CN112957760B - Sucrose-6-ester uninterrupted preparation equipment and production process flow - Google Patents
Sucrose-6-ester uninterrupted preparation equipment and production process flow Download PDFInfo
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- CN112957760B CN112957760B CN202110241301.3A CN202110241301A CN112957760B CN 112957760 B CN112957760 B CN 112957760B CN 202110241301 A CN202110241301 A CN 202110241301A CN 112957760 B CN112957760 B CN 112957760B
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- 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
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Abstract
The invention relates to the technical field of sucrose-6-ester production, in particular to a sucrose-6-ester uninterrupted preparation device and a production process flow, which comprise a tank body, a stirring device, a molecular distillation device and a collection reaction device; according to the invention, all reaction processes for preparing the sucrose-6-ester can be completed in the molecular distillation equipment at one time by reforming 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; simultaneously, the first reaction mixture is heated and mixed with the sucrose solution and the organic tin acylation accelerant in advance through the stirring mechanism, then the first reaction mixture is heated on the heating plate and directly reacts, and the heating plate simultaneously completes heating required for the reaction of the first reaction mixture and heating required for removing moisture, so that the reaction heating and the molecular distillation heating share one heating plate, a set of heating structure is omitted, and the energy consumption and the cost are saved.
Description
Technical Field
The invention relates to the technical field of sucrose-6-ester production, in particular to equipment and a production process flow for continuously preparing sucrose-6-ester.
Background
Sucralose is commonly called sucralose, is an artificial sweetener with high sweetness, can reach about 600 times (400 times and 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 sucrose-6-ester which is a very important intermediate reactant for producing sucralose, has various synthesis routes, 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, mixing and heating sucrose, a polar aprotic solvent and an organotin acylation promoter, 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 production process of sucrose 6 ester, the process time, and the like can be shortened, so as to solve the problems of many production processes and low production efficiency in the prior art, and the present invention achieves the above objects by the following technical solutions:
the equipment for continuously preparing the sucrose-6-ester comprises a tank body, wherein the tank body comprises a lower tank body and an upper tank body, and a tank cover is arranged at the top of the upper tank body; a vacuum port is formed in the rear side of the top of the tank cover, a stirring device is arranged in the middle of the tank cover, and a liquid material inlet I and a liquid material inlet II are respectively formed in the position, close to the left side and the right side of the stirring device, of the top of the tank cover; the stirring device comprises a first driving motor, and the first driving motor is fixedly connected with the middle of the top of the tank cover; the stirring device is characterized in that a stirring rod is arranged at one output end of the driving motor, stirring paddles are arranged around the stirring rod, a mixing drum is arranged outside the stirring paddles, and the bottom of the mixing drum is fixedly connected with the lower end of the stirring rod; the mixing drum is characterized in that liquid outlets are formed in the left side and the right side of the mixing drum, liquid separating discs are arranged on the outer sides of the liquid outlets, the top of each liquid separating disc is fixedly connected with the bottom of the mixing drum, and liquid separating ports are formed in the front side and the rear side of the bottom of each liquid separating disc.
Preferably, the bottom of the liquid separating disc is provided with a molecular distillation device, the molecular distillation device comprises a heating plate, and the outer side of the heating plate is fixedly connected with the inner wall of the upper tank body; both sides are provided with the hydrojet pipe around the hot plate inner wall, the hydrojet mouth has been seted up in the hydrojet pipe outside, the hydrojet top is provided with the inlet tube, inlet tube inner is provided with the upper fixed frame.
Preferably, the top of the liquid inlet pipe is provided with a liquid inlet; the liquid inlet is matched with the liquid separating port; scraping rollers are arranged on the left side and the right side of the inner wall of the heating plate, and connecting rods are arranged on the inner sides of the upper end and the lower end of each scraping roller; the inner ends of the connecting rods are movably connected with the left end and the right end of the upper fixing frame and the lower fixing frame; the middle of the bottom of the upper fixing frame is provided with a condensing plate, and the bottom of the condensing plate is provided with a liquid collecting disc.
Preferably, the left side and the right side of the liquid collecting disc are fixedly connected with the inner end of the lower fixing frame; the condensing plate comprises a light component condensing plate and a heavy component condensing plate, and the liquid collecting disc comprises a light component collecting cavity and a heavy component collecting cavity; liquid leakage ports are formed in the bottoms of the light component collecting cavity and the heavy component collecting cavity; the light component condensation plate is matched with the light component collection cavity, and the heavy component condensation plate is matched with the heavy component collection cavity; and a collecting reaction device is arranged at the bottom of the liquid collecting disc.
Preferably, the collection reaction device comprises a flow distribution plate, a mixing tank and a reaction tank; the splitter disc, the mixing tank and the reaction tank are sequentially connected from top to bottom; a condensation output pipe is arranged inside the left side of the flow distribution disc, and a condensation input pipe is arranged inside the condensation output pipe; the upper end of the condensation input pipe is arranged in the condensation plate and generates reflux with the condensation input pipe; a water collecting area and a heavy component collecting area are arranged on the top of the flow distribution plate from inside to outside, and an arc-shaped notch is formed in the bottom of the heavy component collecting area.
Preferably, a drain pipe is arranged on the right side of the flow distribution disc and communicated with the moisture collection area; a discharge pipe is arranged in the mixing tank, and a feeding pipe is arranged on the right side of the discharge pipe; the reactor is characterized in that a mounting hole is formed in the middle of the bottom of the reactor, a flow divider is arranged in the mounting hole, a second driving motor is arranged at the lower end of the flow divider, a liquid discharge pipe is formed in the right side of the bottom of the reactor, and a liquid discharge pipe is arranged at the lower end of the liquid discharge pipe.
Preferably, the inner end of the connecting rod is provided with a limiting rod, and the outer ends of the upper fixing frame and the lower fixing frame are both provided with limiting ports; the limiting rod is movably connected with the limiting port through a limiting spring.
Preferably, the moisture collection region is matched with the light component collection chamber, and the heavy component collection region is matched with the heavy component collection chamber.
Preferably, the hot plate is inside to be seted up the cylindricality cambered surface, the cylindricality cambered surface with scrape and roll the phase-match, arrange the material socle portion and seted up a plurality of little round holes, light component condensation plate and heavy component condensation plate surface all are provided with a plurality of little cambered surfaces.
A sucrose-6-ester uninterrupted production process flow comprises the following steps:
s1: firstly, mixing a sucrose solution in a polar aprotic solvent;
s2: then respectively inputting the sucrose solution and the organic tin acylation promoter dissolved in the polar aprotic solvent into a mixing cylinder from a liquid material inlet I and a liquid material inlet II, driving a motor I to rotate so as to drive a stirring device and a molecular distillation device to rotate, and mixing the sucrose solution and the organic tin acylation promoter by a stirring rod in the stirring device when the stirring device rotates;
s3: then after mixing, the mixed liquid flows into a liquid separating disc from a liquid outlet on a mixing cylinder, and enters a liquid inlet pipe on a molecular distillation device from a liquid separating port in the liquid separating disc, the liquid spraying port in a liquid spraying pipe on the molecular distillation device sprays the mixed liquid to the surface of a heating plate to form a liquid film when the molecular distillation device rotates, and the liquid film of the mixed liquid starts to carry out a fast stannization reaction under the heating action of the heating plate to generate a heavy component substance organotin sucrose complex and light component substance water;
s4: the secondary water is directly evaporated into gas to escape in the generation process, and water molecules can move to a light component condensation plate with a longer distance to be rapidly condensed into liquid drops and flow away along a cylindrical cambered surface on the light component condensation plate;
s5: secondly, after the liquid spraying pipe rotates ninety degrees, the scraping roller on the upper fixing frame can roll the reacted organotin sucrose complex to form a thinner liquid film, at the moment, the heavy component condensation plate rotates, the organotin sucrose complex can be quickly evaporated and moves to the heavy component condensation plate, and the organotin sucrose complex is condensed into liquid by the heavy component condensation plate, so that the completely dry organotin sucrose complex with lower temperature is obtained;
s6: then the water molecules and the organic tin sucrose complex molecules are condensed into liquid and flow out along the surface of the heavy component condensation plate, the liquid water molecules and the liquid organic tin sucrose complex molecules are respectively collected by the light component collection cavity and the heavy component collection cavity in the liquid collection plate and flow out from respective liquid leakage openings, the liquid water molecules flow into the water collection area in the flow distribution plate and flow out from the drain pipe, and the liquid organic tin sucrose complex molecules also flow into the heavy component collection area in the flow distribution plate and flow out from the arc-shaped notch on the heavy component collection area and flow into the mixing tank;
s7: and finally, filling carboxylic anhydride from a feeding pipe on the mixing tank, enabling the carboxylic anhydride to flow into the mixing tank from a plurality of small circular holes of the discharge pipe in a circumferential manner to be mixed with liquid organotin sucrose complex molecules, enabling the mixed liquid to flow onto the surface of the flow divider, enabling the flow divider to uniformly disperse the liquid onto the inner surface of the reaction tank by rotating under the driving of a driving motor II, forming a liquid film on the inner surface and quickly reacting, and discharging the generated sucrose-6-ester from a liquid discharge pipe after the reaction is completed. 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 directly reach the condensing plate after escaping from the liquid surface and are condensed into liquid, and the liquid does not return to the mixed liquid film, so that the real-time distillation of the water molecules can be realized, the produced water can be removed in time when the stannization reaction of the sucrose solution in the molecular distillation section occurs, the solution does not contain water, the stannization reaction is more favorably carried out, and the stannization reaction efficiency is improved;
4. the organotin sucrose complex solution generated by the stannation reaction is completely dry and the temperature is reduced when the organotin sucrose complex solution is condensed into liquid by the heavy component condensation plate, the reaction can be carried out in the third step at once, and the heavy component condensation plate is cooled simultaneously when the organotin sucrose complex solution is collected, so that the process of independent cooling is omitted, the process is simplified, 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 a heating plate for molecular distillation, so that the process of independently removing the reaction water is omitted, and the production efficiency of the 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 heating plate and the condensing plate, so that the energy consumption of the whole equipment is low;
7. the sucrose solution and the organic tin acylation promoter are mixed by a stirring mechanism in advance before the first reaction mixture is heated, then the first reaction mixture is heated on a heating plate and directly reacts, and the 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 the energy consumption and the cost are saved;
8. the residence time of the first reaction mixture on the heating plate is short, and the temperature of the heating plate is low, so that the sugar is prevented from being decomposed at high temperature to reduce impurities in the solution;
9. the surface of the heating plate is divided into a plurality of parts formed by sequentially arranging the cylindrical cambered surfaces, so that a reaction area of the first reaction mixture solution on the heating plate is divided into a plurality of small reaction units, the contact area of the plurality of cylindrical cambered surfaces and the first reaction mixture is increased, namely, the heating area is increased, the temperature required by the tinning reaction is quickly reached, the reaction efficiency of the tinning reaction is improved, the reaction time is reduced, and the removal efficiency of water molecules is also improved when the heating area is increased;
10. the surfaces of the light component condensation plate and the heavy component condensation plate are also divided into a plurality of cambered surfaces, the surface area of the cambered surfaces is large, the condensation area of the light component gas and the heavy component gas in contact with the cambered surfaces is large, the condensation effect is better, each cambered surface unit is more favorable for converging condensate droplets to accelerate the flow of condensate water, and the condensation efficiency is improved;
11. the light component condensation plate and the heavy component condensation plate share one set of cooling system, so that the cooling cost is reduced;
12. the first reaction mixture is uniformly distributed on the heating plate through the scraping roller and forms a thin liquid film, the first reaction mixture in the liquid film form is small in size, fast in heating and short in reaction time.
Drawings
Fig. 1 is a schematic view of the overall structure of the present invention.
FIG. 2 is a schematic main sectional view of the overall structure of the present invention.
FIG. 3 is a left side cross-sectional view of the present invention.
Fig. 4 is a rear sectional view of the present invention.
FIG. 5 is a schematic view of the structure of the molecular distillation apparatus according to the present invention.
Fig. 6 is a sectional view taken along line a-a of fig. 4.
FIG. 7 is a schematic view showing the assembly and disassembly of the collecting reaction apparatus of the present invention.
Reference numerals: 100. a tank body; 110. a tank body is arranged; 120. feeding the tank body; 130. a can lid; 131. a vacuum port; 132. a liquid material inlet I; 133. a liquid material inlet II; 200. a stirring device; 210. a mixing drum; 211. a liquid outlet; 220. a liquid separating disc; 221. a liquid separation port; 230. a stirring rod; 231. a stirring paddle; 240. driving a motor I; 300. a molecular distillation device; 310. heating plates; 311. a cylindrical arc surface; 320. a liquid inlet pipe; 321. a liquid inlet; 330. a liquid spraying pipe; 331. a liquid spraying port; 340. an upper fixing frame; 341. a limiting port; 350. scraping and rolling; 360. a connecting rod; 361. a limiting rod; 362. a limiting spring; 370. a condensing plate; 371. a light component condensing plate; 372. a heavies condensing panel; 380. a liquid collecting tray; 381. a light component collection chamber; 382. a heavy fraction collection chamber; 383. a liquid leakage port; 390. a lower fixing frame; 400. collecting the reaction device; 410. a diverter tray; 411. a condensation output pipe; 412. a condensing input pipe; 413. a drain pipe; 414. a heavy ends collection area; 414a, an arc-shaped notch; 415. a moisture collection area; 420. a mixing tank; 421. a feed pipe; 422. a discharge pipe; 430. a reaction tank; 431. a flow divider; 432. mounting holes; 433. a liquid discharge pipe; 434. and driving a second motor.
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 figure 1, the equipment for continuously preparing the sucrose-6-ester and the production process flow comprise a tank body 100, a stirring device 200, a molecular distillation device 300 and a collecting reaction device 400;
as shown in fig. 2, the tank 100 is composed of a lower tank 110, an upper tank 120 and a tank cover 130, which are connected to each other, and one of the three parts can be removed for installation and maintenance when necessary, and the tank cover 130 is provided with a vacuum port 131, a first liquid inlet 132 and a second liquid inlet 133;
as shown in fig. 2 to 7, the stirring device 200 includes: the mixing cylinder 210, the liquid distribution plate 220, the stirring rod 230 and the driving motor I240 are arranged in sequence, the liquid distribution plate 220 is a circular disc body with a convex circumferential edge, two liquid distribution ports 221 which are symmetrical along the center are formed in the inner end face of the liquid distribution plate 220, the mixing cylinder 210 is a circular truncated cone-shaped cylinder body, the lower surface of the mixing cylinder is a circular conical surface, the mixing cylinder is arranged right below a liquid material inlet I132 and a liquid material inlet II 133 in the tank cover 130, liquid outlets 211 are symmetrically formed in positions, which are spaced from the lower end face, on the circular conical surface of the lower portion of the mixing cylinder 210, the lower end of the mixing cylinder 210 is fixed on the inner end face of the liquid distribution plate 220, the stirring rod 230 is fixed inside the mixing cylinder 210, a plurality of stirring paddles 231 which are inclined upwards are arranged on the cylindrical surface of the stirring rod 230, the driving motor I240 is fixedly arranged on the surface of the upper tank body 120, an output shaft at the lower end of the driving motor I240 is fixedly connected with the stirring rod 230, and the mixing cylinder 210, the liquid distribution plate 220, and the driving cylinder are driven when the driving motor I240 rotates, The stirring rod 230 rotates together, wherein the stirring paddle 231 on the stirring rod 230 and the mixing cylinder 210 stir the mixed liquid;
the molecular distillation apparatus 300, comprising: the heating plate 310, the liquid inlet pipe 320, the liquid spraying pipe 330, the upper fixing frame 340, the scraping roller 350, the connecting rod 360, the condensing plate 370, the liquid collecting tray 380 and the lower fixing frame 390, the heating plate 310 is a cylindrical barrel fixed on the inner circumferential surface of the upper tank 120, the outer surface of the heating plate 310 is heated by a heating wire, the inner circumferential surface of the heating plate 310 is formed by sequentially arranging a plurality of cylindrical arc surfaces 311, the plurality of cylindrical arc surfaces 311 can increase the inner surface area of the heating plate 310, the upper fixing frame 340 is a cuboid with a certain width, the top end of the upper fixing frame 340 is fixedly connected with the lower end of the liquid collecting tray 220 in the stirring device 200, two limiting ports 341 are symmetrically formed on the left side and the right side of the upper fixing frame 340, two liquid inlet pipes 320 are symmetrically arranged on the front side and the rear side of the upper fixing frame 340 along the center of the end surfaces, the upper half circumferential surface of the liquid inlet pipe 320 is provided with a liquid inlet 321, the liquid inlet 321 is communicated with the liquid separating port 221 on the liquid collecting tray 220 in the stirring device 200, the end of the liquid inlet pipe 320 is fixedly connected with a liquid spraying pipe 330, the interior of the liquid inlet pipe 320 can be communicated with the interior of the liquid spraying pipe 330, the outer circumference of the liquid spraying pipe 330 is provided with a plurality of liquid spraying ports 331, liquid in the liquid distribution plate 220 can enter the liquid inlet pipe 320 through the liquid distribution ports 221 and can be sprayed out from the liquid spraying ports 331 in the liquid spraying pipe 330, the lower fixing frame 390 has the structure completely same as that of the upper fixing frame 340, a condensing plate 370 is fixed between the upper fixing frame 340 and the lower fixing frame 390, the interior of the condensing plate 370 is hollow and consists of a light component condensing plate 371 occupying three quarters of the circumference and a heavy component condensing plate 372 occupying one quarter of the circumference, wherein the diameter of the light component condensing plate 371 occupying three quarters of the circumference is smaller than that of the heavy component condensing plate 372 occupying one quarter of the circumference, the outer surface of the light component condensing plate 371 and the inner surface of the heating plate 310 have the same shape, and the surface area is increased to facilitate the condensation of water, a liquid collecting tray 380 is fixedly installed in the middle of the lower fixing frame 390, the liquid collecting tray 380 is composed of a light component collecting cavity 381 and a heavy component collecting cavity 382, liquid leakage ports 383 are respectively formed in the bottom end faces of the light component collecting cavity 381 and the heavy component collecting cavity 382, wherein the light component collecting cavity 381 is used for collecting light component substances condensed into liquid and discharging the light component substances from the liquid leakage ports 383 under a light component condensing plate 371, the heavy component collecting cavity 382 is used for collecting heavy component substances condensed into liquid and discharging the heavy component substances from the liquid leakage ports 383 under the heavy component condensing plate 372, a connecting rod 360 is movably installed in two limiting ports 341 at the left end and the right end of the upper fixing frame 340 and the lower fixing frame 390, a scraping roller 350 is rotatably installed on the connecting rod 360, and a limiting spring 362 is installed on the limiting rod 361 on the connecting rod 360, so that the connecting rod 360 can move left and right in the limiting ports 341;
the collection reaction apparatus 400 includes: the diverter disc 410 is fixedly arranged at the lower end of a liquid collecting disc 380 in the molecular distillation device 300, a condensation output pipe 411 is arranged in the diverter disc 410, a condensation input pipe 412 is arranged in the condensation output pipe 411, the other end of the condensation input pipe 412 is arranged in the condensation plate 370 in the molecular distillation device 300, condensate can flow into the condensation plate 370 from the condensation input pipe 412 and flows out from the condensation output pipe 411 to achieve the effect of cooling the condensation plate 370, the diverter disc 410 is provided with a heavy component collecting area 414 and a water collecting area 415, an arc-shaped notch 414a is formed in the heavy component collecting area 414, a drain pipe 413 is further arranged in the diverter disc 410, the inlet of the drain pipe 413 is arranged in the water collecting area 415, so that the water can be discharged from the drain pipe 413, the mixing tank 420 is fixedly arranged on the lower end face of the diverter disc 410, a feed pipe 421 is fixedly arranged on the mixing tank 420, the feeding pipe 421 is fixedly provided with a discharging pipe 422, the lower circumferential surface of the discharging pipe 422 is provided with a plurality of small circular holes, liquid entering the feeding pipe 421 can be discharged in a trickle circumferential manner from the plurality of small circular holes on the discharging pipe 422, at this time, heavy component liquid can also flow into the mixing tank 420 from the arc-shaped notch 414a in the diverter disc 410 and can be better mixed with the liquid in the feeding pipe 421, the reaction tank 430 is fixedly arranged on the lower end surface of the mixing tank 420, the reaction tank 430 is internally provided with a diverter 431 capable of being arranged in a central mounting hole 432 of the reaction tank 430, the other end of the diverter 431 is connected with a second driving motor 434, the bottom end surface of the reaction tank 430 is provided with a liquid discharge pipe 433, the mixed liquid from the mixing tank 420 flows onto the surface of the diverter 431, the diverter 431 is driven by the second driving motor 434 to uniformly disperse the liquid onto the inner surface of the reaction tank 430 through rotation, and a liquid film is formed on the inner surface, and is discharged from the liquid discharge pipe 433 after the reaction is completed.
The invention also provides equipment for continuously preparing the sucrose-6-ester and a production process flow, wherein the equipment comprises the following steps:
s1: firstly, mixing a sucrose solution in a polar aprotic solvent;
s2: then, respectively inputting the sucrose solution and the organotin acylation promoter dissolved in the polar aprotic solvent into the mixing cylinder 210 from the first liquid material inlet 132 and the second liquid material inlet 133, driving the first motor 240 to rotate so as to drive the stirring device 200 and the molecular distillation device 300 to rotate, and mixing the sucrose solution and the organotin acylation promoter by a stirring rod 230 in the stirring device 200 when the stirring device 200 rotates;
s3: then, after the mixing, the mixed liquid flows into the liquid separation disc 220 from the liquid outlet 211 on the mixing cylinder 210, and enters the liquid inlet pipe 320 on the molecular distillation device 300 from the liquid separation port 221 in the liquid separation disc 220, when the molecular distillation device 300 rotates, the liquid spray port 331 in the liquid spray pipe 330 on the molecular distillation device firstly sprays the mixed liquid to the surface of the heating plate 310 to form a liquid film, and the liquid film of the mixed liquid starts to perform a stannization reaction rapidly under the heating action of the heating plate 310 to generate a heavy component substance organotin sucrose complex and light component substance water;
s3: the secondary water is directly evaporated into gas to escape in the generation process, and water molecules can move to the light component condensation plate 371 which is far away to be rapidly condensed into liquid drops and flow away along the cylindrical cambered surface 311 on the light component condensation plate 371;
s4: secondly, after the liquid spraying pipe 330 rotates ninety degrees, the scraping roller 350 on the upper fixing frame 340 rolls the reacted organotin sucrose complex to form a thinner liquid film, at this time, the heavy component condensation plate 372 rotates, the organotin sucrose complex is quickly evaporated and moves to the heavy component condensation plate 372, and is condensed into liquid by the heavy component condensation plate 372, so that the completely dried organotin sucrose complex with lower temperature is obtained;
s5: then the water molecules and the organotin sucrose complex molecules are condensed into liquid and flow out along the surface of the heavy component condensation plate 372, the liquid water molecules and the liquid organotin sucrose complex molecules are respectively collected by the light component collection cavity 381 and the heavy component collection cavity 382 in the liquid collection tray 380 and flow out from respective liquid leakage openings 383, the liquid water molecules flow into the moisture collection area 415 in the diverter tray 410 and flow out from the drain pipe 413, and the liquid organotin sucrose complex molecules also flow into the heavy component collection area 414 in the diverter tray 410 and flow out from the arc-shaped notch 414a on the liquid organotin sucrose complex molecules into the mixing tank 420;
s6: and finally, the carboxylic anhydride is filled from a feeding pipe 421 on the mixing tank 420, flows into the mixing tank 420 from a plurality of small round holes of a discharging pipe 422 in a trickle circumferential manner and is mixed with liquid organotin sucrose complex molecules, the mixed liquid flows onto the surface of a flow divider 431, the flow divider 431 is driven by a driving motor II 434 to uniformly disperse the liquid onto the inner surface of the reaction tank 430 through rotation, a liquid film is formed on the inner surface and reacts rapidly, and the sucrose-6-ester generated after the reaction is completed is discharged from a liquid discharging pipe 433.
Claims (10)
1. The utility model provides an incessant preparation facility of sucrose-6-ester, includes jar body (100), its characterized in that: the tank body (100) comprises a lower tank body (110) and an upper tank body (120), and a tank cover (130) is arranged at the top of the upper tank body (120); a vacuum port (131) is formed in the rear side of the top of the tank cover (130), a stirring device (200) is arranged in the middle of the tank cover (130), and a first liquid material inlet (132) and a second liquid material inlet (133) are formed in the top of the tank cover (130) and are close to the left side and the right side of the stirring device (200) respectively; the stirring device (200) comprises a first driving motor (240), and the first driving motor (240) is fixedly connected with the middle of the top of the tank cover (130); the output end of the first driving motor (240) is provided with a stirring rod (230), stirring paddles (231) are arranged around the stirring rod (230), a mixing cylinder (210) is arranged outside the stirring paddles (231), and the bottom of the mixing cylinder (210) is fixedly connected with the lower end of the stirring rod (230); liquid outlets (211) are formed in the left side and the right side of the mixing cylinder (210), liquid separating discs (220) are arranged on the outer sides of the liquid outlets (211), the tops of the liquid separating discs (220) are fixedly connected with the bottom of the mixing cylinder (210), and liquid separating ports (221) are formed in the front side and the rear side of the bottom of each liquid separating disc (220); the molecular distillation device (300) is arranged at the bottom of the liquid distribution disc (220), the molecular distillation device (300) comprises a heating plate (310), liquid spraying pipes (330) are arranged on the front side and the rear side of the inner wall of the heating plate (310), a liquid inlet pipe (320) is arranged at the top of the liquid spraying pipe (330), an upper fixing frame (340) is arranged at the inner end of the liquid inlet pipe (320), scraping rollers (350) are arranged on the left side and the right side of the inner wall of the heating plate (310), a condensing plate (370) is arranged in the middle of the bottom of the upper fixing frame (340), and a liquid collecting disc (380) is arranged at the bottom of the condensing plate (370); the condenser plate (370) comprises a light fraction condenser plate (371) and a heavy fraction condenser plate (372), and the drip pan (380) comprises a light fraction collection chamber (381) and a heavy fraction collection chamber (382); a collecting reaction device (400) is arranged at the bottom of the liquid collecting disc (380); the collection reaction device (400) comprises a diversion disc (410), a mixing tank (420) and a reaction tank (430); a moisture collecting area (415) and a heavy component collecting area (414) are arranged on the top of the diverter disc (410) from inside to outside, and an arc-shaped notch (414 a) is formed in the bottom of the heavy component collecting area (414); a discharge pipe (422) is arranged in the mixing tank (420), and a feeding pipe (421) is arranged on the right side of the discharge pipe (422); the middle of the bottom of the reaction tank (430) is provided with a mounting hole (432), and a flow divider (431) is arranged in the mounting hole (432).
2. The apparatus of claim 1, wherein the apparatus comprises: the outer side of the heating plate (310) is fixedly connected with the inner wall of the upper tank body (120); and a liquid spraying port (331) is formed in the outer side of the liquid spraying pipe (330).
3. The apparatus of claim 1, wherein the apparatus comprises: the top of the liquid inlet pipe (320) is provided with a liquid inlet (321); the liquid inlet (321) is matched with the liquid separating port (221); the inner sides of the upper end and the lower end of the scraping roller (350) are provided with connecting rods (360); the inner end of the connecting rod (360) is movably connected with the left end and the right end of the upper fixing frame (340) and the lower fixing frame (390).
4. The apparatus of claim 1, wherein the apparatus comprises: the left side and the right side of the liquid collecting disc (380) are fixedly connected with the inner end of the lower fixing frame (390); the bottoms of the light component collecting cavity (381) and the heavy component collecting cavity (382) are respectively provided with a liquid leakage port (383); the light fraction condenser plate (371) and the light fraction collection chamber (381) are matched, and the heavy fraction condenser plate (372) and the heavy fraction collection chamber (382) are matched.
5. The apparatus of claim 1, wherein the apparatus comprises: the splitter plate (410), the mixing tank (420) and the reaction tank (430) are sequentially connected from top to bottom; a condensation output pipe (411) is arranged inside the left side of the flow distribution disc (410), and a condensation input pipe (412) is arranged inside the condensation output pipe (411); the upper end of the condensation input pipe (412) is arranged inside the condensation plate (370) and generates backflow with the condensation input pipe (412).
6. The apparatus of claim 1, wherein the apparatus comprises: a drain pipe (413) is arranged on the right side of the flow distribution disc (410), and the drain pipe (413) is communicated with a moisture collection area (415); the lower end of the flow divider (431) is provided with a second driving motor (434), the right side of the bottom of the reaction tank (430) is provided with a liquid discharge pipe (433), and the lower end of the liquid discharge pipe (433) is provided with a liquid discharge pipe (433).
7. The apparatus of claim 3, wherein: the inner end of the connecting rod (360) is provided with a limiting rod (361), and the outer ends of the upper fixing frame (340) and the lower fixing frame (390) are both provided with limiting ports (341); the limiting rods (361) are respectively movably connected with the limiting openings (341) through limiting springs (362).
8. The apparatus of claim 1, wherein the apparatus comprises: the moisture collection region (415) is mated to a light fraction collection chamber (381), and the heavy fraction collection region (414) is mated to a heavy fraction collection chamber (382).
9. The apparatus of claim 1, wherein the apparatus comprises: the hot plate (310) is inside to be seted up cylindricality cambered surface (311), cylindricality cambered surface (311) with scrape and roll (350) phase-match, arrange material pipe (422) bottom and seted up a plurality of little round holes, light component condenser plate (371) and heavy component condenser plate (372) surface all are provided with a plurality of little cambered surfaces.
10. A process flow for the uninterrupted production of sucrose-6-ester, which is characterized in that the uninterrupted preparation equipment of sucrose-6-ester according to any one of claims 1 to 9 is adopted, and comprises the following steps:
s1: firstly, mixing a sucrose solution in a polar aprotic solvent;
s2: then, respectively inputting a sucrose solution dissolved in a polar aprotic solvent and an organotin acylation promoter into a mixing cylinder (210) from a liquid material inlet I (132) and a liquid material inlet II (133), driving a motor I (240) to rotate so as to drive a stirring device (200) and a molecular distillation device (300) to rotate, and mixing the sucrose solution and the organotin acylation promoter by a stirring rod (230) in the stirring device (200) when the stirring device (200) rotates;
s3: then the mixed liquid flows into a liquid separation disc (220) from a liquid outlet (211) on a mixing cylinder (210) after mixing is finished, the mixed liquid enters a liquid inlet pipe (320) on a molecular distillation device (300) from a liquid separation port (221) in the liquid separation disc (220), the mixed liquid is firstly sprayed to the surface of a heating plate (310) by a liquid spraying port (331) in a liquid spraying pipe (330) on the molecular distillation device (300) when the molecular distillation device (300) rotates to form a liquid film, and the liquid film of the mixed liquid starts to carry out a stannization reaction rapidly under the heating action of the heating plate (310) to generate a heavy component substance organotin sucrose complex and light component substance water;
s4: the secondary water is directly evaporated into gas to escape in the process of generation, and water molecules can move to a light component condensation plate (371) which is far away to be rapidly condensed into liquid drops and flow away along a cylindrical cambered surface (311) on the light component condensation plate (371);
s5: secondly, after the liquid spraying pipe (330) rotates ninety degrees, the scraping roller (350) on the upper fixing frame (340) rolls the reacted organotin sucrose complex to form a thinner liquid film, at the moment, the heavy component condensation plate (372) rotates, the organotin sucrose complex is quickly evaporated and moves to the heavy component condensation plate (372), and the organotin sucrose complex is condensed into liquid by the heavy component condensation plate (372), so that the completely dried organotin sucrose complex with low temperature is obtained;
s6: then the water molecules and the organotin sucrose complex molecules are condensed into liquid and flow out along the surface of the heavy component condensation plate (372), the liquid water molecules and the liquid organotin sucrose complex molecules are respectively collected by a light component collection cavity (381) and a heavy component collection cavity (382) in a liquid collection disc (380) and flow out from respective liquid leakage openings (383), the liquid water molecules flow into a moisture collection area (415) in the diverter disc (410) and flow out from a drain pipe (413), and the liquid organotin sucrose complex molecules also flow into a heavy component collection area (414) in the diverter disc (410) and flow out from an arc-shaped notch (414 a) on the liquid organotin sucrose complex molecules into a mixing tank (420);
s7: and finally, carboxylic anhydride is filled from a feeding pipe (421) on the mixing tank (420), flows to the mixing tank (420) from a plurality of small circular holes of a discharge pipe (422) in a trickle circular manner and is mixed with liquid organotin sucrose complex molecules, the mixed liquid flows onto the surface of a flow divider (431), the flow divider (431) is driven by a driving motor II (434) to uniformly disperse the liquid onto the inner surface of the reaction tank (430) through rotation, a liquid film is formed on the inner surface and reacts rapidly, and the sucrose-6-ester generated after the reaction is completed is discharged from a liquid discharge pipe (433).
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