (41), meanwhile, the solvent gasoline and residues on the stirring shaft (413) are washed away together and enter the limiting arc plate (214) of the stirring assembly (41) below for collection, when a distance sensor on a discharge port on the hydrolysis reaction kettle (101) senses the dropped washed object, a valve is opened, and the solvent gasoline automatically falls to the discharge port along the limiting arc plate (214) which is inclined downwards and is output;
and step six, standing for separation, automatically layering after standing, putting a lower water layer into a wastewater storage tank (103), adding a solvent layer into a crystallization kettle (104) for cooling crystallization, and keeping centrifugation after crystallization to obtain a finished product.
6. The process of claim 5, wherein chlorosulfonic acid is present in an amount of 1.65 tons and toluene is present in an amount of 510 kg.
7. The process of claim 5, wherein in the second step, 150kg of water is selected and added dropwise at a temperature below 50 ℃.
8. The processing technology of paratoluensulfonyl chloride as claimed in claim 5, wherein in the fourth step, the solvent gasoline is introduced into the hydrolysis reaction kettle (101) at a temperature of 45 ± 5 ℃, the solvent gasoline is 1500kg, and the mixture is stirred for 30 min.
9. The process for processing p-toluenesulfonyl chloride according to claim 5, wherein in step six, the standing time is 1h to 1.2h, the cooling temperature is 5 ℃ to 10 ℃, and the centrifugal operation is maintained for 1h to 1.5 h.
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| CN1824649A (en) * | 2006-02-22 | 2006-08-30 | 江苏康祥集团公司 | Production technology of phenyl sulfuryl chloride |
| WO2009099218A1 (en) * | 2008-02-08 | 2009-08-13 | Kanagawa Academy Of Science And Technology | Method of hydrolyzing polysaccharide and stirring apparatus therefor |
| CN107383100A (en) * | 2017-08-10 | 2017-11-24 | 林培鹏 | A kind of tenofovir production line |
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| CN1824649A (en) * | 2006-02-22 | 2006-08-30 | 江苏康祥集团公司 | Production technology of phenyl sulfuryl chloride |
| WO2009099218A1 (en) * | 2008-02-08 | 2009-08-13 | Kanagawa Academy Of Science And Technology | Method of hydrolyzing polysaccharide and stirring apparatus therefor |
| CN107383100A (en) * | 2017-08-10 | 2017-11-24 | 林培鹏 | A kind of tenofovir production line |
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