CN112973164B - High-efficiency sucrose 6 ester continuous production equipment and method - Google Patents
High-efficiency sucrose 6 ester continuous production equipment and method Download PDFInfo
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- CN112973164B CN112973164B CN202110240102.0A CN202110240102A CN112973164B CN 112973164 B CN112973164 B CN 112973164B CN 202110240102 A CN202110240102 A CN 202110240102A CN 112973164 B CN112973164 B CN 112973164B
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- 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 field of sucrose 6 ester production, in particular to high-efficiency sucrose 6 ester continuous production equipment and a high-efficiency sucrose 6 ester continuous production method. It includes: the device comprises a tank body, heating equipment, cooling equipment, a mixing tank and a reaction tank; the tank body is provided with a vacuum port, a liquid inlet I, a liquid inlet II and a liquid outlet; the heating apparatus includes: the device comprises a support rod, a heating plate, a liquid distributor, a scraper and a driving motor I, wherein the support rod is fixed at the center of the cooling equipment. According to the invention, through the modification of molecular distillation equipment, all reaction processes can be completed in the equipment at one time, the whole production process of sucrose 6 ester and the time of each process can be shortened, the production efficiency is improved, and the problems of more processes and low production efficiency in the existing production technology are solved.
Description
Technical Field
The invention relates to the field of sucrose 6 ester production, in particular to high-efficiency sucrose 6 ester continuous production equipment and a high-efficiency sucrose 6 ester continuous 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 a relatively mature one, and the method for catalytically synthesizing sucrose 6 ester by using relatively mature organotin comprises the following steps: (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 is complex in flow, low in production efficiency and high in cost, and as the demand of sucralose gradually increases, the existing sucrose 6 ester preparation process and equipment cannot 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:
according to one aspect of the present invention, a high-efficiency sucrose 6 ester continuous production apparatus comprises: the device comprises a tank body, heating equipment, cooling equipment, a mixing tank and a reaction tank; the tank body is provided with a vacuum port, a liquid inlet I, a liquid inlet II and a liquid outlet;
the heating apparatus includes: the cooling device comprises a support rod, a heating plate, a liquid separator, a scraper and a first driving motor, wherein the support rod is fixed at the center of the cooling device, the heating plate is fixed on the support rod, a mixing tank body is also fixed on the upper end face of the heating plate, and the scraper is arranged in the mixing tank body; the liquid separator is fixedly arranged on the scraper, a first material collecting area and a second material collecting area are arranged in the liquid separator, the first material collecting area is positioned right below the first liquid material inlet outlet, and the second material collecting area is positioned right below the second liquid material inlet outlet; the driving motor drives the scraper and the liquid separator to rotate together in the mixing tank on the heating plate;
the cooling apparatus includes: a cooling ring and a water collecting sleeve; the lower end of the water collecting sleeve is connected with a drain pipe, and the cooling ring is fixed in the water collecting sleeve;
a disperser is arranged in the mixing tank, the lower end of the disperser is communicated with a feeding pipe, a helical blade is fixed on the circumferential surface of the outer end of the disperser, and a plurality of liquid spraying holes are formed in the upper end surface of the disperser;
the reaction tank is internally provided with a reaction core, one end of the reaction core is connected with a second driving motor fixed on the outer bottom surface of the tank body, the reaction core is rotatably arranged on the inner bottom surface of the tank body, and a plurality of square reaction holes are uniformly formed in the reaction core along the axial direction.
The invention also discloses a sucrose 6 ester continuous production method, which uses the high-efficiency sucrose 6 ester continuous production equipment of the first aspect and comprises the following specific steps:
s1: firstly, mixing a sucrose solution in a polar aprotic solvent;
s2: then, evacuating the air in the tank through a vacuum port to form negative pressure, and then driving a motor to drive a scraper and a liquid distributor to rotate together in the mixing tank on a heating plate;
s3: then, the sucrose solution and the organic tin acylation promoter dissolved in the polar aprotic solvent are respectively input into a first material collecting area and a second material collecting area in a liquid separator from a first liquid material inlet and a second liquid material inlet, then respectively enter into four pairs of liquid spraying pipes from the first material collecting area and the second material collecting area, then under the rotating action of the liquid separator, the sucrose solution and the organic tin acylation promoter can be uniformly sprayed on the inner wall of the mixing tank body by the four pairs of liquid spraying pipes, and the first liquid spraying pipe and the second liquid spraying pipe are vertically arranged, so that the sucrose solution sprayed by the first liquid spraying pipe and the sucrose solution sprayed by the second liquid spraying pipe fall on the inner wall of the mixing tank body and are primarily mixed in the falling process, and the primarily mixed liquid is secondarily mixed under the scraping action of a cross plate on a scraper plate;
s4: then the mixture flows into a reaction notch on the heating plate to form a mixed liquid film, and the mixed liquid film starts to carry out the tinning reaction rapidly under the heating action of the heating plate to generate a heavy component substance organotin sucrose complex and a light component substance water;
s5: then, water is directly evaporated into gas in the generation process and escapes from the reaction notch, water molecules directly move to the surface of each angular section ring a on the inner surface of a light component condensation area in the cooling equipment, are rapidly condensed into liquid drops and flow to drain troughs at four positions along the angular section rings, flow to a water collecting sleeve through the drain troughs and finally are drained from the drain pipes;
s6: then the gaseous heavy component substance organotin sucrose complex can not reach the inner surface of the light component condensation area due to smaller molecular mean free path, then can move to the surface of the heavy component condensation area under the action of gravity, is condensed into liquid by the surface of the heavy component condensation area to obtain the completely dry organotin sucrose complex with lower temperature, then flows to the heavy component collection area along the surface of the heavy component condensation area, and finally flows into a mixing tank in a smaller water flow dispersion mode from a plurality of liquid leakage ports;
s7: and finally, carboxylic anhydride flows into a feeding pipe of a disperser in a mixing tank and is sprayed out in a form of thin flow from a plurality of small circular liquid spraying holes at the top of the disperser to form convective mixing with organotin sucrose complex liquid molecules leaked from a liquid leakage port, the carboxylic anhydride and the organotin sucrose complex liquid molecules are mixed and then spirally flow out from the surface of a spiral blade on the circumferential end part of the disperser, at the moment, a second driving motor drives a reaction core to rotate, so that the liquid flowing out of the mixing tank can uniformly flow into each square reaction hole in the reaction core, a liquid film is formed on the surface of each square reaction hole and reacts rapidly, and the sucrose 6 ester generated after the reaction is completed is discharged from a liquid discharge pipe in a lower tank body.
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 evaporated steam out of an evaporation cavity for condensation, and water 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 a light component condensation area of a condensation ring to be condensed into liquid and then do not return to a mixed liquid film, so that the real-time distillation of the water molecules can be realized, the generated water can be timely removed when the stannization reaction of the sucrose solution on the heating plate 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 stannization reaction is completely dry and the temperature is reduced when the organotin sucrose complex solution is condensed into liquid through the heavy component condensation zone on the cooling ring, and the reaction can be carried out in the third step at once;
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 water molecules can be removed only by forming a certain temperature difference between the heating plate and the cooling ring, so that the energy consumption of the whole equipment is low;
7. through a first liquid spraying pipe and a second liquid spraying pipe which are arranged up and down in the liquid separator, the organic tin acylation promoter and the sucrose solution are simultaneously sprayed on the inner wall of the mixing tank body and are preliminarily mixed in the falling process, and the liquid after preliminary mixing is secondarily mixed under the scraping action of a cross plate on a scraper, so that the mixing effect of the organic tin acylation promoter and the sucrose solution is better;
8. the first reaction mixture is mixed in advance before being heated, then the first reaction mixture is heated on the heating plate and directly reacts, and the heating plate simultaneously completes the heating required by the reaction of the first reaction mixture and the heating required by the 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;
9. 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;
10. the heating plate is divided into a plurality of reaction notches, 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 reaction notches with 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 by increasing the heating area;
11. the inner surface of the light component condensation area in the cooling ring is formed by sequentially arranging a plurality of angular section rings along the axial direction, so that the surface area of the light component condensation area is increased, the condensation area of light and heavy component gas contacting the light and heavy component gas is large, the condensation effect is better, and the liquid condensed on each angular section ring can directly flow out through the drainage groove, so that the condensation efficiency is improved;
12. the angular section ring on the light component condensation area is inclined to the inner surface of the light component condensation area, and can reflect heat radiation generated on the heating plate to a certain degree so as to reduce the influence of the heat radiation on the light component condensation area and reduce energy consumption;
13. a light component condensation area and a heavy component condensation area in the cooling ring share one set of cooling system, so that the cooling cost is reduced;
14. the carboxylic anhydride is sprayed out from a plurality of small circular liquid spraying holes on the disperser in a trickle mode, forms convection mixing with liquid molecules of the organotin sucrose complex leaked from the liquid leakage port, spirally flows out from the upper surface of a spiral blade on the circumferential end part of the disperser after mixing, and replaces the traditional stirring and mixing by arranging the convection mixing and the spiral flowing mixing, so that the mixing effect of the solution can be improved, and the reaction speed of the carboxylic anhydride and the organotin sucrose complex is accelerated;
15. the reaction core is divided into a plurality of square reaction holes, the contact area of the carboxylic anhydride and the organic tin sucrose complex is increased by the square reaction holes, and the liquid flowing out of the mixing tank can uniformly flow into each square reaction hole in the reaction core and form a liquid film on the surface of the reaction core, so that the reaction speed of the carboxylic anhydride and the organic tin sucrose complex is higher, the reaction time is shortened, and the reaction efficiency is improved.
Drawings
FIG. 1 is a schematic view of the overall structure of a high-efficiency continuous production apparatus for sucrose 6 ester according to the present invention.
FIG. 2 is a schematic diagram of a half-section of the overall structure of a high-efficiency continuous production apparatus for sucrose 6 ester according to the present invention.
FIG. 3 is a schematic structural decomposition diagram of a heating apparatus in a high-efficiency sucrose 6 ester continuous production apparatus according to the present invention.
FIG. 4 is a front view, a half-section and a partially enlarged view of a high-efficiency continuous sucrose 6 ester production apparatus according to the present invention.
FIG. 5 is a side view, a half-section and a partially enlarged view of a high-efficiency continuous production apparatus for sucrose 6 ester according to the present invention.
Fig. 6 is a sectional view taken along line a-a of fig. 5.
Description of the drawings:
100. a tank body; 110. a lower tank body; 111. a liquid discharge pipe; 120. feeding the tank body; 121. a liquid material inlet I; 122. a liquid material inlet II; 130. a can lid; 131. a vacuum port; 200. a heating device; 210. a support bar; 220. heating plates; 221. a reaction tank opening; 222. a mixing tank body; 230. a liquid separator; 231. a liquid spraying pipe; 231a and a first liquid spraying pipe; 231b, a second liquid spraying pipe; 232. a first material collecting region; 233. a second material collecting area; 240. a squeegee; 241. a cross plate; 242. a connecting rod; 250. driving a motor I; 300. a cooling device; 310. a cooling ring; 311. a light component condensation zone; 311a, angular cross-sectional ring; 311b, a drain tank; 312. a heavies condensing zone; 313. a heavies collection zone; 313a, a liquid leakage port; 314. a baffle plate; 316. a first condensing chamber; 315. a second condensation chamber; 317. A communication port; 320. a water collecting sleeve; 321. a drain pipe; 330. a condensing input pipe; 340. a condensation output pipe; 400. a mixing tank; 410. a disperser; 411. a helical blade; 412. a liquid ejection hole; 413. a feed pipe; 500. a reaction tank; 510. a reaction core; 511. a square reaction hole; 520. 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 FIG. 1, a high-efficiency continuous production apparatus for sucrose 6 ester comprises a tank body 100, a heating apparatus 200, a cooling apparatus 300, a mixing tank 400, and a reaction tank 500;
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, the tank cover 130 is provided with a vacuum port 131, the upper tank 120 is provided with a first liquid inlet 121 and a second liquid inlet 122, and the bottom of the lower tank 110 is provided with a drain pipe 111;
as shown in fig. 2 to 6, the heating apparatus 200 includes: the heating device comprises a supporting rod 210, a heating plate 220, a liquid distributor 230, a scraper 240 and a first driving motor 250, wherein the supporting rod 210 is fixed at the center of the cooling device 300, the whole heating plate 220 is cylindrical and is fixedly installed on the supporting rod 210, a plurality of reaction notches 221 which completely penetrate through the heating plate 220 and are uniformly arranged along the circumferential direction are formed in the end face of the heating plate 220 along the axial direction of the cylinder, a heating resistance wire is arranged in the heating plate 220 and can heat the heating plate 220, a mixing tank body 222 is also fixed on the upper end face of the heating plate 220, the scraper 240 is composed of a cross plate 241 and a connecting rod 242, one end of the connecting rod 242 is fixedly connected with the cross plate 241, the other end of the connecting rod 242 is fixedly connected with the first driving motor 250 installed on the tank cover 130, the scraper 240 is integrally installed in the mixing tank body 222, the cross plate 241 can be contacted with the bottom of the mixing tank body 222, the liquid distributor 230 is integrally and fixedly installed on the cross plate 241 on the scraper 240, the liquid distributor 230 is internally provided with a first material collecting area 232 and a second material collecting area 233, the first material collecting area 232 is positioned right below the outlet of the first liquid inlet 121 on the upper tank body 120, the second material collecting area 233 is positioned right below the outlet of the second liquid inlet 122 on the upper tank body 120, four pairs of liquid spraying pipes 231 are uniformly and symmetrically arranged on the circumferential surface of the liquid distributor 230 along the circumferential direction, each pair of liquid spraying pipes 231 consists of a first liquid spraying pipe 231a and a second liquid spraying pipe 231b which are arranged up and down along the axial direction of the liquid distributor 230, wherein the first liquid spraying pipe 231a can be communicated with the first material collecting area 232, the second liquid spraying pipe 231b can be communicated with the second material collecting area 233, the first driving motor 250 can drive the scraper 240 and the liquid distributor 230 to rotate together in the mixing tank body 222 on the heating plate 220, and the liquid flowing out from the first liquid inlet 121 and the second liquid inlet 122 can respectively enter the first material collecting area 232 and the second material collecting area 233 in the liquid distributor 230, then the liquid enters into four pairs of liquid spraying pipes 231 from the first material collecting area 232 and the second material collecting area 233 respectively, then under the rotating action of the liquid separator 230, the four pairs of liquid spraying pipes 231 can uniformly spray the liquid on the inner wall of the mixing tank body 222, because the first liquid spraying pipe 231a and the second liquid spraying pipe 231b are arranged up and down, the two liquids sprayed onto the inner wall of the mixing tank body 222 by the first liquid spraying pipe 231a and the second liquid spraying pipe 231b are mixed in the falling process, and the liquid after primary mixing enters into the reaction notch 221 in the heating plate 220 under the scraping action of the cross plate 241 on the scraping plate 240;
the cooling apparatus 300 includes: the cooling ring 310 and the water collecting sleeve 320, the water collecting sleeve 320 is a cylindrical shell structure and is fixedly installed in the upper tank body 120, the lower end of the water collecting sleeve 320 is connected with a drain pipe 321, the drain pipe 321 can be communicated with the inside of the water collecting sleeve 320, the cooling ring 310 is a truncated cone-shaped hollow shell structure and is fixedly installed in the water collecting sleeve 320, the inside of the shell of the cooling ring 310 is divided into a first condensing chamber 316 and a second condensing chamber 315 by a baffle 314 which is symmetrical to each other, the upper part of the baffle 314 is provided with a communication port 317, the first condensing chamber 316 and the second condensing chamber 315 can be communicated through the communication port 317, the inside of the cooling ring 310 can be sequentially divided into a light component condensing area 311, a heavy component condensing area 312 and a heavy component collecting area 313 from top to bottom, the inner surface of the light component condensing area 311 is formed by sequentially arranging a plurality of angular section rings 311a along the axial direction, the cooling ring 310 is provided with a plurality of drain grooves 311b sequentially arranged in the vertical direction on the circumference of the light component condensing area 311, one end of each drainage groove 311b can be communicated with the angular section ring 311a, the other end can be communicated with the water collecting sleeve 320, the inner surface of the heavy component condensation area 312 is a conical surface, the lower end of the heavy component condensation area 312 is provided with a heavy component collecting area 313, the lower end surface of the heavy component collecting area 313 is provided with a plurality of liquid leakage openings 313a which are uniformly distributed along the circumference, the outer surface of the cooling ring 310 close to the heavy component collecting area 313 is symmetrically provided with a condensation input pipe 330 and a condensation output pipe 340, wherein the condensation input pipe 330 is communicated with the first condensation chamber 316, the condensation output pipe 340 is communicated with the second condensation chamber 315, condensate enters the first condensation chamber 316 from the condensation input pipe 330, then enters the second condensation chamber 315 from the communication opening 317 and finally flows out from the condensation output pipe 340, the cooling ring 310 is cooled in the flowing process of the condensate, when gaseous light component substances move to the surface of each angular section ring 311a on the inner surface of the light component condensation area 311, the gaseous light component condensation area is cooled into liquid, then flows into the water collection jacket 320 through the drainage slot 311b and finally is drained from the drainage pipe 321, and the gaseous heavy component substance moves to the surface of the heavy component condensation area 312 under the action of gravity, then is condensed into liquid and flows to the heavy component collection area 313 along the surface, and finally flows out from the plurality of liquid leakage ports 313a in a small water flow dispersed mode;
a disperser 410 is arranged in the mixing tank 400, a feeding pipe 413 is arranged on the circumferential surface of the lower end of the disperser 410, the feeding pipe 413 can be communicated with the inside of the disperser 410, a helical blade 411 is fixed on the circumferential surface of the outer end of the disperser 410, a plurality of liquid spraying holes 412 uniformly distributed along the circumference are formed in the upper end surface of the disperser 410, reaction materials enter the disperser 410 from the feeding pipe 413, are sprayed out by a plurality of small dispersed water flows to form convective mixing with liquid leaked from a liquid leakage port 313a at the lower end of the cooling ring 310, and spirally flow out from the surface of the helical blade 411 on the circumferential end of the disperser 410 after mixing;
the reaction tank 500 contains a reaction core 510 therein, the reaction core 510 is a cylinder, and one end of the reaction core 510 can be connected with a second driving motor 520 fixed on the lower end of the lower tank 110 and can be rotatably mounted on the lower end surface of the lower tank 110, the reaction core 510 is uniformly provided with a plurality of square reaction holes 511 along the axial direction, when the second driving motor 520 rotates, the reaction core 510 is driven to rotate, so that the liquid flowing out of the mixing tank 400 can uniformly flow into each square reaction hole 511 inside the reaction core 510.
A sucrose 6 ester continuous production method uses the high-efficiency sucrose 6 ester continuous production equipment, and comprises the following specific steps:
s1: firstly, mixing a sucrose solution in a polar aprotic solvent;
s2: then, air in the tank is pumped out through the vacuum port 131 to form negative pressure, and then the first driving motor 250 drives the scraper 240 and the liquid distributor 230 to rotate together in the mixing tank 222 on the heating plate 220;
s3: then the sucrose solution and the organic tin acylation promoter dissolved in the polar aprotic solvent are respectively input into the first material collecting area 232 and the second material collecting area 233 in the liquid distributor 230 from the first liquid material inlet 121 and the second liquid material inlet 122, then respectively enters four pairs of liquid spraying pipes 231 from the first material collecting area 232 and the second material collecting area 233, then under the action of the rotation of the liquid distributor 230, the four pairs of liquid spraying pipes 231 can uniformly spray the sucrose solution and the organotin acylation promoter on the inner wall of the mixing tank 222, since the first liquid spraying tube 231a and the second liquid spraying tube 231b are disposed up and down, the organotin acylation promoter sprayed from the first liquid spraying tube 231a and the sucrose solution sprayed from the second liquid spraying tube 231b fall on the inner wall of the mixing tank 222, and the liquid is primarily mixed in the falling process, and the liquid after primary mixing is secondarily mixed under the scraping action of the cross plate 241 on the scraper 240;
s4: then flows into a reaction notch 221 on the heating plate 220 to form a mixed liquid film, and the mixed liquid film starts to perform a tinning reaction rapidly under the heating action of the heating plate 220 to generate a heavy component substance organotin sucrose complex and a light component substance water;
s5: then, the water is directly evaporated into gas in the process of generation and escapes from the reaction slot 221, and the water molecules directly move onto the surface of each of the angular section rings 311a on the inner surface of the light component condensation area 311 in the cooling device 300, and are rapidly condensed into liquid droplets and flow to the drain grooves 311b at four positions along the angular section rings 311a, flow into the water collecting jacket 320 through the drain grooves 311b, and finally are discharged from the drain pipe 321;
s6: then the gaseous heavy component substance organotin sucrose complex can not reach the inner surface of the light component condensation area 311 due to the small molecular mean free path, then moves to the surface of the heavy component condensation area 312 under the action of gravity, is condensed into liquid by the surface of the heavy component condensation area 312 to obtain the completely dry organotin sucrose complex with low temperature, then flows to the heavy component collection area 313 along the surface of the heavy component condensation area 312, and finally flows into the mixing tank 400 from a plurality of liquid leakage ports 313a in a small water flow dispersion mode;
s7: and finally, the carboxylic anhydride flows in from the feeding pipe 413 of the disperser 410 in the mixing tank 400 and is sprayed in a fine flow form from a plurality of small circular liquid spraying holes 412 at the top of the disperser 410 to form convective mixing with the liquid molecules of the organotin sucrose complex leaked from the liquid leakage port 313a, and the mixed carboxylic anhydride spirally flows out from the surface of the spiral blade 411 at the circumferential end of the disperser 410, at the moment, the second driving motor 520 drives the reaction core 510 to rotate, so that the liquid flowing out from the mixing tank 400 can uniformly flow into each square reaction hole 511 in the reaction core 510, a liquid film is formed on the surface of each square reaction hole 511 and reacts rapidly, and the sucrose 6 ester is formed after the reaction is completed and is discharged from the liquid discharge pipe 111 in the lower tank 110.
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 (8)
1. A high efficiency continuous sucrose 6 ester production facility comprising: the device comprises a tank body (100), a heating device (200), a cooling device (300), a mixing tank (400) and a reaction tank (500); the jar body (100) is gone up to have vacuum mouth (131), liquid material entry (121), liquid material entry two (122), leakage fluid dram, its characterized in that: the heating device (200) comprises: the cooling device comprises a support rod (210), a heating plate (220), a liquid distributor (230), a scraper (240) and a first driving motor (250), wherein the support rod (210) is fixed at the center of the cooling device (300), the heating plate (220) is fixed on the support rod (210), a mixing tank body (222) is further fixed on the upper end face of the heating plate (220), and the scraper (240) is installed inside the mixing tank body (222);
the liquid distributor (230) is fixedly arranged on the scraper (240), a first material collecting region (232) and a second material collecting region (233) are arranged in the liquid distributor (230), the first material collecting region (232) is positioned right below an outlet of the first liquid material inlet (121), and the second material collecting region (233) is positioned right below an outlet of the second liquid material inlet (122); the first driving motor (250) drives the scraper (240) and the liquid distributor (230) to rotate together in the mixing tank body (222) on the heating plate (220);
the cooling apparatus (300) comprising: a cooling ring (310), a water collection sleeve (320); the lower end of the water collecting sleeve (320) is connected with a water discharging pipe (321), and the cooling ring (310) is fixed in the water collecting sleeve (320);
a disperser (410) is arranged in the mixing tank (400), the lower end of the disperser (410) is communicated with a feeding pipe (413), a helical blade (411) is fixed on the circumferential surface of the outer end of the disperser (410), and a plurality of liquid spraying holes (412) are formed in the upper end surface of the disperser (410);
a reaction core (510) is accommodated in the reaction tank (500), one end of the reaction core (510) is connected with a second driving motor (520) fixed on the outer bottom surface of the tank body (100), the reaction core (510) is rotatably installed on the inner bottom surface of the tank body (100), and a plurality of square reaction holes (511) are uniformly formed in the reaction core (510) along the axial direction;
the interior of the cooling ring (310) is sequentially divided into a light component condensation area (311), a heavy component condensation area (312) and a heavy component collection area (313) from top to bottom, and the inner surface of the light component condensation area (311) is formed by sequentially arranging a plurality of angular section rings (311 a) along the axial direction.
2. The high-efficiency continuous sucrose 6 ester production apparatus according to claim 1, wherein: the tank body (100) is composed of a lower tank body (110), an upper tank body (120) and a tank cover (130) which are connected with each other respectively, one of the lower tank body, the upper tank body and the tank cover is disassembled when necessary so as to be convenient for installation and maintenance, and a plurality of reaction notches (221) which completely penetrate through and are uniformly arranged along the circumferential direction are formed in the end surface of the heating plate (220) along the axial direction of a cylinder.
3. The high-efficiency sucrose 6 ester continuous production apparatus as claimed in claim 2, wherein: the scraper (240) consists of a cross plate (241) and a connecting rod (242), one end of the connecting rod (242) is fixedly connected with the cross plate (241), the other end of the connecting rod is fixedly connected with a first driving motor (250) installed on the tank cover (130), and the cross plate (241) is contacted with the bottom of the mixing tank body (222).
4. The high-efficiency sucrose 6 ester continuous production apparatus as claimed in claim 3, wherein: four pairs of liquid spraying pipes (231) are uniformly and symmetrically arranged on the circumferential surface of the liquid distributor (230) along the circumferential direction, each pair of liquid spraying pipes (231) consists of a first liquid spraying pipe (231 a) and a second liquid spraying pipe (231 b) which are arranged up and down along the axial direction of the liquid distributor (230), the first liquid spraying pipe (231 a) can be communicated with the first material collecting area (232), and the second liquid spraying pipe (231 b) can be communicated with the second material collecting area (233).
5. The high-efficiency sucrose 6 ester continuous production apparatus as claimed in claim 4, wherein: the liquid flowing out of the first liquid inlet (121) and the second liquid inlet (122) respectively enters a first material collecting area (232) and a second material collecting area (233) in the liquid separator (230), the interior of the shell of the cooling ring (310) is divided into a first condensing chamber (316) and a second condensing chamber (315) by baffles (314) which are symmetrical to each other, the upper part of each baffle (314) is provided with a communicating opening (317), and the first condensing chamber (316) is communicated with the second condensing chamber (315) through the communicating opening (317).
6. The high-efficiency continuous sucrose 6 ester production apparatus according to claim 5, wherein: the cooling ring (310) is provided with a plurality of water drainage grooves (311 b) which are sequentially arranged in the vertical direction on the circumference of the light component condensation area (311), one end of each water drainage groove (311 b) is communicated with the angular section ring (311 a), the other end of each water drainage groove is communicated with the water collection sleeve (320), the inner surface of the heavy component condensation area (312) is a conical surface, the lower end of the heavy component condensation area (312) is provided with a heavy component collection area (313), and the lower end surface of the heavy component collection area (313) is provided with a plurality of liquid leakage openings (313 a) which are uniformly distributed along the circumference.
7. The high-efficiency sucrose 6 ester continuous production apparatus as claimed in claim 6, wherein: and a condensation input pipe (330) and a condensation output pipe (340) are symmetrically arranged on the outer surface of the cooling ring (310) close to the heavy component collecting region (313), the condensation input pipe (330) is communicated with the first condensing chamber (316), and the condensation output pipe (340) is communicated with the second condensing chamber (315).
8. A high-efficiency sucrose 6 ester continuous production method is characterized in that: the high-efficiency sucrose 6 ester continuous production equipment according to any one of claims 1 to 7 is used, and comprises the following specific steps:
s1: firstly, mixing a sucrose solution in a polar aprotic solvent;
s2: then, air in the tank is pumped out through a vacuum port (131) to form negative pressure, and then a first driving motor (250) drives a scraper (240) and a liquid distributor (230) to rotate together in a mixing tank body (222) on a heating plate (220);
s3: then, the sucrose solution and the organic tin acylation promoter dissolved in the polar aprotic solvent are respectively input into a first material collecting area (232) and a second material collecting area (233) in a liquid divider (230) from a first material inlet (121) and a second material inlet (122), then respectively enter into four pairs of liquid spraying pipes (231) from the first material collecting area (232) and the second material collecting area (233), then under the rotation action of the liquid divider (230), the four pairs of liquid spraying pipes (231) can uniformly spray the sucrose solution and the organic tin acylation promoter on the inner wall of a mixing tank body (222), because the first liquid spraying pipe (231 a) and the second liquid spraying pipe (231 b) are arranged up and down, the sucrose solution sprayed by the first liquid spraying pipe (231 a) and the sucrose solution sprayed by the second liquid spraying pipe (231 b) fall on the inner wall of the mixing tank body (222) and are preliminarily mixed in the falling process, the liquid after primary mixing is subjected to secondary mixing under the scraping action of a cross plate (241) on a scraper (240);
s4: then flows into a reaction notch (221) on the heating plate (220) to form a mixed liquid film, and the mixed liquid film starts to carry out a tinning reaction rapidly under the heating action of the heating plate (220) to generate a heavy component substance organotin sucrose complex and a light component substance water;
s5: then the water is directly evaporated into gas in the process of generation and escapes from the reaction slot (221), water molecules directly move to the surface of each angular section ring (311 a) on the inner surface of the light component condensation area (311) in the cooling device (300), and are rapidly condensed into liquid drops and flow to drain grooves (311 b) at four positions along the angular section ring (311 a), flow to the water collecting sleeve (320) through the drain grooves (311 b), and finally are drained from a drain pipe (321);
s6: then the gaseous heavy component substance organotin sucrose complex can not reach the inner surface of the light component condensation area (311) because the molecular mean free path is smaller than that of the light component, then moves to the surface of the heavy component condensation area (312) under the action of gravity, is condensed into liquid by the surface of the heavy component condensation area (312) to obtain the organotin sucrose complex which is completely dry and lower than the evaporation temperature, then flows to the heavy component collection area (313) along the surface of the heavy component condensation area (312), and finally dispersedly flows into the mixing tank (400) from a plurality of liquid leakage ports (313 a);
s7: and finally, the carboxylic anhydride flows into a feeding pipe (413) of a disperser (410) in a mixing tank (400) and is sprayed in a fine flow form from a plurality of small circular liquid spraying holes (412) at the top of the disperser (410) to form convective mixing with the liquid molecules of the organotin sucrose complex leaked from a liquid leakage port (313 a), the mixed liquid spirally flows out from the surface of a spiral blade (411) at the circumferential end part of the disperser (410), at the moment, a driving motor II (520) drives a reaction core (510) to rotate, so that the liquid flowing out from the mixing tank (400) can uniformly flow into each square reaction hole (511) in the reaction core (510), forms and rapidly reacts on the surface of each square reaction hole (511), and the liquid film 6 ester of the sucrose is formed after the reaction is completely discharged from a liquid discharge pipe (111) in a lower tank body (110).
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| US20230322836A1 (en) * | 2021-02-19 | 2023-10-12 | Anhu Jinhe Industrial Co., Ltd. | Device and method for preparing sucrose-6-ester |
| CN116077962B (en) * | 2023-02-16 | 2023-08-29 | 黑龙江优贝康乳业有限公司 | Drying device for milk powder production and drying process thereof |
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