CN112915565B - Rotary continuous production equipment and production method for sucrose-6-ester - Google Patents
Rotary continuous production equipment and production method for sucrose-6-ester Download PDFInfo
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- CN112915565B CN112915565B CN202110241328.2A CN202110241328A CN112915565B CN 112915565 B CN112915565 B CN 112915565B CN 202110241328 A CN202110241328 A CN 202110241328A CN 112915565 B CN112915565 B CN 112915565B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/12—Molecular distillation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/008—Liquid distribution
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/009—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in combination with chemical reactions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
- B01F27/80—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis
- B01F27/90—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis with paddles or arms
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H13/00—Compounds containing saccharide radicals esterified by carbonic acid or derivatives thereof, or by organic acids, e.g. phosphonic acids
- C07H13/02—Compounds containing saccharide radicals esterified by carbonic acid or derivatives thereof, or by organic acids, e.g. phosphonic acids by carboxylic acids
- C07H13/04—Compounds containing saccharide radicals esterified by carbonic acid or derivatives thereof, or by organic acids, e.g. phosphonic acids by carboxylic acids having the esterifying carboxyl radicals attached to acyclic carbon atoms
Abstract
The invention relates to the technical field of sucrose-6-ester production, in particular to a rotary type sucrose-6-ester continuous production device and a production method, which comprises the following steps: the invention relates to a cane sugar-6-ester preparation device, which comprises a tank body, a cooling body, a conical heating plate, a spray connection pipe, a stirrer, a liquid collecting plate, a pinion, a gearwheel and a driving motor, wherein the tank body is formed by connecting a lower tank cover, a main tank and an upper tank cover, the upper tank cover can be disassembled for convenient installation and maintenance during installation or disassembly, the driving motor is fixedly installed on the lower end surface of the lower tank cover, the pinion is fixedly installed on the driving motor, a vacuum pipe is fixedly installed on the circumference of the main tank, the cooling body is fixedly installed in the main tank, and the whole cooling body is of a shell structure.
Description
Technical Field
The invention relates to the field of sucrose-6-ester production, in particular to rotary sucrose-6-ester continuous production equipment and a production method.
Background
Sucralose is commonly called sucralose, is an artificial sweetener with high sweetness, can reach about 600 times (400-800 times) of sweetness of sucrose, has no energy, high sweetness, pure sweetness, high safety and the like, is one of the most ideal sweeteners at present, is a very important intermediate reactant for producing sucralose, has various synthesis paths, wherein the catalytic synthesis of organotin is relatively mature, and the existing relatively mature method for catalytically synthesizing sucrose-6-ester by organotin is as follows: (a) stirring and mixing sucrose, a polar aprotic solvent and an organotin acylation promoter, and heating, wherein organotin and sucrose are subjected to a stannation reaction in a polar aprotic solvent (DMF) solution of sucrose: sucrose + organotin → organotin sucrose complex + water to obtain a first reaction mixture; (b) removing water from the first reaction mixture to obtain a second reaction mixture free of water; (c) adding carboxylic anhydride into the second reaction mixture, and then cooling and stirring to react to generate sucrose-6-ester;
however, the existing sucrose-6-ester production process flow is complex, the production efficiency is low, the cost is high, and with the increasing demand of sucralose, the existing sucrose-6-ester preparation process flow and equipment can not meet the demand.
Disclosure of Invention
Therefore, the present invention has been made in view of the above problems, and an object of the present invention is to improve the production efficiency by modifying a molecular distillation apparatus so that all reaction processes can be completed in the apparatus at one time, and the whole sucrose-6-ester production process, the process time, and the like can be shortened, to solve the problems of many processes and low production efficiency of the conventional production technology, and to achieve the above objects by the following technical solutions:
a rotary sucrose-6-ester continuous production apparatus comprising: the tank body is formed by connecting a lower tank cover, a main tank and an upper tank cover, the upper tank cover can be disassembled during installation or disassembly so as to be convenient for installation and maintenance, the driving motor is fixedly installed on the lower end surface of the lower tank cover, the small gear is fixedly installed on the driving motor, and the vacuum tube is fixedly installed on the circumference of the main tank;
the cooling body is fixedly arranged in the main tank, the whole cooling body is of a shell structure, the peripheral surface of the cooling body is a cylindrical surface, the upper end surface of the cooling body is a conical surface, the interior of the shell is hollow, a cooling liquid flowing groove is formed in the shell, a cooling liquid input pipe is arranged on the conical surface of the cooling body, a cooling liquid output pipe is arranged on the cylindrical surface of the cooling body, the cooling liquid input pipe and the cooling liquid output pipe can be communicated with the cooling liquid flowing groove in the shell, a vacuum pipe is further arranged on the cylindrical surface of the cooling body, and the vacuum pipe can be communicated with the inner space of the cooling body but cannot be communicated with the cooling liquid flowing groove;
the conical heating plate is rotatably arranged right below the cooling body, a conical heating surface is arranged at the upper end of the conical heating plate, a stirring cavity is arranged in the conical heating surface, a plurality of stirring rods are fixedly arranged on the cavity wall of the stirring cavity, a liquid outlet cavity is arranged at the lower end of the conical heating surface, four liquid outlet notches are uniformly distributed on the circumference of the liquid outlet cavity, a large gear is fixedly arranged at the lowest end of the conical heating plate and can be meshed with a small gear fixed on a driving motor, and the driving motor can drive the conical heating plate to rotate at a high speed;
the spray pipe is fixedly arranged in the conical heating plate, a first feeding pipe, a second feeding pipe and a drain pipe are arranged in the spray pipe, symmetrical liquid spraying notches are formed in the circumferential surface of the upper end of the spray pipe, the liquid spraying notches can be communicated with the insides of the first feeding pipe and the second feeding pipe, a liquid receiving groove is formed above the liquid spraying notches, and the liquid receiving groove can be communicated with the inside of the drain pipe;
the stirrer is fixedly arranged outside the liquid outlet cavity on the conical heating plate, the upper end of the stirrer is contacted with the liquid outlet notch on the liquid outlet cavity, stirring paddles are arranged on the circumference of the stirrer, and the conical heating plate can drive the stirrer to rotate together when rotating;
the liquid collecting disc is fixedly arranged at the lower end of the conical heating disc, the top end of the liquid collecting disc is abutted with the lower end of the cylindrical surface of the cooling body to form a distillation chamber, a liquid collecting cavity and a mixing cavity are formed in the liquid collecting disc, the liquid collecting cavity can be communicated with a liquid outlet cavity in the conical heating disc, a liquid discharging pipe is fixedly arranged below the liquid collecting cavity, the liquid discharging pipe can be communicated with the inside of the liquid collecting cavity, a feeding pipe is further fixedly arranged on the circumferential surface of the liquid collecting cavity and can be communicated with the inside of the mixing cavity, mixed liquid enters the inside of the liquid outlet cavity from four liquid outlet notches in the conical heating disc under the stirring action of a stirring paddle on the stirrer, then flows into the liquid collecting cavity on the liquid collecting disc below from the liquid outlet cavity, and finally flows out from the liquid discharging pipe in the liquid collecting cavity.
In another aspect of the invention, a method for continuous production of sucrose-6-ester by rotary fermentation is provided, comprising the following steps:
s1: firstly, mixing a sucrose solution in a polar aprotic solvent;
s2: then, respectively inputting a sucrose solution dissolved in the polar aprotic solvent and the organotin acylation promoter from a first feeding pipe and a second feeding pipe, then spraying the liquid into a stirring cavity in the conical heating plate from two liquid spraying notches above the spraying pipe, and mixing the sucrose solution and the organotin acylation promoter by a stirring rod rotating at a high speed in the stirring cavity;
s3: then the mixed liquid after complete mixing is thrown onto the surface of the conical heating surface above under the centrifugal action of the conical heating plate, and under the centrifugal action of the conical heating surface, the mixed liquid is expanded continuously along the surface of the conical heating surface to form a uniform and thin liquid film, and meanwhile, the liquid film of the mixed liquid starts to perform a tinning reaction rapidly under the heating action of the conical heating surface to generate a heavy component substance organotin sucrose complex and light component substance water;
s4: the secondary water is directly evaporated into gas and moves upwards in the generation process, and because the molecular mean free path of the water is larger than that of the organic tin sucrose complex, water molecules can directly move to the conical inner surface of the cooling body above the conical heating surface and are rapidly condensed into liquid drops under the cooling action of the cooling body, then flow towards the middle along the conical inner surface of the cooling body, finally flow into a liquid receiving tank above the spray pipe, and then are discharged from a water discharge pipe;
s5: secondly, the gaseous heavy component substance organotin sucrose complex cannot reach the conical inner surface of the upper cooling body due to small molecular mean free path and then returns to the mixed liquid, the liquid heavy component substance organotin sucrose complex is thrown onto the cylindrical inner surface of the cooling body under the action of the conical heating plate and flows to the mixing cavity in the lower liquid collecting plate along the cylindrical inner surface, and the liquid heavy component substance organotin sucrose complex is cooled in the flowing process to obtain the completely dried organotin sucrose complex with low temperature;
s6: and simultaneously, carboxylic anhydride liquid enters the mixing cavity in the liquid collecting tray from the feeding pipe, is mixed under the rotation action of the stirrer and reacts rapidly, and sucrose-6-ester generated after the reaction enters the liquid outlet cavity from the liquid outlet notch above the stirrer, is discharged into the liquid collecting cavity in the liquid collecting tray from the liquid outlet cavity and is finally discharged by the liquid discharge pipe in the liquid collecting cavity.
The invention has the beneficial effects that:
1. all reaction processes for preparing the sucrose-6-ester can be completed in the molecular distillation equipment at one time by modifying the molecular distillation equipment, so that the reaction process and the connection time of upstream and downstream are shortened, and the production efficiency of the sucrose-6-ester is greatly improved;
2. the existing equipment needs to move the evaporated steam out of the evaporation cavity for condensation, and the moisture can be directly collected and discharged in one equipment through molecular distillation, so that the condensation efficiency is improved;
3. the molecular distillation process is irreversible, namely water molecules escape from the liquid surface and directly reach the conical inner surface of the cooling body, and do not return to the mixed liquid film after being condensed into liquid, so that the real-time distillation of the water molecules can be realized, the water generated when the stannization reaction of the sucrose solution on the heating plate occurs can be timely removed, the solution does not contain water, the stannization reaction can be more favorably carried out, and the stannization reaction efficiency is improved;
4. the organotin sucrose complex solution generated by the stannization reaction is directly cooled in the process of flowing on the cylindrical inner surface of the cooling body to obtain the completely dry organotin sucrose complex with low temperature, and at the moment, the reaction can be carried out in the third step at once, and the temperature is reduced in the flowing process, so that the time is saved, and the production efficiency is improved;
5. the stannization reaction of the sucrose solution and the removal of reaction water are simultaneously completed on the conical heating surface on the conical heating plate, so that the process of separately removing the reaction water is omitted, and the production efficiency of sucrose-6-ester is improved;
6. the temperature required by molecular distillation is low, and the removal of water molecules can be realized only by forming a certain temperature difference between the conical heating surface on the conical heating plate and the conical inner surface of the cooling body, so that the energy consumption of the whole equipment is low;
7. the stirring cavity is arranged in the conical heating plate, the organotin acylation promoter and the sucrose solution are mixed by driving the stirring rod in the stirring cavity to rotate rapidly, the mixture is quickly thrown onto the conical heating surface on the conical heating plate under the action of centrifugal force to carry out molecular distillation after being mixed, no stay and no transmission exist in the process from mixing to heating, the heating reaction distillation can be carried out rapidly after the mixture is mixed, and the efficiency is higher;
8. the conical heating plate simultaneously completes heating required by the reaction of the first reaction mixture and heating required by moisture removal, so that the reaction heating and the molecular distillation heating share one heating plate, a set of heating structure is omitted, and energy consumption and cost are saved;
9. the residence time of the first reaction mixture on the conical heating surface is short, and the temperature of the conical heating surface is low, so that the sugar is prevented from being decomposed at high temperature to reduce impurities in the solution;
10. the stirrer is arranged at the lower part of the conical heating plate for stirring and mixing, so that space resources at the lower part of the conical heating plate are fully utilized, the volume of the whole equipment is greatly reduced, and the equipment cost is reduced;
11. the liquid film formed in a rotating way is thinner and more uniform, so that the material is heated for a shorter time, the heating rate and the separation efficiency are higher, the thermal decomposition rate of heat-sensitive substances is lower, the material treatment capacity is increased, and the method is more suitable for industrial continuous production;
12. through carrying out the subregion to the inside of nozzle, make its inside inlet pipe one, inlet pipe two and the drain pipe of having simultaneously, make full use of the inside space resource of nozzle, make it accomplish the transport of the different stages liquid material of whole flow for conveyor volume becomes littleer, and whole cost is lower.
13. The top end of the liquid collecting disc is abutted against the lower end of the cylindrical surface of the cooling body to form a small sealed distillation chamber, and the vacuum tube is installed in the distillation chamber.
Drawings
Fig. 1 is a schematic view of the overall structure of the present invention.
FIG. 2 is a schematic view of the overall half-section structure of the present invention.
FIG. 3 is a schematic view showing the structure of the distillation body according to the present invention.
Fig. 4 is a schematic half-section structure diagram of the conical heating plate in the invention.
Fig. 5 is a front sectional view of the present invention.
Fig. 6 is a side sectional view of the present invention.
Description of the drawings:
100. a tank body; 110. discharging the tank cover; 120. a main tank; 121. a vacuum tube; 130. putting a tank cover on the tank; 200. a cooling body; 210. a coolant input tube; 220. a coolant outlet pipe; 230. a coolant flow tank; 300. a conical heating plate; 310. a conical heating surface; 320. a stirring chamber; 321. a stirring rod; 330. a liquid outlet cavity; 331. a liquid outlet notch; 400. a nozzle pipe; 401. a liquid spraying notch; 402. a liquid receiving tank; 410. a feeding pipe I; 420. a feeding pipe II; 430. a drain pipe; 500. a stirrer; 510. a stirring paddle; 600. a liquid collecting tray; 610. a liquid collection cavity; 620. a mixing chamber; 630. a liquid discharge pipe; 640. a feeding pipe; 700. a pinion gear; 800. a bull gear; 900. the motor is driven.
Detailed Description
Preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings however, the present invention may be embodied in various forms, and thus, the present invention is not limited to the embodiments described hereinafter, and in addition, components not connected to the present invention will be omitted from the drawings for the sake of clearer description of the present invention;
as shown in fig. 1 to 6, a rotary type sucrose-6-ester continuous production apparatus comprises: the cooling device comprises a tank body 100, a cooling body 200, a conical heating plate 300, a spray connecting pipe 400, a stirrer 500, a liquid collecting plate 600, a pinion 700, a bull gear 800 and a driving motor 900;
the tank body 100 is formed by connecting three parts, namely a lower tank cover 110, a main tank 120 and an upper tank cover 130, when in installation or disassembly, the upper tank cover 130 can be disassembled for convenient installation and maintenance, a driving motor 900 is fixedly installed on the lower end surface of the lower tank cover 110, a pinion 700 is fixedly installed on the driving motor 900, and a vacuum pipe 121 is fixedly installed on the circumference of the main tank 120;
the cooling body 200 is fixedly installed inside the main tank 120, the cooling body 200 has a housing structure as a whole, wherein the periphery of the cooling body 200 is a cylindrical surface, the upper end surface is a conical surface, the interior of the housing is hollow, a cooling liquid flowing groove 230 is arranged in the housing, a cooling liquid input pipe 210 is arranged on the conical surface of the cooling body 200, a cooling liquid output pipe 220 is arranged on the cylindrical surface of the cooling body 200, both the cooling liquid input pipe 210 and the cooling liquid output pipe 220 can be communicated with the cooling liquid flowing groove 230 in the housing, a vacuum pipe 121 is also arranged on the cylindrical surface of the cooling body 200, the vacuum pipe 121 can be communicated with the inner space of the cooling body 200 but can not be communicated with the cooling liquid flowing groove 230, the cooling liquid can enter from the cooling liquid input pipe 210 and then flow in the cooling liquid flowing groove 230 in the cooling body 200, cooling the surface of the cooling body 200 during the flowing process, and finally flowing out of the cooling liquid output pipe 220;
the conical heating plate 300 is rotatably arranged right below the cooling body 200, the upper end of the conical heating plate 300 is provided with a conical heating surface 310, the conical heating surface 310 is internally provided with a stirring cavity 320, the wall of the stirring cavity 320 is fixedly provided with a plurality of stirring rods 321, the lower end of the conical heating surface 310 is provided with a liquid outlet cavity 330, four liquid outlet notches 331 are uniformly distributed on the circumference of the liquid outlet cavity 330, the lowest end of the conical heating plate 300 is fixedly provided with a large gear 800, the large gear 800 can be meshed with a small gear 700 fixed on a driving motor 900, the driving motor 900 can drive the conical heating plate 300 to rotate at a high speed, when two liquids enter the stirring cavity 320, the high-speed rotating stirring rods 321 can mix the two liquids, and when the two liquids are completely mixed, under the centrifugal force action of the conical heating plate 300, the mixed liquid can be thrown onto the surface of the conical heating surface 310 above, and will continue to spread along the surface of the conical heating surface 310 to form a uniform and thin liquid film under the centrifugal force of the conical heating surface 310;
the spraying pipe 400 is fixedly arranged in the conical heating plate 300, a first feeding pipe 410, a second feeding pipe 420 and a drain pipe 430 are arranged in the spraying pipe 400, symmetrical liquid spraying notches 401 are formed in the circumferential surface of the upper end of the spraying pipe 400, the liquid spraying notches 401 can be communicated with the first feeding pipe 410 and the second feeding pipe 420, a liquid receiving groove 402 is formed above the liquid spraying notches 401, and the liquid receiving groove 402 can be communicated with the interior of the drain pipe 430;
the stirrer 500 is fixedly arranged outside the liquid outlet cavity 330 on the conical heating plate 300, wherein the upper end of the stirrer 500 is in contact with the liquid outlet notch 331 on the liquid outlet cavity 330, the circumference of the stirrer 500 is provided with a stirring paddle 510, and the conical heating plate 300 can drive the stirrer 500 to rotate together when rotating;
the liquid collecting tray 600 is fixedly installed at the lower end of the conical heating tray 300, the top end of the liquid collecting tray 600 is abutted to the lower end of the cylindrical surface of the cooling body 200 to form a distillation chamber, a liquid collecting cavity 610 and a mixing cavity 620 are formed in the liquid collecting tray 600, the liquid collecting cavity 610 can be communicated with a liquid outlet cavity 330 in the conical heating tray 300, a liquid discharging pipe 630 is fixedly installed below the liquid collecting cavity 610, the liquid discharging pipe 630 can be communicated with the inside of the liquid collecting cavity 610, a feeding pipe 640 is further fixedly installed on the circumferential surface of the liquid collecting cavity 610, the feeding pipe 640 can be communicated with the inside of the mixing cavity 620, mixed liquid enters the inside of the liquid outlet cavity 330 from four liquid outlet notches 331 in the conical heating tray 300 under the stirring action of a stirring paddle 510 on the stirrer 500, then flows into the liquid collecting cavity 610 on the liquid collecting tray 600 below from the liquid outlet cavity 330, and finally flows out from the liquid discharging pipe 630 in the liquid collecting cavity 610.
The invention also provides a method for continuously producing the rotary sucrose-6-ester, which comprises the following steps:
s1: firstly, mixing a sucrose solution in a polar aprotic solvent;
s2: then, a sucrose solution dissolved in the polar aprotic solvent and the organotin acylation promoter are respectively input from the first feeding pipe 410 and the second feeding pipe 420, then the liquid is sprayed into the stirring cavity 320 in the conical heating plate 300 from the two liquid spraying notches 401 above the spraying pipe 400, and the sucrose solution and the organotin acylation promoter are mixed by the stirring rod 321 rotating at a high speed in the stirring cavity 320;
s3: then the mixed liquid after complete mixing is thrown onto the surface of the conical heating surface 310 above under the centrifugal action of the conical heating plate 300, and under the centrifugal action of the conical heating surface 310, the mixed liquid continuously expands along the surface of the conical heating surface 310 to form a uniform and thin liquid film, and meanwhile, the liquid film of the mixed liquid starts to perform a tinning reaction rapidly under the heating action of the conical heating surface 310 to generate a heavy component substance organotin sucrose complex and light component substance water;
s4: the secondary water is directly evaporated into gas and moves upwards in the generation process, and as the molecular mean free path of the water is larger than that of the organic tin sucrose complex, water molecules directly move to the conical inner surface of the cooling body 200 above the conical heating surface 310 and are rapidly condensed into liquid drops under the cooling effect of the cooling body 200, then flow towards the middle along the conical inner surface of the cooling body 200, finally flow into the liquid receiving tank 402 above the spray connecting pipe 400, and then are discharged from the water discharge pipe 430;
s5: secondly, the gaseous heavy component substance organotin sucrose complex cannot reach the conical inner surface of the upper cooling body 200 due to small molecular mean free path and then returns to the mixed liquid, the liquid heavy component substance organotin sucrose complex is thrown onto the cylindrical inner surface of the cooling body 200 under the action of the conical heating plate 300 and flows into the mixing cavity 620 in the lower liquid collecting plate 600 along the cylindrical inner surface, and the liquid heavy component substance organotin sucrose complex is cooled in the flowing process to obtain the completely dried and low-temperature organotin sucrose complex;
s6: and meanwhile, the carboxylic anhydride liquid enters the mixing cavity 620 in the liquid collecting tray 600 from the feeding pipe 640, then is mixed under the rotation action of the stirrer 500 and reacts quickly, and the sucrose-6-ester generated after the reaction completely enters the liquid outlet cavity 330 from the liquid outlet notch 331 above the stirrer 500, then is discharged into the liquid collecting cavity 610 in the liquid collecting tray 600 from the liquid outlet cavity 330, and finally is discharged from the liquid discharge pipe 630 in the liquid collecting cavity 610.
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 person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (2)
1. A rotary sucrose-6-ester continuous production apparatus comprising: the utility model provides a jar body (100), the cooling body (200), toper heating plate (300), spout pipe (400), agitator (500), catch tray (600), pinion (700), gear wheel (800), driving motor (900), jar body (100) is by lower cover (110), main jar (120) and last cover (130) are constituteed, driving motor (900) are installed to the lower terminal surface of lower cover (110), the output shaft of driving motor (900) just is located main jar (120) internally mounted and has pinion (700), fixed mounting vacuum tube (121) on the circumference of main jar (120), its characterized in that: the cooling body (200) is fixedly arranged in the main tank (120), the whole cooling body (200) is of a shell structure, the peripheral surface of the cooling body (200) is a cylindrical surface, the upper end surface of the cooling body is a conical surface, the shell is hollow, a vacuum tube (121) is connected with the cylindrical surface of the cooling body (200), the vacuum tube (121) can be communicated with the inner space of the cooling body (200) but not communicated with a cooling liquid flowing groove (230), the cooling body (200) is internally provided with the cooling liquid flowing groove (230), the conical surface of the cooling body (200) is provided with a cooling liquid input tube (210), one side of the cylindrical surface of the cooling body (200) is provided with a cooling liquid output tube (220), the cooling liquid input tube (210) and the cooling liquid output tube (220) are both communicated with the cooling liquid flowing groove (230), the conical heating plate (300) is arranged right below the cooling body (200), and the lowest end of the conical heating plate (300) is fixedly provided with a large gear (800), the large gear (800) and the small gear (700) are meshed with each other, the spraying pipe (400) is fixedly installed inside the conical heating plate (300), a first feeding pipe (410), a second feeding pipe (420) and a drainage pipe (430) are arranged inside the spraying pipe (400), symmetrical liquid spraying notches (401) are formed in the circumferential surface of the upper end of the spraying pipe (400), the liquid spraying notches (401) are communicated with the insides of the first feeding pipe (410) and the second feeding pipe (420), a liquid receiving groove (402) is formed above the liquid spraying notches (401), the liquid receiving groove (402) is communicated with the inside of the drainage pipe (430), the upper end of the conical heating plate (300) is provided with a conical heating surface (310), the lower end of the conical heating surface (310) is provided with a liquid outlet cavity (330), four liquid outlet grooves (331) are installed on the circumference of the liquid outlet cavity (330), a stirring cavity (320) is formed inside the conical heating surface (310), and a plurality of stirring rods (321) are installed on the cavity wall of the stirring cavity (320), the stirrer (500) is fixedly arranged outside the liquid outlet cavity (330) on the conical heating plate (300), the upper end of the stirrer (500) is in contact with a liquid outlet notch (331) on the liquid outlet cavity (330), stirring paddles (510) are arranged on the circumference of the stirrer (500), the liquid collecting disc (600) is fixedly arranged at the lower end of the conical heating plate (300), the top end of the liquid collecting disc (600) is abutted against the lower end of the cylindrical surface of the cooling body (200) to form a distillation chamber, the liquid collecting cavity (610) and the mixing cavity (620) are arranged in the liquid collecting disc (600), the liquid collecting cavity (610) is communicated with the liquid outlet cavity (330) in the conical heating plate (300), the liquid collecting device is characterized in that a liquid discharge pipe (630) is fixedly mounted below the liquid collecting cavity (610), the liquid discharge pipe (630) is communicated with the inside of the liquid collecting cavity (610), a feeding pipe (640) is further fixedly mounted on the circumferential surface of the liquid collecting cavity (610), and the feeding pipe (640) is communicated with the inside of the mixing cavity (620).
2. A rotary continuous production method of sucrose-6-ester is characterized in that: use of a rotary sucrose-6-ester continuous production facility as claimed in claim 1 comprising the steps of:
s1: firstly, mixing a sucrose solution in a polar aprotic solvent;
s2: then, a sucrose solution dissolved in a polar aprotic solvent and an organotin acylation promoter are respectively input from a first feeding pipe (410) and a second feeding pipe (420), then liquid is sprayed into a stirring cavity (320) in a conical heating plate (300) from two liquid spraying notches (401) above a spraying pipe (400), and a stirring rod (321) rotating at a high speed in the stirring cavity (320) can mix the sucrose solution and the organotin acylation promoter;
s3: then the mixed liquid after complete mixing is thrown onto the surface of the conical heating surface (310) above under the centrifugal force action of the conical heating plate (300), and under the centrifugal force action of the conical heating surface (310), the mixed liquid continuously expands along the surface of the conical heating surface (310) to form a uniform liquid film, and simultaneously the liquid film of the mixed liquid starts to carry out a fast stannization reaction under the heating action of the conical heating surface (310), so that a heavy component substance organotin sucrose complex and a light component substance water are generated;
s4: the secondary water is directly evaporated into gas and moves upwards in the generation process, and as the molecular mean free path of the water is larger than that of the organic tin sucrose complex, the water molecules directly move to the conical inner surface of the cooling body (200) above the conical heating surface (310), are rapidly condensed into liquid drops under the cooling effect of the cooling body (200), then flow towards the middle along the conical inner surface of the cooling body (200), finally flow into the liquid receiving tank (402) above the spray pipe (400), and then are discharged from the water discharge pipe (430);
s5: secondly, the gaseous heavy component substance organotin sucrose complex cannot reach the conical inner surface of the upper cooling body (200) due to the small molecular mean free path and then returns to the mixed liquid, the liquid heavy component substance organotin sucrose complex is thrown onto the cylindrical inner surface of the cooling body (200) under the action of the conical heating plate (300) and flows into the mixing cavity (620) in the lower liquid collecting plate (600) along the cylindrical inner surface, and the liquid heavy component substance organotin sucrose complex is cooled in the flowing process to obtain the completely dried organotin sucrose complex with low temperature;
s6: and meanwhile, the carboxylic anhydride liquid enters the mixing cavity (620) in the liquid collecting tray (600) from the feeding pipe (640), then is mixed under the rotation action of the stirrer (500) and reacts quickly, and the sucrose-6-ester generated after the reaction completely enters the liquid outlet cavity (330) from the liquid outlet notch (331) above the stirrer (500), then is discharged into the liquid collecting cavity (610) in the liquid collecting tray (600) from the liquid outlet cavity (330), and finally is discharged from the liquid discharging pipe (630) in the liquid collecting cavity (610).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN202110241328.2A CN112915565B (en) | 2021-03-04 | 2021-03-04 | Rotary continuous production equipment and production method for sucrose-6-ester |
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| CN202110241328.2A CN112915565B (en) | 2021-03-04 | 2021-03-04 | Rotary continuous production equipment and production method for sucrose-6-ester |
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| CN112915565A CN112915565A (en) | 2021-06-08 |
| CN112915565B true CN112915565B (en) | 2022-04-08 |
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| CN114164343A (en) * | 2021-12-07 | 2022-03-11 | 江西宏科特种合金有限公司 | Method for producing small-particle titanium sponge and special device thereof |
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