CN219218222U

CN219218222U - Psicose crystal preparation system

Info

Publication number: CN219218222U
Application number: CN202222124608.8U
Authority: CN
Inventors: 李明全; 吴泽甫; 常曲; 陈真; 刘晓花; 张飞
Original assignee: Shanghai Donggeng Chemical Technology Co ltd; Ningxia Donggeng New Material Technology Co ltd
Current assignee: Shanghai Donggeng Chemical Technology Co ltd; Ningxia Donggeng New Material Technology Co ltd
Priority date: 2022-08-12
Filing date: 2022-08-12
Publication date: 2023-06-20
Anticipated expiration: 2032-08-12

Abstract

The utility model discloses an allulose crystal preparation system which comprises a tubular falling film crystallizer, a cooler and a plate-type falling film crystallizer which are sequentially communicated, wherein the tubular falling film crystallizer is provided with a first cold and hot medium inlet, a first cold and hot medium outlet, a first feed inlet and a first discharge outlet, the plate-type falling film crystallizer comprises a shell, a second feed inlet and an air outlet are formed in the top of the shell, a second discharge outlet and an air inlet are formed in the bottom of the shell, a crystallization plate which is arranged in the vertical direction is arranged in the shell, a crystallization tank and a heat exchange cavity are arranged in the vertical direction, the crystallization tank is communicated with the second feed inlet, the heat exchange cavity is located in an adjacent area of the crystallization tank, a second cold and hot medium inlet which is communicated with the heat exchange cavity is formed in the lower portion of the shell, an air inlet and an air outlet are formed in the top and the bottom of the shell respectively, and the air inlet is located below the crystallization plate.

Description

Psicose crystal preparation system

Technical Field

The utility model belongs to the technical field of chemical industry, and particularly relates to a psicose crystal preparation system.

Background

With the improvement of living standard, people are increasingly concerned about food safety and other problems, especially various functional additives. Psicose is a low calorie sweetener which is widely sold in the food industry because of its high sweetness and its difficulty in digestion. In addition, allose has the effects of reducing in vivo fat accumulation, inhibiting the rise of blood glucose concentration, improving insulin sensitivity and glucose tolerance in the field of medicine. However, psicose is very small in content in nature, and is difficult to meet market demands, and usually requires artificial synthesis.

Psicose belongs to ketohexose, is hexose, and is epimer corresponding to the carbon number three of D-fructose. The synthesis method of psicose includes chemical synthesis method and biological enzyme method. The production of psicose by chemical synthesis has the following disadvantages: chemical waste and byproducts are easy to form; the purification process is difficult; the operation is complex, and multiple protection and deprotection operations are required. Therefore, the chemical synthesis method is greatly restricted in practical production and application. Compared with a chemical synthesis method, the enzymatic synthesis of the psicose has the advantages that: the process is more environment-friendly; the reaction condition is mild; the specificity is strong; the catalytic efficiency is high; the sustainability is strong. Therefore, bioconversion of psicose is an important and hot spot of current research.

However, the commercially available psicose is basically a liquid product or a powdery solid product, because the psicose is in high supersaturation, crystals are grown faster than crystals, fine crystals are easy to generate, the solution viscosity is increased, the growth of large crystals is unfavorable, if the heating concentration and cooling crystallization processes are carried out for many times, the production process is complex, the operation is difficult, the granularity of the generated psicose crystals is small, the yield of the psicose crystals is only about 20% -30%, and the production economy of the psicose crystal product is seriously affected.

In the related technology, the processes and equipment such as heating concentration, chromatographic separation, evaporative crystallization and the like are generally adopted for coupling, so that the process flow is complicated, the time is long, the energy consumption is high, the actual production economy is poor, and the prepared product crystals are granular, small in size and low in yield.

Disclosure of Invention

In view of the above-mentioned drawbacks of the prior art, the present utility model aims to provide a system for preparing psicose crystals, which is used for solving the technical problems of complicated process flow, long time consumption, high energy consumption, poor practical production economy, small granularity and low yield of the prepared psicose crystals by adopting the existing equipment.

The utility model provides an psicose crystal preparation system, which comprises a tubular falling film crystallizer, a cooler and a plate-type falling film crystallizer which are sequentially communicated, wherein the tubular falling film crystallizer is provided with a first cold and hot medium inlet, a first cold and hot medium outlet, a first feed inlet and a first discharge outlet, the plate-type falling film crystallizer comprises a shell, the top of the shell is provided with a second feed inlet and an air outlet, the bottom of the shell is provided with a second discharge outlet and an air inlet, the inside of the shell is provided with a crystallization plate arranged in the vertical direction, the crystallization plate is provided with a crystallization groove and a heat exchange cavity in the vertical direction, the crystallization groove is communicated with the second feed inlet through a feed pipe, the heat exchange cavity is positioned in an adjacent area of the crystallization groove, the lower part of the shell is provided with a second cold and hot medium inlet communicated with the heat exchange cavity, the top and the bottom of the shell are respectively provided with an air inlet and an air outlet, and the air inlet is positioned below the crystallization plate.

The basic scheme of the utility model is as follows: the tubular falling film crystallizer and the plate falling film crystallizer are combined, so that the purity of the prepared psicose crystal can be improved, the time is shortened, and the energy consumption is reduced; by additionally arranging the air inlet, high-pressure gases such as high-pressure nitrogen, inert gas and the like can be introduced into the shell, so that the high-pressure gases entering from the bottom are in countercurrent contact with the material to be purified in the upward diffusion process, the flow velocity of the material to be purified is reduced, the psicose crystals are better crystallized on the wall surface of the crystallization tank, and the crystallization thickness and the crystallization yield are improved; at the same time, volatile substances in the material to be purified can escape.

The term "psicose crystal" in the present application refers to a D-psicose crystal, an L-psicose crystal, or a D-psicose crystal/L-psicose crystal mixed crystal, i.e., the preparation system of the present application is applicable to a D-psicose crystal, an L-psicose crystal, or a D-psicose crystal/L-psicose crystal mixed crystal.

Optionally, the first discharge port is communicated with a mother liquid tank and/or a sweat tank, and the mother liquid tank and/or the sweat tank is communicated with the first feed port.

Through with first discharge gate intercommunication mother liquor jar and/or sweat jar to with mother liquor jar and/or sweat jar intercommunication first feed inlet, can be with mother liquor, the sweat of discharging from first discharge gate go into tubular falling film crystallizer again and crystallize, in order to retrieve the allose sugar in mother liquor, the sweat, further improve the yield of allose sugar crystal product.

Optionally, the first discharge port is communicated with the first feed port through a first material circulating pipeline, and a circulating pump is arranged on the first material circulating pipeline.

Through the first material circulation pipeline with first discharge gate intercommunication first feed inlet, can be with waiting to purify in the material not send into tubular falling film crystallizer again after the crystallization is carried out to the crystallization of crystallization liquid, further improve the yield of allose crystal product.

Optionally, the first cooling and heating medium outlet is communicated with the first cooling and heating medium inlet through a first cooling and heating medium circulation pipeline, and a circulation pump, a cooling medium cooler and a heating medium heat exchanger are arranged on the first cooling and heating medium circulation pipeline.

Through with first cold and hot medium export through first cold and hot medium circulation pipeline intercommunication first cold and hot medium import to set up circulating pump, refrigerant cooler and heat medium heat exchanger on with first cold and hot medium circulation pipeline, can realize the cyclic utilization of cold and hot medium, improve cold and hot medium utilization ratio, reduction in production cost.

Optionally, the crystallization plate is provided with a plurality of crystallization grooves along the vertical direction.

Through offer a plurality of crystallization tanks with the crystallization board along vertical direction, can carry out crystallization simultaneously through a plurality of crystallization tanks, and then improve production efficiency, reduce the energy consumption.

Optionally, still set up the push rod subassembly inside the plate-type falling film crystallizer, the push rod subassembly is located the crystallization board top, the push rod subassembly include first actuating mechanism and with the push rod that the crystallization tank corresponds, actuating mechanism is used for driving the push rod to make the push rod will crystallize in crystallization tank's crystallization material from crystallization tank wall surface push off, the push rod sets up along vertical direction.

By additionally arranging the push rod component, the psicose crystal substance crystallized on the wall surface of the crystallization tank can be pushed off from the wall surface of the crystallization tank by the push rod corresponding to the crystallization tank, so that the yield of psicose crystal products is further improved.

Optionally, the plate-type falling film crystallizer further comprises a cutting mechanism, the cutting mechanism is fixedly mounted on the inner wall of the shell, the cutting mechanism is arranged along the opposite direction of the crystallization groove, the cutting mechanism is provided with a cutter and a second driving mechanism for driving the cutter to stretch out and draw back, and the cutter is arranged along the direction perpendicular to the crystallization groove.

By additionally arranging the cutting mechanism which is arranged along the opposite direction of the crystallization groove, the psicose crystallization substance crystallized on the wall surface of the crystallization groove can be cut, so that the psicose crystallization substance crystallized on the wall surface of the crystallization groove is easier to fall off from the wall surface of the crystallization groove, and the yield of psicose crystal products is further improved.

Optionally, the plate-type falling film crystallizer further comprises a spray head, wherein the spray head is positioned inside the shell and above the crystallization tank, and the spray head is communicated with a high-pressure air inlet pipe and/or a high-pressure liquid inlet pipe.

By additionally arranging the spray head above the crystallization tank, the spray head is communicated with the high-pressure air inlet pipe, and when sweat separation is carried out in a sweating stage, sweat formed by viscous materials to be purified can be blown off by utilizing high-pressure gas; through with shower nozzle intercommunication high pressure feed liquor pipe, when need wash the crystallization tank, can utilize high pressure liquid to wash the crystallization tank.

Optionally, the plate falling film crystallizer further comprises a filtering mechanism, the filtering mechanism is detachably fixed on the inner wall of the shell, the filtering mechanism is located between the second feeding hole and the second discharging hole, the filtering mechanism is located below the crystallization plate, and an opening is formed in the filtering mechanism.

Optionally, a pipe connecting the heat exchange cavity with the second cold and hot medium outlet and/or a pipe connecting the heat exchange cavity with the second cold and hot medium outlet extends into the heat exchange cavity.

The pipeline communicating the heat exchange cavity with the second cold and hot medium inlet and/or the pipeline communicating the heat exchange cavity with the second cold and hot medium outlet extend into the heat exchange cavity, so that the travel of a refrigerant medium can be shortened, the heat exchange effect between the refrigerant medium and a material to be purified is improved, the crystallization effect (the crystallization thickness) of the psicose crystallization substance on the wall surface of the crystallization tank is ensured, and the yield of psicose crystal products is further improved.

Optionally, the cutting mechanism is provided with a plurality of cutters, and all the cutters are arranged in parallel along the direction perpendicular to the crystallization groove.

Through being provided with a plurality of cutters with cutting mechanism, all cutters are along setting up in parallel with the direction of crystallization groove vertically, can cut the allose crystalline substance of crystallization in crystallization cell wall face through a plurality of cutters simultaneously to make the allose crystalline substance of crystallization in crystallization cell wall face more easily drop from the crystallization cell wall face, further improve the yield of allose crystalline product.

Optionally, the spray head adopts a rotary spray head.

By arranging the spray head into a rotary spray head, the psicose crystal substance can fall off from the wall surface of the crystallization tank more easily, and the yield of the psicose crystal product is further improved.

Optionally, the push rod is arranged to be matched with the crystallization tank, so that more psicose crystallization substances can be pushed off from the wall surface of the crystallization tank, and the yield of psicose crystal products is further improved.

Optionally, the crystallization plate is further provided with a heat exchange groove, the refrigerant heat exchange groove is located in an adjacent area of the crystallization groove, and the heat exchange groove is communicated with the second cold and heat medium inlet and the second cold and heat medium outlet.

Through addding the heat transfer groove, can carry out the heat exchange through coolant medium and the material that waits to purify in heat exchange cavity and the heat transfer groove simultaneously, be favorable to waiting to purify the material rapid cooling, further improve crystallization effect, improve the yield of psicose crystal product.

Optionally, a pipe connecting the heat exchange tank with the second cold and hot medium outlet and/or a pipe connecting the heat exchange tank with the second cold and hot medium outlet extend into the heat exchange tank.

The travel of the refrigerant medium can be shortened through the pipeline which is communicated with the heat exchange groove and the second cold and hot medium inlet and/or the pipeline part heat exchange groove which is communicated with the heat exchange groove and the second cold and hot medium outlet, so that the heat exchange effect between the refrigerant medium and the material to be purified is improved, the crystallization effect (the crystallization thickness) of the psicose crystallization substance on the wall surface of the crystallization groove is ensured, and the yield of the psicose crystal product is further improved.

Optionally, the second discharging hole is further communicated with a residual liquid tank and/or a sweat storage tank, the residual liquid tank is communicated with the first feeding hole, and the sweat storage tank is communicated with the second feeding hole.

Through with second discharge gate intercommunication residuum jar and/or sweat storage tank to with the first feed inlet of residuum jar intercommunication, with sweat storage tank intercommunication second feed inlet, can be with in the board-like falling film crystallizer crystallization of going into again from board-like falling film crystallizer of the raffinate that discharges, sweat, with the recovery raffinate, the yield of the psicose crystal product in the sweat, further improve.

Optionally, the second discharge port is communicated with the second feed port through a second material circulation pipeline, and a circulation pump is arranged on the second material circulation pipeline.

Through the second discharge hole communicated with the second feed inlet through the second circulating pipeline, the uncrystallized liquid in the intermediate product can be sent into the plate-type falling film crystallizer again for crystallization after being circulated, and the yield of the psicose crystal product is further improved.

Optionally, the second cold and hot medium outlet is communicated with the second cold and hot medium inlet through a second cold and hot medium circulation pipeline, and a circulation pump, a refrigerant cooler and a hot medium heat exchanger are arranged on the second cold and hot medium circulation pipeline.

Through with second cold and hot medium export through second cold and hot medium circulation pipeline intercommunication second cold and hot medium import to set up circulating pump, refrigerant cooler and heat medium heat exchanger on the second cold and hot medium circulation pipeline, can realize the cyclic utilization of cold and hot medium, improve cold and hot medium utilization ratio, reduction in production cost.

Optionally, the psicose crystal preparation system further comprises a solvent tank, wherein the solvent tank is communicated with the bottom of the shell through a pipeline.

Through addding the solvent jar to with solvent jar through pipeline intercommunication casing bottom, can send into solvents such as ethanol in the casing, make solvents such as ethanol dissolve the uncrystallized liquid in the intermediate product, improve the velocity of flow of uncrystallized liquid in the intermediate product, avoid the unable effective cyclic crystallization's that leads to because of uncrystallized liquid viscosity is too big in the intermediate product problem, further improve the yield of psicose crystal product.

Optionally, the air outlet is communicated with the solvent tank through a pipeline, and a condenser is arranged on a communication pipeline between the air outlet and the solvent tank.

Through add the condenser on the communication pipeline between gas outlet and solvent jar, can retrieve the reuse to solvents such as ethanol, improve the recycle rate of solvents such as ethanol, and then reduction in production cost improves the benefit.

Drawings

FIG. 1 is a schematic diagram of the structure of a system for preparing psicose crystals of example 1;

FIG. 2 is a schematic view of the plate-type falling film crystallizer in FIG. 1;

FIG. 3 is a schematic view of the structure of the crystallization plate in FIG. 2;

FIG. 4 is a perspective view of the cutting mechanism of FIG. 2 mated with a crystallization plate;

FIG. 5 is a schematic diagram showing the structure of a push rod assembly of a falling film crystallizer of the psicose crystal production system of example 2;

FIG. 6 is an assembly drawing of a falling film crystallizer crystallization plate and a shell of the psicose crystal production system of example 3;

FIG. 7 is a schematic diagram showing the structure of a system for preparing psicose crystals of example 4.

Reference numerals

1-a plate type falling film crystallizer; 101-a housing; 102-second feed inlet, 1021-feed pipe, 1022-feed manifold, 1023-barrier element; 103-crystallization plates, 1031-crystallization tanks, 1032-heat exchange cavities and 1033-heat exchange tanks; 104-a push rod assembly, 1041-a push rod, 1042-a first driving mechanism, 1043-a push block; 105-filtering means, 1051-openings; 106-a cutting mechanism, 1061-a cutter, 1062-a second driving mechanism; 107-air inlet; 108-a second discharge port; 109-spray head; 1010-an air outlet; 1012-a second cold and hot medium inlet, 10121-a cold and hot medium inlet pipe; 1013-a second cold and hot medium outlet, 10131-a cold and hot medium outlet pipe;

2-a tubular falling film crystallizer;

3-an intermediate product tank;

4-a cooler;

5-a mother liquor tank;

6-a sweat tank;

7-a raw material tank;

8-a residue tank;

9-sweat storage tank;

10-a circulating pump;

11-a centrifugal pump;

12-switching a valve;

13-a refrigerant cooler;

14-a heat medium heat exchanger;

15-a solvent tank;

16-condenser.

Detailed Description

Other advantages and effects of the present utility model will become apparent to those skilled in the art from the following disclosure, which describes the embodiments of the present utility model with reference to specific examples. The utility model may be practiced or carried out in other embodiments that depart from the specific details, and the details of the present description may be modified or varied from the spirit and scope of the present utility model.

It should be noted that, the illustrations provided in the present embodiment merely illustrate the basic concept of the present utility model by way of illustration, and only the components related to the present utility model are shown in the drawings and are not drawn according to the number, shape and size of the components in actual implementation, and the form, number and proportion of the components in actual implementation may be arbitrarily changed, and the layout of the components may be more complex. The structures, proportions, sizes, etc. shown in the drawings attached hereto are for illustration purposes only and are not intended to limit the scope of the utility model, which is defined by the claims, but rather by the claims. Meanwhile, the terms such as "upper", "lower", "top", "bottom", "vertical" and the like are used in the present specification for convenience of description, and are not intended to limit the scope of the present utility model, but the relative changes or modifications thereof are also regarded as the scope of the present utility model without substantial modification of the technical content. It should be understood that the orientation word "inner and outer" refers to inner and outer relative to the contour of the components themselves.

In the description of the present utility model, it should be understood that the terms "first," "second," and the like are used for defining the components, and are merely for convenience in distinguishing the corresponding components, and the terms are not meant to have any special meaning unless otherwise indicated, so that the scope of the present utility model is not to be construed as being limited.

The application provides a production method of psicose crystals, which comprises the following steps:

s1, delivering an psicose solution with the temperature of 80-120 ℃ and the concentration of 70-80 wt% into a tubular falling film crystallizer for crystallization, specifically, firstly cooling to 40-45 ℃ at the speed of 3-5 ℃/min, then cooling to 30-35 ℃ at the speed of 0.5-1 ℃/min, and then crystallizing for 90-100min at the temperature of 30-35 ℃; subsequent sweating, in particular: heating to 80-90deg.C at a rate of 3-5deg.C/min, heating to 105-110deg.C at a rate of 0.5-1deg.C/min, and maintaining at 105-110deg.C for 40-50min to obtain sweat; and then melting, specifically: heating to 115-125 ℃ at a speed of 0.5-1 ℃/min, then preserving heat at 115-125 ℃ for 30-40min to obtain an intermediate product, and then preserving heat at 120-125 ℃ for 30-40min to obtain a liquid intermediate product; concentrating and recovering mother liquor generated in the crystallization process and sweat obtained in the sweating process, and sending the mother liquor and sweat obtained in the enrichment and recovery process into a tubular falling film crystallizer for crystallization;

S2, precooling the intermediate product to 60-80 ℃, and then feeding the intermediate product into a plate-type falling film crystallizer for crystallization, wherein the steps are as follows: firstly cooling to 30-40 ℃, and then crystallizing at 30-40 ℃; then heating to 80-90 ℃ at the speed of 3-5 ℃/min, then heating to 105-110 ℃ at the speed of 0.5-1 ℃/min, then heating to 105-110 ℃ at the speed of 0.6-1 ℃/min, and then preserving heat at the temperature of 105-110 ℃ for 40-50min; then preserving heat at 105-110deg.C for 40-50min to obtain sweat; and (3) sending mother liquor generated in the crystallization process and sweat obtained in the sweating process into a tubular falling film crystallizer for secondary crystallization to obtain psicose crystals.

The application also provides a production system adopted by the production method, which comprises a tubular falling film crystallizer, a cooler and a plate falling film crystallizer which are communicated in sequence;

the tubular falling film crystallizer is provided with a first feed inlet, a first discharge outlet, a first cold and hot medium inlet and a first cold and hot medium outlet, wherein the first discharge outlet is communicated with a mother liquid tank and/or a sweat tank, the mother liquid tank and/or the sweat tank is communicated with the first feed inlet, the first discharge outlet is communicated with the first feed inlet through a first material circulating pipeline, a circulating pump is arranged on the first material circulating pipeline, the first cold and hot medium outlet is communicated with the first cold and hot medium inlet through a first cold and hot medium circulating pipeline, and the first cold and hot medium circulating pipeline is provided with a circulating pump, a refrigerant cooler and a hot medium heat exchanger;

The plate type falling film crystallizer comprises a shell, wherein a second feed inlet and an air outlet are formed in the top of the shell, the second feed inlet is flat, a second discharge outlet and an air inlet are formed in the bottom of the shell, the second discharge outlet is communicated with the second feed inlet through a second material circulation pipeline, and a push rod assembly, a crystallization plate, a filter mechanism and a liquid collecting cavity are sequentially arranged in the shell along the vertical direction;

the crystallization plate is provided with a plurality of crystallization tanks, a plurality of heat exchange cavities and a plurality of heat exchange tanks along the vertical direction, the crystallization tanks are communicated with a feed inlet through a feed pipe, the heat exchange cavities are positioned in adjacent areas of the crystallization tanks, the lower part of the shell is provided with a second cold and heat medium inlet communicated with the heat exchange cavities, the upper part of the shell is provided with a second cold and heat medium outlet communicated with the heat exchange cavities, the second cold and heat medium outlet is communicated with the second cold and heat medium inlet through a second cold and heat medium circulation pipeline, and the second cold and heat medium circulation pipeline is provided with a circulation pump, a refrigerant cooler and a heat medium heat exchanger;

the top and the bottom of the shell are respectively provided with an air inlet and an air outlet, and the air inlet is positioned below the crystallization plate; the refrigerant heat exchange groove is positioned in the adjacent area of the crystallization groove and is communicated with the second cold and heat medium inlet and the second cold and heat medium outlet; the pipeline for communicating the heat exchange cavity with the second cold and hot medium inlet and/or the pipeline for communicating the heat exchange cavity with the second cold and hot medium outlet extend into the heat exchange cavity; the pipeline for communicating the heat exchange groove with the second cold and hot medium inlet and/or the pipeline for communicating the heat exchange groove with the second cold and hot medium outlet extend into the heat exchange groove;

The filtering mechanism is detachably fixed on the inner wall of the shell, the filtering mechanism is positioned between the second feeding hole and the second discharging hole, the filtering mechanism is positioned below the crystallization plate, and an opening is formed in the shell, close to the filtering mechanism;

the push rod assembly is positioned above the crystallization plate and comprises a first driving mechanism and a plurality of push rods corresponding to the crystallization grooves, the driving mechanism is used for driving the push rods so that the push rods push crystalline substances crystallized in the crystallization grooves from the wall surfaces of the crystallization grooves, and the push rods are arranged along the vertical direction;

the plate-type falling film crystallizer further comprises a cutting mechanism, the cutting mechanism is fixedly arranged on the inner wall of the shell, the cutting mechanism is arranged along the opposite direction of the crystallization groove, the cutting mechanism is provided with a plurality of cutters and a second driving mechanism for driving the cutters to stretch out and draw back, and all the cutters are arranged in parallel along the direction perpendicular to the crystallization groove;

the plate-type falling film crystallizer further comprises a spray head, wherein the spray head is positioned in the shell and above the crystallization tank, the spray head is communicated with a high-pressure air inlet pipe and/or a high-pressure liquid inlet pipe, and the spray head adopts a rotary spray head;

the second discharge port is communicated with a residual liquid tank and/or a sweat storage tank, and the residual liquid tank and/or the sweat storage tank is communicated with a second feed port.

In another embodiment of the present application, the bottom of the housing is further communicated with a solvent tank, the solvent tank is communicated with an air outlet through a pipe, and a condenser is arranged on a communication pipe between the air outlet and the solvent tank.

In another embodiment of the present application, the pushrod is mated to the crystallization tank.

The present utility model will be described in detail with reference to specific exemplary examples. It is also to be understood that the following examples are given solely for the purpose of illustration and are not to be construed as limitations upon the scope of the utility model, as many insubstantial modifications and variations are within the scope of the utility model as would be apparent to those skilled in the art in light of the foregoing disclosure. The specific process parameters and the like described below are also merely examples of suitable ranges, i.e., one skilled in the art can make a suitable selection from the description herein and are not intended to be limited to the specific values described below. The term "wt%" as used herein refers to the mass content unless otherwise specified.

Example 1

Referring to fig. 1, fig. 1 is a schematic structural diagram of an psicose crystal preparation system according to the present embodiment, which is used for producing psicose crystal products.

As shown in fig. 1, the psicose crystal production system of the present embodiment comprises a tubular falling film crystallizer 2, a cooler 4 and a plate falling film crystallizer 1 which are sequentially connected.

With continued reference to fig. 1, the tubular falling film crystallizer 1 is a crystallization apparatus using a crystallization tube as a crystallization component. The bottom of the tubular falling film crystallizer 2 is provided with a first feed inlet (not shown) and a first discharge outlet (not shown), the upper part of the tubular falling film crystallizer 2 is provided with a first cold and heat medium inlet (not shown), and the lower part of the tubular falling film crystallizer 2 is provided with a first cold and heat medium outlet (not shown).

With continued reference to fig. 1, the first discharge port is connected to the first feed port through a first material circulation pipe, and a circulation pump 10 is disposed on the first material circulation pipe. The circulation pump is prior art and will not be described here in detail.

Specifically, through the first discharge port which is communicated with the first feed port through the first material circulation pipeline, uncrystallized liquid in the material to be purified can be sent into the tubular falling film crystallizer 2 for crystallization after being circulated, and the yield of psicose crystal products is further improved.

With continued reference to fig. 1, the first cooling and heating medium inlet is used for introducing cooling and heating medium (cooling water and the like can be adopted as the cooling medium, heat exchange oil and the like can be adopted as the heating medium) into the tubular falling film crystallizer 2, and the first cooling and heating medium outlet is used for discharging the cooling and heating medium after heat exchange treatment from the tubular falling film crystallizer 2. The first cooling and heating medium outlet is communicated with the first cooling and heating medium inlet through a first cooling and heating medium circulation pipeline, and a circulation pump 10, a cooling medium cooler 13 and a heating medium heat exchanger 14 are arranged on the first cooling and heating medium circulation pipeline.

With continued reference to fig. 1, the refrigerant cooler 13 is configured to cool the refrigerant (the refrigerant may adopt cooling water or other substances) with a temperature increased after heat exchange (crystallization stage), so that the refrigerant is sent into the tubular falling film crystallizer 2 again to exchange heat with the uncrystallized material to be purified, and the uncrystallized material in the uncrystallized material to be purified after primary crystallization is recrystallized, thereby improving yield of psicose crystals. The heat medium heat exchanger 14 is used for heating the heat medium (heat medium can be heat exchange oil or the like) with reduced temperature after heat exchange (sweating and melting stages), so that the heat medium enters the tubular falling film crystallizer 2 again through the first cold and heat medium circulating pipeline to exchange heat with the crystal substances obtained again on the pipe wall of the crystallizing pipe, and the purity of the psicose crystal is improved. The refrigerant cooler 13 may be a tube type cooler, a plate type cooler, an air-cooled cooler, or the like. The heat medium heat exchanger 14 may be a dividing wall type heat exchanger, a hybrid type heat exchanger, a regenerative type heat exchanger, or the like. The tubular falling film crystallizer, the switching valve, the centrifugal pump, the tubular cooler, the plate cooler, the air-cooled cooler, the dividing wall type heat exchanger, the hybrid heat exchanger, the heat accumulating type heat exchanger and the like are in the prior art, and are not repeated here.

Specifically, through with first cold and hot medium export through first cold and hot medium circulation pipeline intercommunication first cold and hot medium import to set up circulating pump, refrigerant cooler and heat medium heat exchanger on the second cold and hot medium circulation pipeline, can realize the cyclic utilization of cold and hot medium, improve cold and hot medium utilization ratio, reduction in production cost.

With continued reference to fig. 1, the first feed port is connected to a raw material tank 7, and a centrifugal pump 11 and a switch valve 12 are disposed on a communication pipe between the raw material tank 7 and the first feed port. The raw material tank 7 is used as a storage place of a crystal raw material to be purified, namely, the psicose solution, and the psicose solution with the concentration of 70-80 wt% is stored in the raw material tank 7. A switching valve 12 and a centrifugal pump 11 are arranged on a communication pipeline between the raw material tank 7 and the first feed inlet.

With continued reference to fig. 1, the first outlet is in communication with a mother liquor tank 5 and a sweat tank 6. A mother liquor tank 5 and a sweat tank 6 are positioned below the tubular falling film crystallizer 2. The liquid inlet end of the liquid tank 5 and/or the liquid inlet end of the sweat tank 6 are/is communicated with a first discharge port through a pipeline, and a switch valve 12 is arranged on a communication pipeline between the first discharge port and the mother liquor tank 5 and a communication pipeline between the first discharge port and the sweat tank 6. The on-off valve 12 and the centrifugal pump 11 are arranged on the communicating pipeline between the liquid outlet end of the mother liquid tank 5 and/or the liquid outlet end of the sweat tank 6 and the first feed port.

With continued reference to fig. 1, a sealing valve (not shown) is disposed at the first outlet, and the mother liquor tank 5 and the sweat tank 6 are respectively storage containers for mother liquor (residual solution after crystallization, containing a small amount of psicose) and sweat (liquid discharged during heating and sweating, and sweat contains a large amount of psicose) obtained after treatment by the tubular falling film crystallizer 2. The liquid outlet end of the mother liquid tank 5 and the liquid outlet end of the sweat tank 6 are communicated with the first feed inlet. The liquid outlet end of the mother liquid tank 5 and the communication pipeline between the liquid outlet end of the sweat tank 6 and the first feed inlet are respectively provided with a switch valve 12 and a centrifugal pump 11.

Specifically, the mother liquor and the sweat discharged from the first discharge port can be sent into the tubular falling film crystallizer 2 again for crystallization by communicating the mother liquor tank 5 and the sweat tank 6 with the first discharge port and the first feed port, so as to recover the psicose in the mother liquor and the sweat and improve the yield of psicose crystal products.

With continued reference to fig. 1, the first discharge port is connected to the plate-type falling film crystallizer 1 via a pipeline, a cooler 4 and an intermediate product tank 3 are disposed on a pipeline between the first discharge port and the plate-type falling film crystallizer 1, a switch valve 12 is disposed on a pipeline between the first discharge port and the intermediate product tank 3, a switch valve 12 and a centrifugal pump 11 are disposed on a pipeline between the intermediate product tank 3 and the cooler 4, and a switch valve 12 and a centrifugal pump 11 are disposed on a pipeline between the cooler 4 and the plate-type falling film crystallizer 1.

With continued reference to fig. 1, the intermediate product tank 3 is a storage container for liquid intermediate products obtained by preliminary purification, which are discharged after the temperature of the crystal product crystallized on the wall of the crystallization tube of the tubular falling film crystallizer 2 is raised, and the intermediate product tank 3 is located below the tubular falling film crystallizer 2.

With continued reference to fig. 1, the cooler 4 is used for cooling the liquid intermediate product discharged after the temperature is raised, and the cooler 4 may be a tube type cooler, a plate type cooler, an air-cooled cooler, or the like. The shell and tube cooler, the plate cooler and the air-cooled cooler are prior art and are not described herein.

Referring to fig. 2, the plate-type falling film crystallizer includes a casing 101, a second inlet 102 and an outlet 1010 are provided at the top of the casing 101, a second outlet 108 and an inlet are provided at the bottom of the casing 101, a second cold and hot medium outlet 1013 is provided at the upper part of the casing 101, and a second cold and hot medium inlet 1012 and an inlet 107 are provided at the lower part of the casing 101.

With continued reference to fig. 2, the housing 101 is rectangular, square, cylindrical or other shape, the second inlet 102 is flat, and the second inlet 102 is communicated with the cooler 4. The inner diameter of the portion of the communication pipe between the cooler 4 and the second feed port 102 near the second feed port 102 is gradually reduced and flat. The second feed port 102 is used for feeding the liquid intermediate product after preliminary purification into the housing 101. A sealing valve (not shown) is arranged at the second discharging port 102.

Specifically, the part of the communicating pipeline between the cooler 4 and the second feed inlet 102, which is close to the second feed inlet 102, is provided with the inner diameter gradually reduced and is flat, so that the liquid intermediate product can enter the shell 101 in a membranous rather than a strand form, the technical problem of poor crystallization effect caused by the flow of the liquid intermediate product in a strand form is avoided, and the crystallization effect is further improved; by arranging the feed inlet 102 in a flat shape, the liquid intermediate product can enter the shell 101 in a film shape rather than a strand shape, so that the technical problem of poor crystallization effect caused by the flow of the liquid intermediate product in a strand shape is avoided, and the crystallization effect is improved.

With continued reference to fig. 2, the second discharge port is connected to the second feed port 102 via a second material circulation pipe, on which the circulation pump 10 is disposed.

Specifically, the second discharge port is communicated with the second feed port 102 through the second material circulation pipeline, so that the uncrystallized liquid in the intermediate product can be circulated and then sent into the plate-type falling film crystallizer again for crystallization, and the yield of the psicose crystal product is further improved.

With continued reference to fig. 2, the second cooling medium outlet 1013 is connected to the second cooling medium inlet 1012 through a second cooling medium circulation pipe, and the second cooling medium circulation pipe is provided with a circulation pump 10, a refrigerant cooler 13 and a heat medium heat exchanger 14.

Specifically, the second cold and hot medium outlet 1013 is communicated with the second cold and hot medium inlet 1012 through the second cold and hot medium circulation pipeline, and the circulation pump, the refrigerant cooler and the heat medium heat exchanger are arranged on the second cold and hot medium circulation pipeline, so that the cyclic utilization of cold and hot medium can be realized, the utilization rate of the cold and hot medium is improved, and the production cost is reduced.

With continued reference to fig. 2, the gas inlet 107 is configured to introduce high-pressure gas such as high-pressure nitrogen gas, inert gas, etc. into the housing 101.

Specifically, by adding the gas inlet 107, high-pressure gas such as high-pressure nitrogen and inert gas can be introduced into the shell, so that the gas entering from the bottom is in countercurrent contact with the liquid intermediate product in the upward diffusion process, the flow velocity of the liquid intermediate product is reduced, and the psicose in the intermediate product is better crystallized on the wall surface of the crystallization tank 1031; at the same time, volatile substances in the material to be purified can escape and be discharged to the atmosphere through the air outlet 1010.

With continued reference to fig. 2, the housing 101 is provided with a push rod assembly 104, a crystallization plate 103 and a filtering structure 105 in sequence from top to bottom, and a liquid collecting cavity 1014 is provided between the filtering structure 105 and the discharge port 108. The cross section of the portion of the plenum 10104 near the outlet 108 is V-shaped. A sealing valve (not shown) is arranged at the discharge hole 108, the liquid collecting cavity 1014 is communicated with the discharge hole 108, and the liquid collecting cavity 1014 is positioned above the discharge hole 108.

Specifically, by setting the cross section of the portion of the liquid collection chamber 10104 near the discharge port 108 to be V-shaped, it is possible to promote as much material as possible to be discharged through the discharge port, avoiding that the material cannot be completely discharged in the housing 101.

Referring to fig. 3, the crystallization plate 103 is disposed along a vertical direction, the crystallization plate 103 is located above the air inlet 107, and a plurality of crystallization grooves 1031, a plurality of heat exchange cavities 1032 and a plurality of heat exchange grooves 1033 are disposed along the vertical direction of the crystallization plate 103.

Specifically, by opening the crystallization plate 103 in the vertical direction with a plurality of crystallization grooves 1031, crystallization can be performed simultaneously by the plurality of crystallization grooves 1031, and the production efficiency is improved. Through setting up a plurality of heat transfer chamber 1032 and a plurality of heat transfer groove 1033, can carry out the heat exchange through the refrigerant medium in heat transfer chamber 1032 and the heat transfer groove 1033 and the liquid intermediate product simultaneously, be favorable to liquid intermediate product rapid cooling, further improve crystallization effect.

With continued reference to fig. 2-3, the crystallization tank 1031 is connected to the feed port 102 via a feed pipe, and the crystallization tank 1031, the heat exchange chamber 1032 and the heat exchange tank 1033 all penetrate through the crystallization plate 103. A plurality of parallel blocking elements 1023 are arranged in the feeding pipe 1021 along the material flow direction, and the blocking elements 1023 are used for dividing the material entering the feeding pipe 1021 into a plurality of branches so that the material enters different crystallization tanks 1031 through different feeding branches 1022 respectively. The feeding branch pipes 1022 are in one-to-one correspondence with the crystallization tanks 1031, and the cross sections of the feeding branch pipes 1022 near the pipe sections of the crystallization tanks 1031 are arc-shaped. The heat exchange chamber 1032 and the heat exchange grooves 1033 are located in the adjacent areas of the crystallization groove 1031. The blocking member 1023 may be a blocking member made of stainless steel 316 or the like.

Specifically, by arranging a plurality of parallel blocking elements 1023 inside the second feeding pipe 1021 along the material flow direction and arranging the cross section of the feeding manifold 1022 near the pipe section of the crystallization tank 1031 to be arc-shaped, the liquid intermediate product can be split, and then the liquid intermediate product can enter the shell 101 in a film form rather than a strand form, so that the technical problem of poor crystallization effect caused by the flow of the liquid intermediate product in a strand form is avoided, and the crystallization effect is improved.

With continued reference to fig. 4, the heat exchange chamber 1032 is located at the back of the crystallization tank 1031, and the heat exchange tank 1033 is located at the side of the adjacent region of the crystallization tank 1031. The heat exchange cavity 1032 is communicated with the second cold and hot medium inlet 1012 through the cold and hot medium inlet pipe 10121, and the heat exchange cavity 1032 is communicated with the second cold and hot medium outlet 1013 through the cold and hot medium outlet pipe 10131.

Specifically, the heat exchange chamber 1032 is disposed at the back of the crystallization tank 1031, and the heat exchange tank 1033 is disposed at the side of the adjacent area of the crystallization tank 1031, so that heat exchange between the refrigerant medium entering the heat exchange chamber and the liquid intermediate product flowing along the crystallization tank is facilitated, and the psicose in the intermediate product is crystallized on the wall surface of the crystallization tank 1031 better.

With continued reference to fig. 1, the cold and hot medium inlet pipe includes a cold and hot medium inlet main pipe (not shown) and a plurality of cold and hot medium inlet branch pipes (not shown) connected to the cold and hot medium inlet main pipe. The second cold and hot medium outlet pipe comprises a cold and hot medium outlet main pipe (not shown) and a plurality of cold and hot medium outlet branch pipes (not shown) communicated with the cold and hot medium outlet main pipe. The cold and hot medium inlet branch pipe and the cold and hot medium outlet branch pipe are communicated with the heat exchange cavity 1032 and the heat exchange groove 1033, and the cold and hot medium inlet branch pipe and/or the cold and hot medium outlet branch pipe are partially inserted into the heat exchange cavity 1032 and the heat exchange groove 1033. The bottom walls of the heat exchange cavity 1032 and the heat exchange groove 1033 are closed bottom walls, and through holes (not shown) for inserting the cooling and heating medium inlet branch pipes are arranged on the bottom walls of the heat exchange cavity 1032 and the heat exchange groove 1033.

Specifically, the cold medium inlet pipe 1021 and/or the cold medium outlet pipe 1031 are/is partially inserted into the heat exchange groove 1032 of the heat exchange cavity 1032, so that the stroke of the refrigerant medium can be shortened, and the heat exchange effect between the refrigerant medium and the liquid intermediate product is improved, so that the crystallization effect (the crystallization thickness) of the psicose crystals on the crystallization groove is ensured, and the problem of thinner crystallization thickness caused by poor heat exchange effect is avoided.

Referring to fig. 1, the push rod assembly 104 is provided with a plurality of push rods 1041 corresponding to the crystallization tanks 0131 one by one, i.e. the positions of the push rods 1041 correspond to the positions of the crystallization tanks 1031 one by one. The push rod 1041 is disposed along a vertical direction, the shape of the push rod 1041 is matched with the shape of the crystallization tank 1031, and the width of the push rod 1041 is slightly smaller than the width of the crystallization tank 1031. The push rod assembly 104 is provided with a first driving mechanism 1042, a driving shaft of the first driving mechanism 1042 is connected with a connecting block, the connecting block is connected with a first end of the push rod 1041, and the first driving mechanism 1042 is used for driving the push rod 1041 so that the push rod 1041 pushes the crystallization substance to fall from the wall surface of the crystallization tank 1031. The first driving mechanism 1042 may be a hydraulic machine, an air press, a driving machine, or the like. The hydraulic machine, the pneumatic machine and the driving machine are the prior art and are not described in detail herein.

Specifically, by adding the push rod assembly 4, the psicose crystal substance can be pushed off from the wall surface of the crystallization tank 1031, and the yield of the psicose crystal product can be improved. By arranging the push rod 1041 to match the crystallization tank 1031, more psicose crystal product can be pushed off from the wall surface of the crystallization tank 31, and the yield of psicose crystal product can be improved.

With continued reference to fig. 2, the filtering mechanism 105 may be detachably fixed to the inner wall of the housing 101, and the detachable fixing manner may be implemented by using a bolt for fixing, suspending, or the like. The filter mechanism 105 is located between the second inlet 102 and the second outlet 108, and the filter mechanism 105 is located below the crystallization plate 103. The filter mechanism 105 employs a filter screen, and an opening 1051 is provided in the housing 101 near the filter mechanism 105. The opening 1051 is used to manually remove the filter mechanism 105 through the opening 1051.

Referring to fig. 2 and 4, the plate-type falling film crystallizer 1 further includes a cutting mechanism 106, the cutting mechanism 106 is fixedly mounted on an inner wall of the housing 101, the cutting mechanism 106 is disposed along an opposite direction of the crystallization tank 1031, the cutting mechanism 106 is provided with a plurality of cutters 1061 and a second driving mechanism 1062 for driving the cutters 1061 to stretch out and draw back, and the cutters 1061 are disposed in parallel along a direction perpendicular to the crystallization tank 1032, i.e., the cutters 1061 are disposed along a direction perpendicular to a bottom wall of the crystallization tank 1032. The driving shaft of the second driving mechanism 1062 is connected with a connecting block, and all cutters 1061 are connected with the connecting block and the second driving mechanism 1062 can be hydraulic machine, pneumatic machine, driving machine, etc. The cutter 1061 may be a dicing blade or the like. The hydraulic press, the pneumatic press, the driving machine and the dicing blade are prior art and will not be described here.

By additionally arranging the cutting machine 106 which is arranged along the crystallization groove 1031 in opposite directions, the crystal substance can be cut, so that the psicose crystal substance is easier to fall off from the wall surface of the crystallization 1031, and the yield of the psicose crystal product is further improved; through setting up a plurality of cutters 0161 with cutting mechanism 106, cutter 1061 along with the direction parallel arrangement of crystallization groove 1031, can cut the psicose crystal material through a plurality of cutters 1061 simultaneously to make psicose crystal product more easily drop from the crystallization groove 131 wall, further improve the yield of psicose crystal product.

With continued reference to FIG. 2, the falling film crystallizer further includes a spray nozzle 109. The nozzle 109 is fixedly mounted on the inner wall of the housing 11, the nozzle 109 is located above the crystallization tank 1031, and the nozzle 109 is communicated with a high-pressure air inlet pipe (not shown) and/or a high-pressure liquid inlet pipe (not shown). Specifically, in the present embodiment, the showerhead 109 is a rotary showerhead.

Specifically, by connecting the nozzle 109 to the high-pressure air inlet pipe, when sweat separation is performed in the sweating stage, sweat can be blown off (particularly suitable for viscous materials) by using high-pressure gas, so that the purity of the obtained psicose crystal product is improved; when the high-pressure liquid inlet pipe is connected to the nozzle 109, the crystallization tank 1031 and the filtration mechanism 105 can be rinsed with the high-pressure liquid to remove the psicose crystal substance remaining on the wall 1031 of the crystallization tank 1031, thereby improving the yield of the psicose crystal product, and cleaning the filtration mechanism 105 when the crystallization tank 1031 and the filtration mechanism 105 are to be cleaned. Through setting the shower nozzle 109 to adopt rotatory nozzle, can make high-pressure gas and/or high-pressure liquid sweep crystallization tank 1031 and filtering mechanism 105 simultaneously along different angles, further improve the yield of psicose crystal product, reach the better cleaning performance to filtering mechanism 105.

With continued reference to fig. 1, the second outlet 108 is connected to the raffinate tank 8 and/or the sweat tank 9, and the raffinate tank 5 and the sweat tank 6 are located below the plate-type falling film crystallizer 1.

With continued reference to fig. 1, the raffinate tank 8 and the sweat tank 9 are storage containers for raffinate (residual solution after crystallization, containing a small amount of psicose) and sweat (liquid discharged during the heating and sweating stage, and containing a large amount of psicose) obtained after treatment by the plate-type falling film crystallizer 1. The liquid outlet end of the residual liquid tank 5 is communicated with the first feed inlet, the liquid outlet end of the sweat storage tank 6 is communicated with the second feed inlet 102, and the on-off valve 12 and the centrifugal pump 11 are arranged on a communication pipeline between the residual liquid tank 5 and the first feed inlet and a communication pipeline between the liquid outlet end of the sweat storage tank 6 and the second feed inlet 102. Through the liquid outlet end of the residual liquid tank 8 and the sweat storage tank 9 are communicated with the second feed inlet 102, residual liquid and sweat discharged from the second discharge outlet 108 can be respectively fed into the tubular falling film crystallizer 2 and the plate falling film crystallizer 1 for crystallization, so as to recover psicose in the residual liquid and sweat, and improve the yield of psicose crystal products.

The working procedure of the psicose crystal preparation system of this example is as follows:

feeding an 80wt% psicose solution with the temperature of 70-80 ℃ and the concentration of 70wt% into a raw material tank 7, and then pumping the psicose solution into the bottom of a tubular falling film crystallizer 2 by a centrifugal pump 11 for standby;

Starting a circulating pump 10 on a first material circulating pipeline, a circulating pump 10 on a first cold and hot medium circulating pipeline and a refrigerant cooler 13, feeding refrigerant cooling water into a tubular falling film crystallizer 2, feeding a D-psicose solution to a first feed inlet by the circulating pump 10, cooling the psicose solution to 40-45 ℃ at a speed of 3-5 ℃/min, slowly cooling the psicose solution to 30-35 ℃ at a cooling speed of 0.5-1 ℃/min, and then carrying out heat preservation treatment at a temperature of 30-35 ℃ by a cold and hot medium to circulate falling film crystallization for 90-100min; then opening a switch valve 12 on a pipeline between the mother liquor tank 5 and the first discharge port, discharging the mother liquor to the mother liquor tank 5, and weighing and sampling;

the mother solution accumulated by multiple falling film crystallization is enriched and recovered, a switch valve 12 and a centrifugal pump 11 on a communication pipeline between a mother solution tank 5 and a first feed port are opened, and the mother solution obtained by enrichment and recovery is pumped to the bottom of a tubular falling film crystallizer 2 by the centrifugal pump 11 for crystallization;

after the temperature of the crystal on the wall surface of the crystallization tube of the tubular falling film crystallizer 2 is raised to 80-90 ℃ at the speed of 3-5 ℃/min by a heating medium, the internal environment temperature of the tubular falling film crystallizer 2 is raised to 105-110 ℃ at the heating speed of 0.5-1 ℃/min, and then the temperature is kept for 40-50min at the temperature of 105-110 ℃; in the process, the temperature of the crystal substance crystallized on the wall surface of the crystallization tank 1031 is increased, the crystal substance is partially melted to sweat after being heated, the psicose and impurities in the melted sweat are redistributed and enriched, the sweat contains more impurities, and the sweat is gradually discharged outside the crystal layer under the pushing of heat transfer and mass transfer, so that the psicose content in the crystal layer is increased;

In the process, high-pressure nitrogen is fed into the spray head 109 through a high-pressure air inlet pipe, and the high-pressure nitrogen sweeps sweat on the crystal surface on the wall surface of the crystallization tank 101 along different angles, so that viscous sweat is blown off;

then opening a switch valve 12 and a sealing valve at the first discharge port on a pipeline between the sweat tank 6 and the first discharge port, discharging the sweat to the sweat tank 6, and weighing and sampling;

opening a switch valve 12 and a centrifugal pump 11 on a communication pipeline between the sweat tank 6 and the first feed port, pumping sweat to the tubular falling film crystallizer 2 by the centrifugal pump 11 to serve as raw materials for the next batch of crystallization, and closing a sealing valve at the first feed port;

heating to 115-125 ℃ at a heating rate of 0.5-1 ℃/min, carrying out heat preservation treatment at 115-125 ℃ for 30-40min, opening a switch valve 12 and a centrifugal pump 11 on a communication pipeline between the intermediate product tank 3 and a first discharge port after melting is finished, and conveying liquid (i.e. intermediate product) to the intermediate product tank 3 for temporary storage;

the centrifugal pump 11 and the on-off valve 12 on the pipe between the intermediate product tank 3 and the cooler 4 are opened, and the cooler 4 is started. The intermediate product is pumped by a centrifugal pump 11 to the cooler 4 and precooled by the cooler 4 to 60-80 ℃.

Subsequently, the centrifugal pump 11 and the switch valve 12 on the pipeline between the cooler 4 and the second feed port 102 are opened, and the cooled intermediate product is pumped to the plate heat exchanger 1 by the centrifugal pump 11 and enters the crystallization tank 1031 in a membranous form through the feed pipe 1021;

starting a circulating pump 10 and a refrigerant cooler 13 on a second cold and hot medium circulating pipeline to pre-cool, so that the internal environment temperature of the shell 1 is kept at 30-40 ℃;

after all materials enter the plate-type falling film crystallizer 1, starting a circulating pump 10 on a second material circulating pipeline, and keeping the internal temperature of the shell 101 at 30 ℃ for continuous crystallization; in the process, high-pressure nitrogen is sent into the shell 101 through the air inlet 107, the high-pressure nitrogen entering from the air inlet 107 diffuses upwards and contacts with the intermediate product in a countercurrent way in the diffusion process, so that the flow speed of the intermediate product is reduced, and the psicose crystalline substance is better crystallized on the wall surface of the crystallization tank 1031; simultaneously, volatile substances in the intermediate product are allowed to escape and are discharged to the atmosphere through the air outlet 1010;

opening a switch valve 12 on a pipeline between the residual liquid tank 8 and the second discharge port 108 after crystallization is completed, discharging mother liquid to the residual liquid tank 8, weighing and sampling;

enriching and recycling residual liquid accumulated by repeated falling film crystallization; opening a switch valve 12 and a centrifugal pump 11 on a communication pipeline between the residual liquid tank 8 and the first feed port, and pumping residual liquid to the tubular falling film crystallizer 2 by the centrifugal pump 11 for crystallization again;

Starting a circulating pump 10 and a second heat medium heat exchanger 16 on a second cold and heat medium circulating pipeline of the plate-type falling film crystallizer 1 to heat, heating the crystal temperature to 80-90 ℃ at a speed of 3-5 ℃/min through a heat medium, heating the internal environment temperature of the shell 101 to 105-110 ℃ at a speed of 0.5-1 ℃/min, and then preserving heat at the temperature of 105-110 ℃ for 40-50min; in the process, the temperature of the crystallized substances crystallized on the wall surface of the crystallization tank 1031 is increased, the crystallized substances are partially melted after being heated to sweat, the allose and impurities in the melted sweat are redistributed and enriched, the sweat contains more impurities, and the sweat is gradually discharged outside the crystal layer under the pushing of heat transfer and mass transfer, so that the content of the allose in the crystal layer is increased;

in the process, high-pressure nitrogen is fed into the spray head 109 through a high-pressure air inlet pipe, and the high-pressure nitrogen sweeps sweat on the crystal surface on the wall surface of the crystallization tank 1031 along different angles, so that viscous sweat is blown off;

then opening a switch valve 12 on a pipeline between the sweat storage tank 9 and the second discharge port 108 and a sealing valve at the second discharge port 108, discharging the sweat to the sweat storage tank 9, and weighing and sampling;

opening a switch valve 12 and a centrifugal pump 11 on a communication pipeline between the sweat storage tank 9 and the second feed port 102, pumping sweat to the plate-type falling film crystallizer 1 by the centrifugal pump 11 for crystallization again, and closing a sealing valve at the second discharge port 108;

Starting a cutting mechanism 16, driving a cutter 1061 through a second driving mechanism 1062 to cut psicose crystal substances on the wall surface of a crystallization tank 1031 of the tubular falling film crystallizer 2 into blocks, and then starting a first driving mechanism 1042 to drive a push rod 1041 to move towards the crystallization tank 1031, so that the crystal blocks are pushed off from the wall surface of the crystallization tank 1031, and the crystal blocks fall to a filtering mechanism 105;

after the filtering mechanism 15 filters the crystal mixed with the liquid substance, the solid substance such as the crystal block is trapped on the filtering mechanism 15, and the impurities such as the liquid substance fall into the liquid collecting cavity 1014 due to the gravity;

opening the outlet 1051, taking out the filter 105, removing the crystalline material from the filter 105 to obtain a crystal product of psicose, and weighing and sampling the product.

High-pressure water is fed into the spray head 109 through a high-pressure liquid inlet pipe, and the crystallization tank 1031 and the filtering mechanism 105 are rinsed by the high-pressure water;

the sealing valve at the second discharge port 108 is opened, and impurities such as liquid substances in the liquid collection chamber 1014 are discharged from the second discharge port 108 to the outside.

The method of this example was examined to produce D-psicose crystals with a crystallization rate of 100% and a yield of 85.2%, and the purity of the produced D-psicose crystals was 99.8%.

Example 2

As shown in fig. 5, this embodiment differs from embodiment 1 in that: the push rod assembly 104 includes a driving mechanism 1042 and a push rod 1041, a first end of the push rod 1041 is connected with a connecting block, the connecting block is connected with a driving shaft of the driving mechanism 1042, a second end of the push rod 1041 is connected with a push block 1043, and the push block 1043 is matched with the crystallization tank 1031. The driving mechanism 1042 is used for driving the pushing rod 1041 and the pushing block 1043 to move toward the crystallization tank 1031, and further pushing the crystallized material crystallized in the crystallization tank 1031 by the pushing rod 142 from the wall surface of the crystallization tank 31.

Example 3

As shown in the assembled view of the crystallization plate and the case in fig. 6, this embodiment is different from embodiment 1 in that: the crystallization plate 103 is fixedly installed on the inner wall of the housing 101, and a space between the crystallization plate 103 and the housing 101 forms a heat exchange chamber 1032 and a heat exchange groove 1033.

Example 4

As shown in fig. 7, the psicose crystal production system of the present embodiment further comprises a solvent tank 15 and a condenser 16.

With continued reference to fig. 7, the solvent tank 15 is a storage container for a solvent such as ethanol, and the solvent tank 15 stores the solvent such as ethanol. The liquid outlet end of the solvent tank 15 is communicated with the bottom of the shell 101 through a pipeline, and the gas outlet 1010 is communicated with the liquid inlet end of the solvent tank 15 through a pipeline. By additionally arranging the solvent tank 15 and communicating the liquid outlet end of the solvent tank 15 with the bottom of the shell 101 through a pipe, the solvent such as ethanol can be fed into the shell 101, so that the solvent such as ethanol can dissolve the uncrystallized liquid in the intermediate product, the flow rate of the uncrystallized liquid in the intermediate product is improved, the problem that the uncrystallized liquid in the intermediate product cannot be effectively and circularly crystallized due to overlarge viscosity is avoided, and the yield of the psicose crystal product is further improved.

With continued reference to fig. 7, the condenser 16 is configured to cool the solvent such as ethanol that is discharged from the plate-type falling film crystallizer 1 and is converted into a gaseous state after being heated, so that the solvent such as ethanol is cooled and is converted into a liquid state, and then the liquid state is pumped into the solvent tank 15 by the centrifugal pump 11, so as to realize recycling of the solvent such as ethanol. The condenser 16 may be a water-cooled condenser, an air-cooled condenser, a water-air-cooled condenser, or the like. The water-cooled condenser, the air-cooled condenser, and the water-air cooled condenser are prior art and are not described herein. By additionally arranging the condenser 16, the solvents such as ethanol and the like can be recycled, the recycling rate of the solvents such as ethanol and the like is improved, the production cost is reduced, and the income is improved;

this embodiment also differs from embodiment 1 in that: the absolute ethyl alcohol stored in the solvent tank 15 is pumped to the crystallization tank 1031 by the centrifugal pump 11, the absolute ethyl alcohol dissolves the psicose, so that the psicose material which is remained on the wall surface of the crystallization tank 1031 and is difficult to fall off is caused to flow at a certain speed so as to be crystallized, and the yield of the psicose crystal product is further improved; in the sweating stage, the ambient temperature in the shell 101 rises, absolute ethyl alcohol volatilizes into gas, is discharged from the gas outlet 1010, enters the condenser 16, is converted into liquid absolute ethyl alcohol after being treated by the condenser 16, and flows into the solvent tank 15 through the pipe.

It should be understood that the crystallization plate may be provided with only the heat exchange chamber or the heat exchange groove, and it is not necessary to provide the heat exchange chamber and the heat exchange groove at the same time, in this application, without being limited thereto. The first feed inlet can also be arranged at the upper part of the tubular falling film crystallizer.

In the application, a second cooling and heating medium inlet communicated with the heat exchange cavity may be formed in the upper portion of the shell, and a second cooling and heating medium outlet communicated with the heat exchange cavity may be formed in the lower portion of the shell.

The above embodiments are merely illustrative of the principles of the present utility model and its effectiveness, and are not intended to limit the utility model. Modifications and variations may be made to the above-described embodiments by those skilled in the art without departing from the spirit and scope of the utility model. Accordingly, it is intended that all equivalent modifications and variations of the utility model be covered by the claims, which are within the ordinary skill of the art, be within the spirit and scope of the present disclosure.

Claims

1. The utility model provides an allulose crystal preparation system, a serial communication port, including the tubular falling film crystallizer that communicates in proper order, cooler and board-like falling film crystallizer, tubular falling film crystallizer is provided with first cold and hot medium import, first cold and hot medium export, first feed inlet and first discharge gate, board-like falling film crystallizer includes the casing, second feed inlet and gas outlet have been seted up at the casing top, second discharge gate and air inlet have been seted up to the casing bottom, the inside crystallization board that sets up along vertical direction that is provided with of casing, crystallization board is provided with crystallization tank and heat transfer chamber along vertical direction, crystallization tank intercommunication second feed inlet, the heat transfer chamber is located crystallization tank adjacent region, the casing lower part is equipped with the second cold and hot medium import with the heat transfer chamber intercommunication, the second cold and hot medium export with the heat transfer chamber intercommunication has been seted up to casing top and bottom, air inlet and gas outlet are located crystallization board below respectively.

2. The psicose crystal production system of claim 1, wherein the first outlet is in communication with a mother liquor tank and/or a sweat tank, the mother liquor tank and/or sweat tank being in communication with the first inlet.

3. The psicose crystal preparation system according to claim 1, wherein the first discharge port is communicated with the first feed port through a first material circulation pipeline, and a circulation pump is arranged on the first material circulation pipeline;

and/or the first cold and hot medium outlet is communicated with the first cold and hot medium inlet through a first cold and hot medium circulation pipeline, and a circulation pump, a refrigerant cooler and a hot medium heat exchanger are arranged on the first cold and hot medium circulation pipeline.

4. The psicose crystal preparation system according to claim 1, wherein the crystallization plate is provided with a plurality of crystallization grooves along a vertical direction;

and/or, the inside of the plate-type falling film crystallizer is also provided with a push rod assembly, the push rod assembly is positioned above the crystallization plate, the push rod assembly comprises a first driving mechanism and a push rod corresponding to the crystallization tank, the driving mechanism is used for driving the push rod so that the push rod pushes crystalline substances crystallized in the crystallization tank to fall from the wall surface of the crystallization tank, and the push rod is arranged along the vertical direction;

And/or, the plate-type falling film crystallizer further comprises a cutting mechanism, the cutting mechanism is fixedly arranged on the inner wall of the shell, the cutting mechanism is arranged along the opposite direction of the crystallization groove, the cutting mechanism is provided with a cutter and a second driving mechanism for driving the cutter to stretch out and draw back, and the cutter is arranged along the direction perpendicular to the crystallization groove;

and/or; the plate-type falling film crystallizer further comprises a spray head, wherein the spray head is positioned in the shell and above the crystallization tank, and the spray head is communicated with a high-pressure air inlet pipe and/or a high-pressure liquid inlet pipe;

and/or; the plate type falling film crystallizer further comprises a filtering mechanism, the filtering mechanism is detachably fixed on the inner wall of the shell, the filtering mechanism is positioned between the second feeding hole and the second discharging hole, the filtering mechanism is positioned below the crystallization plate, and an opening is formed in the part, close to the filtering mechanism, of the shell; and/or a pipeline which is communicated with the heat exchange cavity and the second cold and hot medium inlet and/or a pipeline which is communicated with the heat exchange cavity and the second cold and hot medium outlet extend into the heat exchange cavity.

5. The psicose crystal production system according to claim 4, wherein the cutting mechanism is provided with a plurality of cutters, all of which are arranged in parallel in a direction perpendicular to the crystallization tank;

And/or the spray head adopts a rotary spray head;

and/or the push rod is matched with the crystallization tank.

6. The psicose crystal preparation system of claim 1, wherein the crystallization plate is further provided with a heat exchange groove, the heat exchange groove is located in an adjacent area of the crystallization groove, and the heat exchange groove is communicated with the second cold and heat medium inlet and the second cold and heat medium outlet.

7. The psicose crystal production system according to claim 6, wherein a pipe connecting the heat exchange tank with the second cooling medium inlet and/or a pipe connecting the heat exchange tank with the second cooling medium outlet partially extends into the heat exchange tank.

8. The psicose crystal preparation system according to claim 1, wherein the second discharging port is further communicated with a residual liquid tank and/or a sweat storage tank, the residual liquid tank is communicated with the first feeding port, and the sweat storage tank is communicated with the second feeding port;

and/or the second discharge port is communicated with the second feed port through a second material circulating pipeline, and a circulating pump is arranged on the second material circulating pipeline;

and/or the second cold and hot medium outlet is communicated with the second cold and hot medium inlet through a second cold and hot medium circulation pipeline, and a circulation pump, a refrigerant cooler and a hot medium heat exchanger are arranged on the second cold and hot medium circulation pipeline.

9. The psicose crystal production system of claim 8, further comprising a solvent tank in communication with the bottom of the housing via a pipe.

10. The psicose crystal production system of claim 9, wherein the air outlet is communicated with the solvent tank through a pipeline, and a condenser is arranged on a communicating pipeline between the air outlet and the solvent tank.