CN114345283B - High-purity sodium cyclamate production process and production device thereof - Google Patents
High-purity sodium cyclamate production process and production device thereof Download PDFInfo
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- CN114345283B CN114345283B CN202210066712.8A CN202210066712A CN114345283B CN 114345283 B CN114345283 B CN 114345283B CN 202210066712 A CN202210066712 A CN 202210066712A CN 114345283 B CN114345283 B CN 114345283B
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
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- 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
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
- B01J2219/00121—Controlling the temperature by direct heating or cooling
- B01J2219/00123—Controlling the temperature by direct heating or cooling adding a temperature modifying medium to the reactants
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The invention belongs to the technical field of sodium cyclamate synthesis and discloses a high-purity sodium cyclamate production device which comprises a reaction kettle, wherein a reaction cavity for substance reaction precipitation is arranged in the reaction kettle, a top cover is movably arranged at the opening end of the reaction cavity, the reaction cavity is in a sealing state under the action of the reaction kettle and the top cover, a stirring assembly is arranged in the reaction cavity, the stirring assembly comprises a continuous carrying column, and a cooling assembly is connected to the continuous carrying column.
Description
Technical Field
The invention belongs to the technical field of sodium cyclamate synthesis, and particularly relates to a high-purity sodium cyclamate production process and a production device thereof.
Background
Sodium cyclamate with chemical name of sodium cyclamate and molecular formula of C 6 H 12 NO 3 SNa, a white crystalline or powdered solid, is a non-nutritive high sweetness synthetic sweetener. Has sweet taste similar to granulated sugar and good fruit flavor, has sweetness 50-60 times that of white sugar, is easy to dissolve in water, and has stable chemical property.
Patent application number CN202110772083.6 discloses a sodium cyclamate production process and device, and production of sodium cyclamate and recovery of cyclohexylamine are realized through a plurality of devices, but in the sodium cyclamate reaction process, adjustment cannot be made on the reaction environment, so that the condition of changing the precipitation rate in the reaction process occurs.
The synthesis of sodium cyclamate at home and abroad generally adopts cyclohexane and sulfamic acid as raw materials, and the synthesis is carried out under normal pressure. However, before the reaction is finished, the product can be solidified and separated out to generate coking, so that the reaction is affected, and the yield is reduced. Excessive cyclohexylamine is adopted as a solvent in China, but the reaction speed is greatly slowed down due to the fact that the cyclohexylamine is excessively introduced, the yield cannot be improved, and the synthesis of sodium cyclamate by a pressurizing method is studied, and the coking of the solution is difficult to control by the pressure of the method, and the cost is high.
Disclosure of Invention
The invention aims at solving the problems, and provides a high-purity sodium cyclamate production process and a high-purity sodium cyclamate production device, which have the advantage of controlling the precipitation rate and purity of sodium cyclamate through the temperature and pressure in a reaction kettle.
In order to achieve the above purpose, the present invention provides the following technical solutions: the high-purity sodium cyclamate production device comprises a reaction kettle, wherein a reaction cavity for substance reaction precipitation is arranged in the reaction kettle, a top cover is movably arranged at the opening end of the reaction cavity, the reaction cavity is in a sealing state under the action of the reaction kettle and the top cover, a stirring assembly is arranged in the reaction cavity, the stirring assembly comprises a continuous loading column, and a cooling assembly is connected to the continuous loading column;
the cooling assembly comprises a cooling support column, the cooling support column rotates along with the continuous carrying column, the cooling support column can slide along the length direction of the continuous carrying column, a cavity for cooling gas to pass through is formed in the cooling support column, and a cooling hole is formed in the cooling support column and is communicated with the cavity for cooling gas to pass through;
a temperature control telescopic block is fixedly arranged on the inner wall of the reaction cavity, and one end of the loading column, which is far away from the top cover, is rotationally connected to the temperature control telescopic block;
the top cover is connected with a liquid inlet assembly, the liquid inlet assembly comprises a sliding liquid inlet block, and the sliding liquid inlet block is connected to the outer circumference of the cooling support column in a sliding manner through a controller;
when the temperature control telescopic block is in a contracted state, the cooling assembly is in an unoperated state, the sliding speed of the sliding liquid inlet block on the liquid inlet assembly is stable, the stirring speed of the stirring assembly is constant, when the temperature control telescopic block is in an elongated state after the temperature is increased, the continuous loading column slides towards one end close to the top cover, cooling gas of the cooling assembly cools solution in the reaction cavity through the cooling hole, and meanwhile, the feeding speed of the reaction solution is reduced by the controller, so that the stirring speed of the stirring assembly is accelerated.
A high-purity sodium cyclamate production process comprises the following steps:
s1: enabling the dried carbon tetrachloride and cyclohexylamine to enter a reaction cavity of a reaction kettle;
s2: the reaction cavity of the reaction kettle is sealed, and the temperature in the reaction cavity is regulated and controlled to be lower than 5 ℃;
s3: placing proper amount of chlorosulfonic acid at a feed port to enable the chlorosulfonic acid to enter the reaction kettle at a uniform speed;
s4: then alkalizing, regulating pH, extracting, evaporating solvent, crystallizing and drying to obtain the product sodium cyclamate.
Compared with the prior art, the invention has the following beneficial effects:
1. the cooling support column is internally provided with a groove capable of sliding along the length direction of the continuous loading column, so that the cooling support column can rotate along with the continuous loading column, relative sliding between the continuous loading column and the cooling support column is not influenced, a chamber for cooling gas to pass through is arranged on the cooling support column, one end of the chamber can be communicated with external cooling gas, a cooling hole penetrating through the cooling support column is arranged on the chamber, external cooling gas is discharged through the cooling hole after entering the chamber, and the temperature in the reaction chamber is cooled, so that the precipitation rate of sodium cyclamate is ensured not to be influenced.
2. Through the feed liquor subassembly that sets up to take out appropriate amount of reaction solution and place in the slip feed liquor piece, slip feed liquor piece can carry out periodic reciprocating slip on the outer circumference of cooling support column, simultaneously the reaction time of the reaction solution of placing in the slip feed liquor piece, with slip feed liquor piece slip time and fluid replacement time sum the same, thereby make the solution in the slip feed liquor piece fully react, can not appear the unable timely replenishment of reaction solution yet, lead to the condition emergence that the precipitation rate slows down.
3. Through the flexible piece of control by temperature change that sets up, and then realize the control to solution temperature to through utilizing the expansion with heat and contraction principle of flexible piece of control by temperature change, make solution temperature rise back, the high length of flexible piece of control by temperature change, thereby drive the flexible piece of control by temperature change is prolonged, drives and carries the post to remove, makes the cooling hole open, reduces the solution temperature in the reaction chamber, ensures precipitation rate and the purity stability of sodium cyclamate.
4. When the continuous loading column ascends under the action of the temperature control telescopic block, relative sliding occurs between the cooling support column and the continuous loading column, the spoiler connected to the cooling support column is rotated out of the cooling support column, and meanwhile the continuous loading column drives the cooling support column to rotate under the action of the motor, so that the stirring rate of the solution is accelerated, cooling gas sprayed out of the cooling hole can be quickly contacted with the reaction solution in the reaction cavity, and the temperature dropping rate is improved.
Drawings
FIG. 1 is a schematic diagram of the main structure of a high purity sodium cyclamate production apparatus of the present invention;
FIG. 2 is a schematic view of a main structure of another direction of the present invention;
FIG. 3 is a schematic cross-sectional view of the body structure of FIG. 2;
FIG. 4 is a schematic view of the structure of the stirring assembly of the present invention;
FIG. 5 is an enlarged schematic view of the structure of FIG. 3A;
fig. 6 is a schematic structural diagram of embodiment 3 of the present invention.
Description of the drawings: 1. a reaction kettle; 11. a discharge port; 12. a reaction chamber; 2. a top cover; 21. a pressure control valve; 3. a flow blocking bar; 4. a stirring assembly; 41. a loading column; 42. a main stirring rod; 43. an auxiliary stirring rod; 44. a swing column; 5. a liquid inlet component; 51. a liquid inlet hole; 52. a raw material storage box; 53. sliding the liquid inlet block; 6. a cooling assembly; 61. cooling the support column; 62. a cooling hole; 63. an air inlet pipe; 71. a spoiler; 8. temperature control telescopic block.
Description of the embodiments
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Examples
The invention also provides a production process of the high-purity sodium cyclamate, which comprises the following detailed operation steps:
s1: enabling the dried carbon tetrachloride and cyclohexylamine to enter a reaction cavity of a reaction kettle;
s2: the reaction cavity of the reaction kettle is sealed, and the temperature in the reaction cavity is regulated and controlled to be lower than 5 ℃;
s3: placing proper amount of chlorosulfonic acid at a feed port to enable the chlorosulfonic acid to enter the reaction kettle at a uniform speed;
s301, controlling the pressure in the feeding port to be constant, so that chlorosulfonic acid uniformly enters the reaction kettle and fully reacts;
s302, stirring the solution through a stirrer in the chlorosulfonic acid reaction process to fully precipitate sodium cyclamate;
s303, controlling the temperature and the pressure in the reaction kettle to be stable in an interval, and ensuring the stable yield and purity of sodium cyclamate;
s4: then alkalizing, regulating pH, extracting, evaporating solvent, crystallizing and drying to obtain the product sodium cyclamate.
Examples
As shown in fig. 1-5, a high-purity sodium cyclamate production device comprises a reaction kettle 1, a reaction cavity 12 for substance reaction precipitation is arranged in the reaction kettle 1, a top cover 2 is movably arranged at the opening end of the reaction cavity 12, the reaction cavity 12 is in a sealing state under the action of the reaction kettle 1 and the top cover 2, and further, the temperature and pressure maintaining interval in the reaction cavity 12 are kept constant during the operation of the reaction cavity 12, so that the precipitation rate and concentration of sodium cyclamate are ensured to be the same, a stirring assembly 4 is arranged in the reaction cavity 12, the stirring assembly 4 can stir a solution in the reaction cavity 12 during the reaction, the stirring assembly 4 comprises a continuous loading column 41, one end of the continuous loading column 41 is positioned in the reaction cavity 12, the other end of the continuous loading column 41 penetrates through the top cover 2, a power source of the continuous loading column 41 is provided by a servo motor, a cooling assembly 6 is connected to the continuous loading column 41, and the cooling assembly 6 can cool the liquid temperature of the solution, and thus the normal precipitation of sodium cyclamate is ensured.
The cooling assembly 6 comprises a cooling support column 61, the cooling support column 61 rotates along with the continuous loading column 41, the cooling support column 61 can slide along the length direction of the continuous loading column 41, a cavity for cooling gas to pass through is formed in the cooling support column 61, the cooling gas is preferably nitrogen, a cooling hole 62 is formed in the cooling support column 61, and the cooling hole 62 is communicated with the cavity for cooling gas to pass through; while the position of the cooling support column 61 within the reaction chamber 12 is not shifted.
The cooling support column 61 is inboard along carrying post 41 length direction to be equipped with the gliding groove, and then make cooling support column 61 can rotate along with carrying post 41, do not influence simultaneously and carry the relative slip between post 41 and the cooling support column 61, set up the cavity that cooling gas passed through simultaneously on cooling support column 61, the one end of cavity can with outside cooling gas intercommunication to be equipped with the cooling hole 62 that runs through cooling support column 61 on the cavity, make outside cooling gas get into after the cavity, discharge through cooling hole 62, and then cool off the temperature in the reaction chamber 12, ensure that the precipitation rate of sodium cyclamate can not be influenced.
It should be noted that, when no relative sliding occurs between the connection post 41 and the cooling support post 61, the cooling hole 62 is not communicated with the cooling cavity, and the cooling gas does not enter the cooling cavity, which is a conventional closing technique, and thus will not be described in detail here.
The inner wall of the reaction cavity 12 is fixedly provided with a temperature control telescopic block 8, and one end of the continuous loading column 41 far away from the top cover 2 is rotationally connected to the temperature control telescopic block 8.
Through the flexible piece 8 of control by temperature change that sets up, and then realize the control to solution temperature to through utilizing the expansion with heat and contraction principle of flexible piece 8 of control by temperature change, make solution temperature rise back, the height of flexible piece 8 of control by temperature change becomes long, thereby drive flexible piece 8 of control by temperature change grow, drive and link post 41 and remove, make cooling hole 62 open, carry out the temperature reduction to the solution in the reaction chamber 12, ensure the precipitation rate and the purity stability of sodium cyclamate.
The top cover 2 is connected with a liquid inlet assembly 5, the liquid inlet assembly 5 comprises a sliding liquid inlet block 53, and the sliding liquid inlet block 53 is connected to the outer circumference of the cooling support column 61 in a sliding manner through a controller.
Through the liquid inlet component 5, a proper amount of reaction solution is taken out and placed in the sliding liquid inlet block 53, and then the solution to be reacted is directly fed into the deep part of the solution in the reaction cavity 12 through the sliding liquid inlet block 53, so that the condition that the reaction rate is slow and the reaction is insufficient due to the fact that the reaction solution takes on a round water drop shape in the process of dripping and then only reacts with the surface of the water drop is avoided; the sliding liquid inlet block 53 can periodically and reciprocally slide on the outer circumference of the cooling support column 61, and meanwhile, the reaction time of the reaction solution placed in the sliding liquid inlet block 53 is the same as the sum of the sliding time and the liquid supplementing time of the sliding liquid inlet block 53, so that the solution in the sliding liquid inlet block 53 fully reacts, and the situation that the reaction solution cannot be timely supplemented, and the precipitation rate is slow is avoided.
The controller can adjust the sliding rate of the sliding liquid inlet block 53 on the cooling support column 61 through the state of the temperature control telescopic block 8, when the temperature control telescopic block 8 is in a contracted state, the liquid inlet feeding rate of the sliding liquid inlet block 53 is stable and constant, and when the temperature control telescopic block 8 is in an extended state, the liquid inlet feeding rate of the sliding liquid inlet block 53 is reduced.
When the temperature control telescopic block 8 is in a contracted state, the cooling assembly 6 is in an unoperated state, the sliding speed of the sliding liquid inlet block 53 on the liquid inlet assembly 5 is stable, namely, the liquid inlet speed in the reaction cavity 12 is stable, the stirring speed of the stirring assembly 4 is constant, when the temperature control telescopic block 8 is in an extended state under the influence of temperature, the relative position between the continuous column 41 and the cooling assembly 6 moves, the cooling gas of the cooling assembly 6 cools the solution in the reaction cavity 12 through the cooling hole 62, and meanwhile, the sliding liquid inlet block 53 is controlled by a controller to reduce the feeding speed of the reaction solution, and meanwhile, the stirring speed of the stirring assembly 4 is accelerated, so that the feeding amount of the reaction solution can be fully reacted when the temperature rises.
Advantageously, the cooling support column 61 is provided with a spoiler 71 for rapid cooling of the solution by rotating the side away from the top cover 2, and when not in operation, the spoiler 71 is accommodated on the cooling support column 61, and does not stir the solution in the reaction chamber 12.
When the carrying column 41 ascends under the action of the temperature control telescopic block 8, the cooling support column 61 and the carrying column 41 slide relatively in position, at the moment, the spoiler 71 connected to the cooling support column 61 rotates out of the cooling support column 61, and meanwhile, the carrying column 41 drives the cooling support column 61 to rotate under the action of the motor, so that the stirring rate of the solution is accelerated, the cooling gas sprayed out of the cooling hole 62 can be quickly contacted with the reaction solution in the reaction cavity 12, and the temperature dropping rate is increased.
Advantageously, the stirring assembly 4 further comprises a main stirring rod 42 and an auxiliary stirring rod 43, one side of the continuous loading column 41 away from the opening end of the reaction cavity 12 is fixedly provided with a plurality of main stirring rods 42, and one end of the main stirring rod 42 away from the continuous loading column 41 is rotatably provided with the auxiliary stirring rod 43.
Through foretell technical scheme, and then make stirring assembly 4 in the in-process of stirring, can stir the reaction chamber 12 in a large scale of solution through main stirring rod 42 to rotate through vice stirring rod 43 and connect on main stirring rod 42, thereby when main stirring rod 42 in the rotation in-process, through the resistance that produces between vice stirring rod 43 and the solution, thereby drive vice stirring rod 43 and take place to rotate, and then carry out irregular stirring to the solution in the reaction chamber 12, thereby make the solution in the in-process of reaction, can separate out the reaction with faster speed, reduce the time loss in the reaction process.
Advantageously, the cooling assembly 6 further comprises an air inlet duct 63, one end of which duct 63 communicates with the cooled chamber and the other end extends through the top cover 2 and outside the reaction chamber 12.
The air inlet pipe 63 is connected to the cooling support column 61 for being used as a source of cooling gas, and the top cover 2 is observed through the air inlet pipe 63, so that the tightness of the reaction chamber 12 is not affected, and one end of the air inlet pipe 63 extending to the outside of the reaction chamber 12 is communicated with a storage box of the cooling gas.
Advantageously, the liquid inlet assembly 5 further comprises a raw material storage box 52, the raw material storage box 52 is fixedly connected to one end of the top cover 2 far away from the reaction cavity 12, the top cover 2 is provided with a liquid inlet hole 51 in a penetrating manner, and raw materials in the raw material storage box 52 can enter the sliding liquid inlet block 53 through the liquid inlet hole 51.
Through the above technical scheme, place the raw materials case 52 in the outside of reation kettle 1, conveniently observe the raw materials surplus in the case 52 is deposited to the raw materials, also conveniently supply the raw materials in the case 52 to through set up the feed liquor hole 51 that runs through on top cap 2, make the raw materials in the case 52 can be through feed liquor hole 51 with the raw materials removal to slip feed liquor piece 53 in.
When the sliding liquid inlet block 53 is close to the top cover 2, the raw material storage box 52 can only enter the stored reaction raw materials into the sliding liquid inlet block 53 through the liquid inlet hole 51, and when the sliding liquid inlet block 53 slides on the continuous loading column 41, the liquid discharge port on the raw material storage box 52 is in a closed state.
Advantageously, an air pressure punch for breaking up and fusing the reaction solution is provided in the slide feed block 53.
When the sliding liquid inlet block 53 moves to the end of the cooling support column 61 away from the top cover 2, the reaction raw material is blown out of the sliding liquid inlet block 53 by the pneumatic punch installed in the sliding liquid inlet block 53, and the reaction raw material is powdered under the impact of the pneumatic punch, so that the reaction can be fully performed by fully contacting with the solution in the reaction chamber 12.
Advantageously, the inner wall of the reaction chamber 12 is provided with a flow-blocking strip 3 for turbulence of the solution in the reaction chamber 12.
Through the above technical scheme, the solution in the reaction chamber 12 is not regularly rotated, so that the raw materials which are not reacted or are not reacted completely are contacted with the reaction solution through the oscillating solution, and the reaction is sufficient.
Advantageously, the top cover 2 is connected to a pressure control valve 21 for regulating the pressure in the reaction chamber 12.
Through the above technical scheme, when the pressure in the reaction chamber 12 changes due to factors such as temperature rise or cooling gas injection, the pressure in the reaction chamber 12 is stably regulated through the pressure control valve 21, so that the precipitation rate of sodium cyclamate in the reaction chamber 12 is ensured to be stable, and the influence of the change of the pressure on the purity of sodium cyclamate is avoided.
Advantageously, one end of the reaction kettle 1 far away from the top cover 2 is provided with a discharge hole 11 in a penetrating way. After the reaction of sodium cyclamate in reaction chamber 12 is accomplished, can take out sodium cyclamate in reation kettle 1 through the discharge gate 11 that reation kettle 1 set up, simultaneously through setting up the one end that top cap 2 was kept away from to reation kettle 1 with discharge gate 11 to when taking out sodium cyclamate, there is not the remaining condition of raw materials in reation kettle 1, and then can not produce the influence to reation kettle 1 subsequent use.
The working process of the device is as follows:
when the temperature is constant, the continuous loading column 41 drives the main stirring rod 42 to rotate, so as to drive the solution in the reaction cavity 12 to rotate, the continuous loading column 41 and the cooling support column 61 do not slide relatively in position, the temperature control telescopic block 8 is in an initial shrinkage state, the cooling hole 62 is not opened, the spoiler 71 is not unfolded, and the liquid feeding rate of the liquid feeding assembly 5 maintains normal liquid feeding and supplementing.
The solution to be reacted is placed in the sliding liquid inlet block 53 through the raw material storage box 52 and the liquid inlet, thereby the solution to be reacted is directly sent into the reaction cavity 12 through the sliding liquid inlet block 53 and is blown out in a powdery state through the pneumatic punch, the reaction solution is enabled to fully react in a shorter time, at this time, the reaction temperature is enabled to rise through the reaction of the reaction solution, the precipitation rate of the reaction solution to sodium cyclamate is enabled to be slowed down, simultaneously after the temperature is raised, the temperature-controlled telescopic block 8 is heated and expanded to be elongated, thereby the continuous carrying column 41 and the cooling support column 61 are driven to slide relatively, so that cooling gas is injected into the cooling support column 61 through the air inlet pipe 63, and enters the reaction cavity 12 through the cooling hole 62 to be fused with the solution, and the spoiler 71 is unfolded after the continuous carrying column 41 moves, along with the continuous carrying column 41 and the main stirring rod 42, at this time, the temperature-controlled telescopic block 8 is enabled to allocate the controller, the liquid inlet rate of the reaction solution is enabled to be slowed down, the reaction solution supply quantity is enabled to be reduced, the reaction solution is enabled to be cooled down, the temperature is enabled to be increased, the temperature of the reaction solution is enabled to be cooled down stably, the temperature is enabled to be cooled down, the temperature is enabled to be stably and the temperature is enabled to be cooled down, and the temperature is enabled to be stably and the temperature is enabled to be cooled.
In order to facilitate the control of the liquid inlet rate of the cooling assembly 6 and the liquid inlet assembly 5, the extension condition of the temperature-controlled telescopic block 8 is set to three states:
1. when the temperature is 3-3 ℃ below zero, the temperature control telescopic block 8 is in an unextended state, the cooling component 6 does not start to work, and the liquid inlet rate of the liquid inlet component 5 is stable.
2. When the temperature is greater than 3 ℃ and less than 10 ℃, the temperature control telescopic block 8 is stretched by one third of the original length, the cooling holes 62 on the cooling assembly 6 are in a semi-open state, the spoiler 71 is in a semi-open state, and the liquid inlet rate of the liquid inlet assembly 5 is slowed down.
3. When the temperature is greater than or equal to 10 ℃, the temperature control telescopic block 8 is in the longest state, the cooling holes 62 on the cooling assembly 6 are in the all-open state, the cooling gas runs in full power, the spoiler 71 is in the full-open state, the liquid inlet rate of the liquid inlet assembly 5 is further slowed down, and the stirring rate of the stirring assembly 4 is increased.
When the pressure in the reaction chamber 12 is high due to the rise of cooling gas or temperature, the pressure in the reaction chamber 12 is regulated by the pressure control valve 21, so that the pressure can be stabilized in the reaction process, and the precipitation rate and concentration of sodium cyclamate are ensured not to be influenced.
Examples
As shown in fig. 6, based on the above-described example 2, the following modifications were made to solve the problem that the phenomenon of crystal precipitation easily occurs during precipitation of sodium cyclamate, affecting the stirring rate of the solution by the stirring member 4.
The main stirring rod 42 and the continuous loading column 41 are connected and provided with the swinging column 44, one end of the swinging column 44, which is close to the continuous loading column 41, is movably connected to the continuous loading column 41, so that when crystals of sodium cyclamate are precipitated, in order to avoid accumulation of crystals in the reaction kettle 1, the conditions that the sodium cyclamate is unsmooth in taking out are caused, when a solution in the reaction kettle 1 reacts for a period of time, the stirring state of the main stirring rod 42 is adjusted, the swinging state of the main stirring rod 42 is controlled through the swinging column 44, so that the main stirring rod 42 can lift the precipitated sodium cyclamate crystals, and at the moment, the main stirring rod 42 continuously rotates along with the continuous loading column 41, and after the precipitation reaction of sodium cyclamate is completed, the taking out of the subsequent sodium cyclamate is not influenced.
When the temperature control telescopic block 8 is in the first stage shrinkage state, the precipitation rate of sodium cyclamate in the reaction kettle 1 is the fastest, the phenomenon of sodium cyclamate crystal precipitation is easy to cause, and the main stirring rod 42 is subjected to the fastest swinging stirring through the swinging column 44, so that the sodium cyclamate crystal precipitation coking is avoided.
When the temperature control telescopic block 8 is in the second stage semi-extension state, at this time, the precipitation rate of sodium cyclamate in the reaction kettle 1 is reduced, the phenomenon of sodium cyclamate crystal precipitation is easier to be caused, and at this time, the rate of oscillating stirring the main stirring rod 42 by the oscillating column 44 is reduced.
When the temperature control telescopic block 8 is in the third stage full extension state, at this time, the precipitation rate of sodium cyclamate in the reaction kettle 1 is the slowest, the phenomenon of sodium cyclamate crystal precipitation is not easy to be caused, and at this time, the swing column 44 stops the swing stirring of the main stirring rod 42.
In the swinging process of the swinging column 44, uniform speed swinging of the swinging column 44 is realized through a cam structure, so that stirring of sodium cyclamate is realized, and meanwhile, the fluctuation influence on the reaction solution in the reaction kettle 1 is avoided.
It is noted that relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (8)
1. A production process of high-purity sodium cyclamate is characterized by comprising the following steps of: the method comprises the following steps:
s1, enabling dried carbon tetrachloride and cyclohexylamine to enter a reaction cavity of a reaction kettle;
s2, sealing a reaction cavity of the reaction kettle, and regulating and controlling the temperature in the reaction cavity to be lower than 5 ℃;
s3, a proper amount of chlorosulfonic acid is placed at a feed port, so that the chlorosulfonic acid can enter the reaction kettle at a uniform speed;
s301, controlling the pressure in the feeding port to be constant, so that chlorosulfonic acid uniformly enters the reaction kettle and fully reacts;
s302, stirring the solution through a stirrer in the chlorosulfonic acid reaction process to fully precipitate sodium cyclamate;
s303, controlling the temperature and the pressure in the reaction kettle to be stable in an interval, and ensuring the stable yield and purity of sodium cyclamate;
s4, alkalizing, regulating pH, extracting, evaporating a solvent, crystallizing and drying to obtain the sodium cyclamate;
the high-purity sodium cyclamate production device comprises a reaction kettle, wherein a reaction cavity for separating out substances by reaction is arranged in the reaction kettle, a top cover is movably arranged at the opening end of the reaction cavity, the reaction cavity is in a sealing state under the action of the reaction kettle and the top cover, a stirring assembly is arranged in the reaction cavity, the stirring assembly comprises a continuous loading column, and a cooling assembly is connected to the continuous loading column;
the cooling assembly comprises a cooling support column, the cooling support column rotates along with the continuous carrying column, the cooling support column can slide along the length direction of the continuous carrying column, a chamber for cooling gas to pass through is formed in the cooling support column, and a cooling hole is formed in the cooling support column and is communicated with the chamber for cooling gas to pass through;
a temperature control telescopic block is fixedly arranged on the inner wall of the reaction cavity, and one end of the loading column, which is far away from the top cover, is rotationally connected to the temperature control telescopic block;
the top cover is connected with a liquid inlet component, the liquid inlet component comprises a sliding liquid inlet block, the sliding liquid inlet block is connected to the outer circumference of the cooling support column in a sliding manner, and a controller is arranged on the sliding liquid inlet block;
when the temperature control telescopic block is in a contracted state, the cooling assembly is in an unoperated state, the sliding speed of the sliding liquid inlet block on the liquid inlet assembly is stable, the stirring speed of the stirring assembly is constant, when the temperature control telescopic block is in an elongated state after the temperature is increased, the continuous loading column slides towards one end close to the top cover, cooling gas of the cooling assembly cools solution in the reaction cavity through the cooling hole, and meanwhile, the feeding speed of the reaction solution is reduced by the controller, so that the stirring speed of the stirring assembly is accelerated.
2. The process for producing high purity sodium cyclamate of claim 1 wherein: and a spoiler is rotatably arranged on one side of the cooling support column away from the top cover.
3. The process for producing high purity sodium cyclamate of claim 2 wherein: the stirring assembly further comprises a main stirring rod and an auxiliary stirring rod, one side, away from the opening end of the reaction cavity, of the continuous loading column is fixedly provided with a plurality of main stirring rods, and one end, away from the continuous loading column, of the main stirring rod is rotatably provided with the auxiliary stirring rod.
4. The process for producing high purity sodium cyclamate of claim 1 wherein: the cooling assembly further comprises an air inlet pipe, one end of the air inlet pipe is communicated with the cooled cavity, and the other end of the air inlet pipe penetrates through the top cover and extends to the outside of the reaction cavity.
5. The process for producing high purity sodium cyclamate of claim 1 wherein: the feed liquor subassembly still includes the raw materials and deposits the case, raw materials are deposited case fixed connection the top cap is kept away from on the one end of reaction chamber, run through on the top cap and be equipped with the feed liquor hole, raw materials in the raw materials are deposited the case can pass the feed liquor hole enters into in the slip feed liquor piece.
6. The process for producing high purity sodium cyclamate as claimed in claim 5, wherein: and an air pressure punch for scattering and fusing the reaction solution is arranged in the sliding liquid inlet block.
7. The process for producing high purity sodium cyclamate of claim 1 wherein: and a flow blocking strip for turbulence of the solution in the reaction cavity is arranged on the inner wall of the reaction cavity.
8. The process for producing high purity sodium cyclamate of claim 1 wherein: the top cover is connected with a pressure control valve for adjusting the pressure in the reaction cavity.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2129336A1 (en) * | 1970-06-15 | 1971-12-23 | Bridgestone Tire Co Ltd | Method for carrying out a gas-liquid contact reaction and there for suitable device |
| CN101468303A (en) * | 2007-12-29 | 2009-07-01 | 亚申科技研发中心（上海）有限公司 | Device for developing catalysis technique |
| CN102728259A (en) * | 2012-07-13 | 2012-10-17 | 东阿阿胶阿华医疗器械有限公司 | Filtering machine and filtering process for producing rubber paste |
Family Cites Families (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06102388A (en) * | 1992-09-18 | 1994-04-15 | Hitachi Ltd | Control rod extension shaft |
| US5511519A (en) * | 1994-07-05 | 1996-04-30 | Homelite, Inc. | Temperature adjusting automatic choke system |
| AU7206901A (en) * | 2000-05-18 | 2001-11-26 | Sharp Kabushiki Kaisha | Sterilization method, ion generating element, ion generating device, and air conditioning device |
| CN101601987B (en) * | 2009-06-30 | 2012-05-09 | 宁波大学 | Device and method for realizing transportation of digital micro-fluid between microfluidic chips |
| CN205462255U (en) * | 2016-01-22 | 2016-08-17 | 江苏联威生化实业有限公司 | Reation kettle is used in happy plain production |
| CN207703024U (en) * | 2017-12-21 | 2018-08-07 | 广州奇劲机电工程有限公司 | A kind of water power mix-driving and energy-saving control system for cooling tower |
| CN213254367U (en) * | 2020-09-06 | 2021-05-25 | 绍兴东泰聚合材料有限公司 | Chemical industry reation kettle convenient to cooling |
| CN112316879A (en) * | 2020-11-26 | 2021-02-05 | 德清县虎马中环佳科技有限公司 | Mechanical device for producing low-toxicity urea-formaldehyde glue |
| CN112845400B (en) * | 2020-12-29 | 2022-04-19 | 芜湖发电有限责任公司 | Self-washing cooling device of transformer cooler |
-
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2129336A1 (en) * | 1970-06-15 | 1971-12-23 | Bridgestone Tire Co Ltd | Method for carrying out a gas-liquid contact reaction and there for suitable device |
| CN101468303A (en) * | 2007-12-29 | 2009-07-01 | 亚申科技研发中心（上海）有限公司 | Device for developing catalysis technique |
| CN102728259A (en) * | 2012-07-13 | 2012-10-17 | 东阿阿胶阿华医疗器械有限公司 | Filtering machine and filtering process for producing rubber paste |
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