CN112933635B - Surrounding centrifugal type sucrose-6-ester continuous production equipment and production method - Google Patents
Surrounding centrifugal type sucrose-6-ester continuous production equipment and production method Download PDFInfo
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- CN112933635B CN112933635B CN202110241297.0A CN202110241297A CN112933635B CN 112933635 B CN112933635 B CN 112933635B CN 202110241297 A CN202110241297 A CN 202110241297A CN 112933635 B CN112933635 B CN 112933635B
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- 238000010924 continuous production Methods 0.000 title claims abstract description 11
- 238000004519 manufacturing process Methods 0.000 title abstract description 17
- 238000003756 stirring Methods 0.000 claims abstract description 54
- 238000004821 distillation Methods 0.000 claims abstract description 44
- 238000005192 partition Methods 0.000 claims abstract description 34
- 238000000199 molecular distillation Methods 0.000 claims abstract description 28
- 230000005540 biological transmission Effects 0.000 claims abstract description 26
- 238000006243 chemical reaction Methods 0.000 claims abstract description 23
- 239000007788 liquid Substances 0.000 claims description 189
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 62
- 238000002156 mixing Methods 0.000 claims description 54
- 238000009833 condensation Methods 0.000 claims description 42
- 230000005494 condensation Effects 0.000 claims description 42
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims description 37
- 229930006000 Sucrose Natural products 0.000 claims description 37
- 239000005720 sucrose Substances 0.000 claims description 37
- 238000000034 method Methods 0.000 claims description 20
- 239000011344 liquid material Substances 0.000 claims description 18
- 238000010079 rubber tapping Methods 0.000 claims description 16
- 238000001816 cooling Methods 0.000 claims description 12
- 239000000126 substance Substances 0.000 claims description 12
- 238000003860 storage Methods 0.000 claims description 10
- 230000010933 acylation Effects 0.000 claims description 9
- 238000005917 acylation reaction Methods 0.000 claims description 9
- 239000003880 polar aprotic solvent Substances 0.000 claims description 8
- 238000005507 spraying Methods 0.000 claims description 7
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 6
- 150000001244 carboxylic acid anhydrides Chemical class 0.000 claims description 4
- 238000005485 electric heating Methods 0.000 claims description 4
- 230000000694 effects Effects 0.000 claims description 3
- 238000009434 installation Methods 0.000 abstract description 6
- 238000012423 maintenance Methods 0.000 abstract description 3
- 238000011144 upstream manufacturing Methods 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 description 15
- 239000011541 reaction mixture Substances 0.000 description 6
- 239000004376 Sucralose Substances 0.000 description 4
- 239000000110 cooling liquid Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- BAQAVOSOZGMPRM-QBMZZYIRSA-N sucralose Chemical compound O[C@@H]1[C@@H](O)[C@@H](Cl)[C@@H](CO)O[C@@H]1O[C@@]1(CCl)[C@@H](O)[C@H](O)[C@@H](CCl)O1 BAQAVOSOZGMPRM-QBMZZYIRSA-N 0.000 description 4
- 235000019408 sucralose Nutrition 0.000 description 4
- 238000007599 discharging Methods 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- 208000032370 Secondary transmission Diseases 0.000 description 1
- 239000008122 artificial sweetener Substances 0.000 description 1
- 235000021311 artificial sweeteners Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000007036 catalytic synthesis reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 235000003599 food sweetener Nutrition 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000001802 infusion Methods 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000003765 sweetening agent Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
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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
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F33/00—Other mixers; Mixing plants; Combinations of mixers
- B01F33/80—Mixing plants; Combinations of mixers
- B01F33/81—Combinations of similar mixers, e.g. with rotary stirring devices in two or more receptacles
- B01F33/811—Combinations of similar mixers, e.g. with rotary stirring devices in two or more receptacles in two or more consecutive, i.e. successive, mixing receptacles or being consecutively arranged
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
-
- 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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- Organic Chemistry (AREA)
- Biotechnology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Genetics & Genomics (AREA)
- Molecular Biology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
- Mixers Of The Rotary Stirring Type (AREA)
- Saccharide Compounds (AREA)
Abstract
The invention relates to the technical field of molecular distillation, in particular to a surrounding centrifugal type sucrose-6-ester continuous production device and a production method, which comprises the following steps: the tank body is composed of a main tank and a tank cover which are connected with each other, the tank cover can be detached for convenient installation and maintenance during installation or detachment, the tank cover is provided with a driving motor, the tank cover is also provided with a vacuum port, three drain pipes are uniformly distributed on the circumferential surface of the main tank, an upper partition plate, a middle partition plate and a lower partition plate are sequentially arranged on the inner wall of the main tank from top to bottom, the three partition plates divide the inner part of the whole main tank into a main transmission chamber, a stirring chamber, a distillation chamber and an auxiliary transmission chamber, the invention improves molecular distillation equipment, all reaction processes for preparing the sucrose-6-ester can be completed in the reactor at one time, so that the reaction process and the connection time of the upstream and downstream are shortened, and the production efficiency of the sucrose-6-ester is greatly improved.
Description
Technical Field
The invention relates to the field of sucrose-6-ester production, in particular to a surrounding centrifugal type sucrose-6-ester continuous production device 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 surrounding centrifugal sucrose-6-ester continuous production device comprises a tank body, a main transmission chamber, a stirring chamber, a distillation chamber, an auxiliary transmission chamber and a driving motor;
the tank body is formed by connecting a main tank and a tank cover, the tank cover can be detached during installation or detachment to facilitate installation and maintenance, a driving motor is installed on the tank cover, a vacuum port is further formed in the tank cover and can pump air out of the tank, three drain pipes are uniformly distributed on the circumferential surface of the main tank, an upper partition plate, a middle partition plate and a lower partition plate are sequentially installed on the inner wall of the main tank from top to bottom, and the three partition plates enable the inner part of the whole main tank to be a main transmission chamber, a stirring chamber, a distillation chamber and an auxiliary transmission chamber;
the main transmission chamber comprises a main shaft, a driving gear, driven gears and rotating shafts, the upper end of the main shaft is connected with a driving motor on the tank cover, the driving gear is fixedly arranged in the middle of the main shaft, stirring paddles are further arranged at the lowest end of the main shaft, the three rotating shafts are uniformly and rotatably arranged on the upper partition plate, the driven gears are arranged at the upper ends of the rotating shafts and can be connected with the driving gear on the main shaft;
a mixing drum is fixedly arranged in the mixing chamber, a first liquid material inlet and a second liquid material inlet are symmetrically arranged on the circumferential surface of the mixing drum close to the lower end, the first liquid material inlet and the second liquid material inlet can be communicated with the interior of the mixing drum, and a mixing paddle at the lower end of a main shaft in the main transmission chamber is positioned in the mixing chamber;
the distillation chamber comprises: the condenser, the centrifuge, the condenser pipe, the inlet pipe, the finished product connects the liquid disc, mix the rotary table, a condenser and a centrifuge are arranged up and down and made up into a single molecule distillation system, the distillation chamber is the double molecule distillation system that two single molecule distillation systems are arranged up and down and made up, the condenser is made up of condensation disc, light component connects the liquid disc and fixed mount, fix on median septum through the fixed mount wholly, the quantity of condensation disc is three and mount on fixed mount evenly, the inside of condensation disc is the hollow structure and has cooling chamber, the internal surface of condensation disc is the circular conical surface, and have multiple water collecting troughs evenly arranged along the circumference on the circular conical surface, there are liquid inlet pipes on the outer circumference of condensation disc, the liquid inlet pipe can communicate with cooling chamber inside the condensation disc, the light component connects the liquid disc for the circular ring form and suits the bottom end of condensation disc, there is annular catchment notch in the light component connects the liquid disc, the outer circumferential surface of the light component liquid receiving disc is provided with a water outlet pipe, the water collecting notch can be communicated with the water outlet pipe, and the water outlet pipe can be communicated with a water outlet pipe on the main tank;
the centrifuge consists of a recombined tapping liquid disc, centrifugal discs and connecting pipes, wherein the recombined tapping liquid disc is of a three-ring structure, each ring is provided with a liquid collecting notch, the centrifugal discs are three in number and rotatably arranged in the three rings of the recombined tapping liquid disc respectively, the inner surface of each centrifugal disc is a conical surface, heating wires capable of heating are arranged in the centrifugal discs, the connecting pipes are fixedly arranged in the centers of the recombined tapping liquid discs, the connecting pipes are provided with liquid outlets on the circumferential surfaces of the positions of the liquid collecting notches on the rings of the recombined tapping liquid discs, the liquid outlets can enable liquid collected by the liquid collecting notches on the rings to flow into the connecting pipes, and the centrifuge can be connected with a condenser through the connecting pipes;
the rotating shaft in the main transmission chamber can penetrate through each centrifugal disc in the double-molecular distillation system and is fixedly connected with each centrifugal disc, the interior of the rotating shaft is hollow, a liquid inlet is formed in the circumferential part at the bottom end of the stirring chamber, a liquid spraying port is formed in the circumferential part at the inner bottom end of the centrifuge in each single-molecular distillation system in the distillation chamber, and liquid can enter the interior of the rotating shaft from the liquid inlet in the stirring chamber and flow onto the inner conical surface of each centrifuge from the interior of the rotating shaft;
the condenser pipe is arranged in a connecting pipe of two monomolecular distillation systems which are arranged up and down, the outer surface of the condenser pipe positioned in the bimolecular distillation system is provided with a helical blade, the condenser pipe can be communicated with a liquid inlet pipe on the condenser of each monomolecular distillation system, and when cooling liquid flows into the condenser pipe, the cooling liquid flows through the condenser pipe to cool the helical blade and simultaneously flows into each condensation disc in each monomolecular distillation system to cool the condensation disc;
the feeding pipe is arranged on a connecting pipe of a centrifugal disc in the single molecular distillation system below the double molecular distillation system and can be communicated with the inside of the connecting pipe;
the finished product liquid receiving disc is of an annular disc structure, a liquid storage tank is arranged in the finished product liquid receiving disc, the finished product liquid receiving disc is integrally and fixedly installed on the lower partition plate, a liquid outlet pipe is arranged on the lower end face of the finished product liquid receiving disc and can be communicated with the liquid storage tank in the finished product liquid receiving disc, a mixing rotary disc is rotatably installed in the finished product liquid receiving disc, the upper half inner surface of the mixing rotary disc is a conical surface, the lower half inner surface of the mixing rotary disc is a cylindrical surface, a plurality of stirring rods are uniformly arranged on the inner cylindrical surface, and a connecting pipe of a centrifugal disc in a lower monomolecular distillation system in the bimolecular distillation system is also positioned in the inner cylindrical surface;
the auxiliary transmission chamber is internally provided with a first gear and a second gear, the first gear is installed on the lower cylindrical surface of the finished product liquid receiving disc, the second gear is installed on the three rotating shafts, and the first gear can be meshed with the second gear simultaneously, so that the first gear rotates when the second gear rotates to drive the mixing turntable to rotate, the mixing turntable rotates to drive the stirring rod to rotate, the mixed liquid is stirred, and the uniformly mixed liquid is thrown out from the upper semi-conical surface of the mixing turntable in the form of a liquid film.
In another aspect, the invention provides a continuous process for the production of sucrose-6-ester by the surrounding centrifugal process, comprising the steps of:
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 stirring cylinder in a stirring chamber from a liquid material inlet I and a liquid material inlet II, and mixing the sucrose solution and the organic tin acylation promoter under the rotation of a stirring paddle on a main shaft;
s3: then the mixed liquid overflows from an opening above the mixing drum and flows onto a middle partition plate, then the mixed liquid on the middle partition plate enters the interior of each rotating shaft from a liquid inlet on each rotating shaft and is discharged into a centrifugal disc in each centrifuge in a double molecular distillation system from two liquid spraying ports on each rotating shaft, the mixed liquid is expanded on a conical surface under the action of centrifugal force under the high-speed rotation action of the centrifugal disc to form a thin liquid film, and meanwhile, the liquid film of the mixed liquid is heated by an electric heating wire in the centrifugal disc and starts to carry out fast stannization reaction to generate an organotin sucrose complex compound with heavy components and substance water with light components;
s4: the secondary water is directly evaporated into gas and moves upwards in the generation process, water molecules directly move to the conical surface of the condensation disc of the condenser, are rapidly condensed into liquid drops under the cooling action of the condensation disc, are converged into liquid flow in the water collecting tank on the inner conical surface of the condensation disc, flow to the water collecting tank opening in the light component liquid collecting disc below the condensation disc along the water collecting tank, and finally flow to the water discharging pipe from the water discharging pipe to be discharged by the water discharging pipe;
s5: secondly, the gaseous heavy component substance organotin sucrose complex cannot reach the inner conical surface of the condensation disc due to the small average free path of molecules and can return to the mixed liquid on the centrifugal disc, then the liquid heavy component substance organotin sucrose complex can be thrown into a liquid collecting notch in the heavy component liquid disc under the action of the centrifugal force of the centrifugal disc, and finally the liquid heavy component substance organotin sucrose complex flows into the connecting pipe through a liquid outlet on the connecting pipe, and the liquid heavy component substance organotin sucrose complex in the connecting pipe continuously flows downwards along the spiral blade on the surface of the condensation pipe, is cooled in the flowing process, and finally flows into a mixing turntable below to obtain the completely dried organotin sucrose complex with lower temperature;
s6: and finally, the carboxylic anhydride liquid enters the mixing turntable from the feeding pipe, is mixed under the stirring action of the stirring rod on the lower semi-cylindrical surface of the mixing turntable, moves to the upper semi-conical surface of the mixing turntable after being mixed, is expanded to form a thin liquid film on the upper semi-conical surface under the centrifugal action of the mixing turntable, reacts quickly, generates sucrose-6-ester after the reaction is completed, is thrown into a liquid storage tank in a finished product liquid receiving disc from the surface of the upper semi-conical surface of the mixing turntable, and is discharged from a liquid outlet pipe.
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 inner surface of the condensation disc after escaping from the liquid surface and are condensed into liquid, and then the liquid molecules do not return to the mixed liquid film, 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 removed in time, the solution does not contain water, the stannization reaction can be carried out more favorably, and the stannization reaction efficiency is improved;
4. the organotin sucrose complex solution generated by the stannation reaction can be cooled through the helical blades on the condensing tube in the flowing process of the organotin sucrose complex solution in the connecting tube, and can enter the third step for reaction immediately after being cooled, so that the temperature is reduced in the flowing process, 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 in a centrifugal disc on the centrifuge, 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 centrifugal disc and the condensing disc, so that the energy consumption of the whole equipment is low;
7. the sucrose solution and the organic tin acylation promoter enter from the lower part of the stirring cylinder and are mixed under the rotation of the stirring paddle, and the mixed liquid overflows from an opening on the upper part of the stirring cylinder, so that the mixing effect of the organic tin acylation promoter and the sucrose solution is better;
8. the heating wire on the centrifugal disc 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 wire, 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 centrifugal disc is short, and the temperature of the centrifugal disc is low, so that sugar is prevented from being decomposed at high temperature to reduce impurities in the solution;
11. the centrifugal device is provided with a plurality of centrifugal discs, the corresponding condenser is provided with a plurality of condensing discs, one centrifugal disc and one condensing disc can form a molecular distillation system, one centrifugal device and one condenser can simultaneously form three molecular distillation systems, and two pairs of centrifugal devices and condensers are arranged in the distillation chamber, so that six molecular distillations can be simultaneously carried out, the reaction amount in unit time is more, and the yield is greatly improved;
13. the liquid film formed by the centrifugal process is thinner and more uniform, so that the heating time of the material is shorter, the heating rate and the separation efficiency are higher, the thermal decomposition rate of the heat-sensitive material is lower, the material treatment capacity is increased, and the method is more suitable for industrial continuous production;
14. the condensing pipe cools the helical blades and simultaneously flows into each condensing disc in each monomolecular distillation system to cool the condensing discs, and the material cooling and light component condensation share one condensing system, so that one condensing system is omitted, and the energy consumption and the cost are saved;
15. the mixing turntable is divided into an upper area and a lower area, a stirring rod arranged in the lower half area can stir the mixed liquid, a conical surface is arranged in the upper half area, the mixed liquid can be expanded on the conical surface under the centrifugal action of the mixing turntable to form a thin liquid film, and the mixed liquid in a liquid film state can react rapidly, so that the production efficiency of the whole sucrose-6-ester is improved;
16. the mixed liquid enters each centrifugal disc from the inside of each rotating shaft, the internal space of the rotating shaft is fully utilized, an independent infusion tube is cut, the structure is simplified, and the cost is reduced.
Drawings
Fig. 1 is a schematic view of the overall structure of the present invention.
Fig. 2 is a top view of the overall structure of the present invention.
Fig. 3 is a cross-sectional view taken along line a-a of fig. 2 in accordance with the present invention.
Fig. 4 is a cross-sectional view taken along line D-D of fig. 3 in accordance with the present invention.
Fig. 5 is a cross-sectional view taken along line B-B of fig. 2 in accordance with the present invention.
FIG. 6 is a schematic view showing the structural decomposition of the molecular distillation system of the present invention.
Fig. 7 is a schematic structural view of a condenser in the present invention.
Fig. 8 is a cross-sectional view taken along line C-C of fig. 2 in accordance with the present invention.
Fig. 9 is a schematic structural view of the present invention with the casing and the upper partition removed as a whole.
Description of the drawings:
100. a tank body; 110. a main tank; 110a, a drain pipe; 111. an upper partition plate; 112. a middle partition plate; 113. a lower partition plate; 120. a can lid; 121. a vacuum port; 200. a main transmission chamber; 210. a main shaft; 211. a stirring paddle; 220. a driving gear; 230. a driven gear; 240. a rotating shaft; 241. a liquid inlet; 242. a liquid spraying port; 300. a stirring chamber; 310. a mixing drum; 320. a liquid material inlet I; 330. a liquid material inlet II; 400. a distillation chamber; 410. a condenser; 411. a condensation pan; 411a, a water collecting tank; 411b, a cooling chamber; 411c, a liquid inlet pipe; 412. the light component is connected with a liquid tray; 412a, a water collection slot; 412b, a water outlet pipe; 413. a fixed mount; 420. a centrifuge; 421. recombining the tapping liquid discs; 421a, a liquid collecting notch; 422. a centrifugal pan; 423. a connecting pipe; 423a and a liquid outlet; 430. a condenser tube; 431. a helical blade; 440. A feed pipe; 450. a finished product liquid receiving disc; 451. a liquid storage tank; 452. a liquid outlet pipe; 460. a mixing carousel; 461. a stirring rod; 500. a secondary transmission chamber; 510. a first gear; 520. a second gear; 600. 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 3, a continuous production apparatus of sucrose-6-ester by a surrounding centrifugal type, comprising: the tank body 100, the main transmission chamber 200, the stirring chamber 300, the distillation chamber 400, the auxiliary transmission chamber 500 and the driving motor 600;
the tank body 100 is formed by connecting a main tank 110 and a tank cover 120, the tank cover 120 can be detached for convenient installation and maintenance during installation or detachment, a driving motor 600 is installed on the tank cover 120, a vacuum port 121 is also arranged on the tank cover 120, the vacuum port 121 can pump air in the tank out, three drain pipes 110a are uniformly distributed on the circumferential surface of the main tank 110, an upper partition plate 111, a middle partition plate 112 and a lower partition plate 113 are sequentially installed on the inner wall of the main tank 110 from top to bottom, and the three partition plates enable the inner part of the whole main tank 110 to be a main transmission chamber 200, a stirring chamber 300, a distillation chamber 400 and an auxiliary transmission chamber 500;
as shown in fig. 3 and 4, the main transmission chamber 200 includes a main shaft 210, a driving gear 220, a driven gear 230 and a rotating shaft 240, the upper end of the main shaft 210 is connected to a driving motor 600 on the tank cover 120, the driving gear 220 is fixedly installed in the middle of the main shaft 210, a stirring paddle 211 is further disposed at the lowest end of the main shaft 210, the three rotating shafts 240 are rotatably and uniformly installed on the upper partition 111, the driven gear 230 is installed at the upper end of the rotating shaft 240, the driven gear 230 can be connected to the driving gear 220 on the main shaft 210, and when the driving motor 600 drives the driving gear 220 to rotate, the three rotating shafts 240 rotate simultaneously;
a stirring cylinder 310 is fixedly installed inside the stirring chamber 300, a first liquid material inlet 320 and a second liquid material inlet 330 are symmetrically installed on the circumferential surface of the stirring cylinder 310 close to the lower end, the first liquid material inlet 320 and the second liquid material inlet 330 can be communicated with the inside of the stirring cylinder 310, a stirring paddle 211 at the lower end of a main shaft 210 in the main transmission chamber 200 is located inside the stirring chamber 300, and when the main shaft 210 rotates, the stirring paddle 211 stirs the mixed liquid in the stirring chamber 300;
as shown in fig. 5 to 9, the distillation chamber 400 includes: the condenser 410, the centrifuge 420, the condenser pipe 430, the feed pipe 440, the finished product liquid receiving disc 450, the mixing turntable 460, the condenser 410 and the centrifuge 420 are arranged up and down to form a single molecular distillation system, and a double molecular distillation system formed by two single molecular distillation systems arranged up and down is arranged in the distillation chamber 400;
the condenser 410 is composed of a condensation plate 411, a light component liquid receiving plate 412 and a fixing frame 413, the whole is fixed on the middle partition plate 112 through the fixing frame 413, the number of the condensation plates 411 is three and is uniformly arranged on the fixing frame 413, the inside of the condensation plate 411 is a hollow structure and is provided with a cooling chamber 411b, the inner surface of the condensation plate 411 is a conical surface, the conical surface is provided with a plurality of water collecting grooves 411a which are uniformly arranged along the circumference, the outer circumference of the condensation disc 411 is provided with a liquid inlet pipe 411c, the liquid inlet pipe 411c can be communicated with a cooling chamber 411b in the condensation disc 411, the light component liquid receiving disc 412 is annular and is sleeved at the lower end of the condensation disc 411, the light component liquid receiving disc 412 is internally provided with an annular water collecting notch 412a, the outer circumference of the light component liquid receiving disc 412 is provided with a water outlet pipe 412b, the water collecting notch 412a can be communicated with the water outlet pipe 412b, and the water outlet pipe 412b can be communicated with the water outlet pipe 110a on the main tank 110;
the centrifuge 420 consists of a recombined tapping liquid disc 421, a centrifugal disc 422 and a connecting pipe 423, the recombined tapping liquid disc 421 is a three-ring structure, each ring is provided with a liquid collecting notch 421a, the centrifugal discs 422 are three in number and rotatably installed in the three rings of the recombined tapping liquid disc 421 respectively, the inner surface of the centrifugal disc 422 is a conical surface and is internally provided with a heating wire capable of heating, the connecting pipe 423 is fixedly installed at the center of the recombined tapping liquid disc 421, the connecting pipe 423 is provided with a liquid outlet 423a on the circumferential surface of the recombined tapping liquid disc 421 at the position of the liquid collecting notch 421a on each ring, the liquid outlet 423a can make the liquid collected by the liquid collecting notch 421a on each ring flow into the connecting pipe 423, and the centrifuge 420 can be connected with the condenser 410 through the connecting pipe 423;
the rotating shaft 240 in the main transmission chamber 200 can penetrate through each centrifugal disc 422 in the double molecular distillation system and is fixedly connected with each centrifugal disc 422, the interior of the rotating shaft 240 is hollow, a liquid inlet 241 is arranged on the circumferential portion at the bottom end of the stirring chamber 300, a liquid spraying port 242 is arranged on the circumferential portion at the bottom end of the centrifuge 420 in each single molecular distillation system in the distillation chamber 400, and liquid can enter the interior of the rotating shaft 240 from the liquid inlet 241 in the stirring chamber 300 and flow onto the inner conical surface of each centrifuge 420 from the interior of the rotating shaft 240;
the condensation pipe 430 is installed in a connecting pipe 423 of two monomolecular distillation systems arranged up and down, the condensation pipe 430 is provided with a helical blade 431 on the outer surface of the inner part of the bimolecular distillation system, and the condensation pipe 430 can be communicated with a liquid inlet pipe 411c of the condenser 410 in each monomolecular distillation system, when a cooling liquid flows into the condensation pipe 430, the cooling liquid flows through the condensation pipe 430 to cool the helical blade 431 and simultaneously flows into each condensation disc 411 in each monomolecular distillation system to cool the condensation disc 411;
the feed pipe 440 is installed on a connecting pipe 423 of a centrifugal disc 422 in a lower monomolecular distillation system in a bimolecular distillation system and can be communicated with the inside of the connecting pipe 423;
the finished product liquid receiving disc 450 is of an annular disc structure, a liquid storage tank 451 is arranged in the finished product liquid receiving disc 450, the finished product liquid receiving disc is integrally and fixedly installed on the lower partition plate 113, a liquid outlet pipe 452 is arranged on the lower end face of the finished product liquid receiving disc 450, the liquid outlet pipe 452 can be communicated with the liquid storage tank 451 in the finished product liquid receiving disc 450, a mixing rotary disc 460 is rotatably installed in the finished product liquid receiving disc 450, the upper half inner surface of the mixing rotary disc 460 is a conical surface, the lower half inner surface of the mixing rotary disc is a cylindrical surface, a plurality of stirring rods 461 are uniformly arranged on the inner cylindrical surface, and a connecting pipe 423 of a centrifugal disc 422 in a lower single molecular distillation system in a double molecular distillation system is also positioned in the inner cylindrical surface;
the auxiliary transmission chamber 500 is internally provided with a first gear 510 and a second gear 520, the first gear 510 is installed on the lower cylindrical surface of the finished product liquid receiving disc 450, the second gear 520 is three and installed on the three rotating shafts 240, and the first gear 510 can be simultaneously meshed with the second gear 520, so that when the second gear 520 rotates, the first gear 510 rotates to drive the mixing turntable 460 to rotate, the mixing turntable 460 rotates to drive the stirring rod 461 to rotate, the mixed liquid is stirred, and the uniformly mixed liquid is thrown out from the upper semi-conical surface of the mixing turntable 460 in the form of a liquid film.
The invention provides a method for continuously producing sucrose-6-ester in a surrounding centrifugal mode, which comprises the following steps:
s1: firstly, mixing a sucrose solution in a polar aprotic solvent;
s2: then, a sucrose solution and an organotin acylation promoter dissolved in the polar aprotic solvent are respectively input into the stirring cylinder 310 in the stirring chamber 300 from the first liquid material inlet 320 and the second liquid material inlet 330, and the sucrose solution and the organotin acylation promoter are mixed under the rotation of the stirring paddle 211 on the main shaft 210;
s3: then the mixed liquid overflows from the upper opening of the mixing drum 310 and flows onto the middle partition plate 112, then the mixed liquid on the middle partition plate 112 enters the interior of each rotating shaft 240 from the liquid inlet 241 on each rotating shaft 240 and is discharged into the centrifugal disc 422 in each centrifuge 420 in the dual molecular distillation system from the two liquid spraying ports 242 on each rotating shaft 240, the mixed liquid is expanded on the conical surface under the action of centrifugal force under the high-speed rotation of the centrifugal disc 422 to form a thin liquid film, and meanwhile, the liquid film of the mixed liquid is heated by the electric heating wires in the centrifugal disc 422 and starts to perform fast stannization reaction to generate an organotin sucrose complex with heavy components and a light component water;
s4: the secondary water is directly evaporated into gas and moves upwards in the process of generation, the water molecules directly move to the conical surface of the condensation disc 411 of the condenser 410, are rapidly condensed into liquid drops under the cooling effect of the condensation disc 411, are converged into liquid flow in a water collecting groove 411a on the inner conical surface of the condensation disc 411, flow to a water collecting notch 412a in a light component liquid collecting disc 412 below the condensation disc 411 along the water collecting groove 411a, and finally flow to a water drainage pipe 110a from a water drainage pipe 412b to be drained out of the water drainage pipe 110 a;
s5: secondly, the gaseous heavy component substance organotin sucrose complex cannot reach the inner conical surface of the condensing disc 411 due to the small average free path of molecules and can return to the mixed liquid on the centrifugal disc 422, then the liquid heavy component substance organotin sucrose complex is thrown into a liquid collecting notch 421a in the heavy component liquid collecting disc 421 under the action of the centrifugal force of the centrifugal disc 422, and finally flows into the connecting pipe 423 through the liquid outlet 423a on the connecting pipe 423, the liquid heavy component substance organotin sucrose complex in the connecting pipe 423 continuously flows downwards along the spiral blade 431 on the surface of the condensing pipe 430, is cooled in the flowing process, and finally flows into the lower mixing turntable 460, so that the completely dry organotin sucrose complex with lower temperature is obtained;
s6: and finally, the carboxylic anhydride liquid enters the mixing turntable 460 from the feeding pipe 440, is mixed under the stirring action of the stirring rod 461 on the lower semi-cylindrical surface of the mixing turntable 460, moves to the upper semi-conical surface of the mixing turntable 460, is expanded to form a thin liquid film on the upper semi-conical surface under the centrifugal action of the mixing turntable 460, reacts quickly, generates sucrose-6-ester after the reaction is completed, is thrown into a liquid storage tank 451 in the finished product liquid receiving plate 450 from the surface of the upper semi-conical surface of the mixing turntable 460, and is finally discharged from the liquid outlet pipe 452.
Claims (2)
1. A wrap-around centrifugal sucrose-6-ester continuous production facility comprising: the device comprises a tank body (100), a main transmission chamber (200), a stirring chamber (300), a distillation chamber (400), an auxiliary transmission chamber (500) and a driving motor (600), wherein the tank body (100) consists of a main tank (110) and a tank cover (120); the method is characterized in that: the upper end of the tank cover (120) is provided with a driving motor (600), the tank cover (120) is also provided with a vacuum port (121), three drain pipes (110 a) are uniformly distributed on the circumferential surface of the main tank (110), an upper partition plate (111), a middle partition plate (112) and a lower partition plate (113) are sequentially arranged inside the main tank (110) from top to bottom, the three partition plates enable the inside of the whole main tank (110) to be a main transmission chamber (200), a stirring chamber (300), a distillation chamber (400) and an auxiliary transmission chamber (500), the main transmission chamber (200) internally comprises a main shaft (210), a driving gear (220), a driven gear (230) and a rotating shaft (240), the upper end of the main shaft (210) is connected with an output shaft of the driving motor (600), the driving gear (220) is arranged on the main shaft (210) and positioned in the main transmission chamber (200), the upper end of the rotating shaft (240) is provided with the driven gear (230), on main shaft (210) and be located teeter chamber (300) and be equipped with stirring rake (211), teeter chamber (300) inside fixed mounting churn (310), the symmetry sets up liquid material entry one (320) and liquid material entry two (330) on the periphery of churn (310) lower extreme, and distillation chamber (400) includes: the condenser (410), the centrifuge (420), the condenser pipe (430), the feed pipe (440), the finished product liquid receiving disc (450), the mixing turntable (460), the condenser (410) is composed of a condensing disc (411), a light component liquid receiving disc (412) and a fixing frame (413), the whole is fixed on the middle partition plate (112) through the fixing frame (413), the number of the condensing discs (411) is three and is uniformly installed on the fixing frame (413), the inside of the condensing disc (411) is a hollow structure and is provided with a cooling chamber (411 b), the outer circumference of the condensing disc (411) is provided with a liquid inlet pipe (411 c), the liquid inlet pipe (411 c) is communicated with the cooling chamber (411 b) inside the condensing disc (411), the light component liquid receiving disc (412) is in a circular ring shape and is sleeved at the lower end of the condensing disc (411), the light component liquid receiving disc (412) is internally provided with a circular water collecting notch (412 a), the outer circumference of the light component liquid receiving disc (412) is provided with a water outlet pipe (412 b), the water collecting notch (412 a) is communicated with a water outlet pipe (412 b), the water outlet pipe (412 b) is communicated with a water discharge pipe (110 a) on the main tank (110), the centrifuge (420) consists of three recombined tapping liquid discs (421), centrifugal discs (422) and connecting pipes (423), each recombined tapping liquid disc (421) is of a three-ring structure, each ring is provided with a water collecting notch (421 a), the centrifugal discs (422) are three in number and rotatably arranged in the three rings of the recombined tapping liquid discs (421) respectively, the connecting pipe (423) is fixedly arranged in the center of the recombined tapping liquid discs (421), the connecting pipe (423) is provided with a liquid outlet (423 a) on the circumferential surface at the position of the water collecting notch (421 a) on each ring of the recombined tapping liquid discs (421), the centrifuge (420) is connected with the condenser (410) through the connecting pipe (423), the circumferential part of the rotating shaft (240) at the bottom end of the stirring chamber (300) is provided with a liquid inlet (241), a liquid spraying port (242) is arranged on the circumferential part of the rotating shaft (240) which is positioned at the inner bottom end of the centrifuge (420), a condensing pipe (430) is arranged in a connecting pipe (423) of two single-molecule distillation systems which are arranged up and down, the condensing pipe (430) is communicated with a liquid inlet pipe (411 c) on a condenser (410) in each single-molecule distillation system, a feed pipe (440) is arranged on the connecting pipe (423) of a centrifugal disc (422) in the single-molecule distillation system below the double-molecule distillation system and can be communicated with the inside of the connecting pipe (423), the finished product liquid receiving disc (450) is of an annular disc structure and is internally provided with a liquid storage tank (451), the whole body is fixedly arranged on a lower partition plate (113), a liquid outlet pipe (452) is arranged on the lower end surface of the finished product liquid receiving disc (450), the liquid outlet pipe (452) can be communicated with the liquid storage tank (451) in the finished product liquid receiving disc (450), and a mixing rotary disc (460) is arranged in the finished product liquid receiving disc (450), the connecting pipe (423) of a centrifugal disc (422) in a lower monomolecular distillation system in the bimolecular distillation system is also positioned in an inner cylindrical surface, the inner surface of a condensing disc (411) is a conical surface, the conical surface is provided with a plurality of water collecting grooves (411 a) which are uniformly arranged along the circumference, the inner surface of the centrifugal disc (422) is a conical surface, electric heating wires are arranged in the centrifugal disc (422), three rotating shafts (240) are uniformly and rotatably arranged on an upper partition plate (111), a driven gear (230) can be connected with a driving gear (220) on a main shaft (210), a condenser (410) and a centrifuge (420) are vertically arranged to form a monomolecular distillation system, a bimolecular distillation chamber (400) is internally provided with the bimolecular distillation system which is formed by vertically arranging two monomolecular distillation systems, and the rotating shafts (240) can penetrate through each centrifugal disc (422) in the bimolecular distillation system and are fixedly connected with each centrifugal disc (422), the rotating shaft (240) is hollow, the upper half inner surface of the mixing turntable (460) is a conical surface, the lower half inner surface is a cylindrical surface, a plurality of stirring rods (461) are uniformly arranged on the inner cylindrical surface, a first gear (510) and a second gear (520) are arranged in the auxiliary transmission chamber (500), the first gear (510) is installed on the lower cylindrical surface of the finished product liquid receiving disc (450) and is three, the second gear (520) is installed on the three rotating shaft (240), the first gear (510) can be meshed with the second gear (520) simultaneously, and the condensing pipe (430) is located on the outer surface of the inner part of the double molecular distillation system and is provided with spiral blades (431).
2. A method for continuous production of sucrose-6-ester by a surrounding centrifugal process, comprising the steps of: a continuous process plant using the wrap-around centrifugal sucrose-6-ester of claim 1 comprising the steps of:
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 stirring cylinder (310) in a stirring chamber (300) from a liquid material inlet I (320) and a liquid material inlet II (330), and mixing the sucrose solution and the organic tin acylation promoter under the rotation of a stirring paddle (211) on a main shaft (210);
s3: then the mixed liquid overflows from an upper opening of the mixing drum (310) and flows onto the middle partition plate (112), then the mixed liquid on the middle partition plate (112) enters the interior of each rotating shaft (240) from a liquid inlet (241) on each rotating shaft (240), then is discharged into a centrifugal disc (422) in each centrifuge (420) in the double-molecular distillation system from two liquid spraying ports (242) on each rotating shaft (240), the mixed liquid is expanded on the conical surface under the action of centrifugal force under the high-speed rotation of the centrifugal disc (422) to form a thin liquid film, and meanwhile, the liquid film of the mixed liquid is heated by an electric heating wire in the centrifugal disc (422) and starts to carry out a fast stannization reaction to generate an organotin sucrose complex with heavy components and a substance water with light components;
s4: the secondary water is directly evaporated into gas and moves upwards in the generation process, water molecules directly move to the conical surface of a condensation disc (411) of the condenser (410), are rapidly condensed into liquid drops under the cooling effect of the condensation disc (411), are converged into liquid flow in a water collecting groove (411 a) on the inner conical surface of the condensation disc (411), flow into a water collecting notch (412 a) in a light component liquid collecting disc (412) below the condensation disc (411) along the water collecting groove (411 a), and finally flow into a water drainage pipe (110 a) from a water outlet pipe (412 b) and are drained out of the water drainage pipe (110 a);
s5: secondly, the gaseous heavy component substance organotin sucrose complex cannot reach the inner conical surface of the condensing disc (411) due to the small molecular mean free path and returns to the mixed liquid on the centrifugal disc (422), then the liquid heavy component substance organotin sucrose complex is thrown into a liquid collecting notch (421 a) in the heavy component liquid dividing disc (421) under the action of the centrifugal force of the centrifugal disc (422), finally flows into the connecting pipe (423) through the liquid outlet (423 a) on the connecting pipe (423), the liquid heavy component substance organotin sucrose complex in the connecting pipe (423) continuously flows downwards along the spiral blade (431) on the surface of the condensing pipe (430), is cooled in the flowing process, and finally flows into the mixing rotary disc (460) below to obtain the completely dried organotin sucrose complex with lower temperature;
s6: and finally, the carboxylic anhydride liquid enters the mixing turntable (460) from the feeding pipe (440), is mixed under the stirring action of the stirring rod (461) on the lower semi-cylindrical surface of the mixing turntable (460), the mixed liquid moves to the upper semi-conical surface of the mixing turntable (460), is expanded to form a thin liquid film on the upper semi-conical surface under the centrifugal action of the mixing turntable (460), reacts quickly, generates sucrose-6-ester after the reaction is completed, is thrown from the surface of the upper semi-conical surface of the mixing turntable (460) into a liquid storage tank (451) in the finished product liquid receiving plate (450), and is finally discharged from the liquid outlet pipe (452).
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