CN115160386A - Production method and production system of psicose crystals - Google Patents
Production method and production system of psicose crystals Download PDFInfo
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- CN115160386A CN115160386A CN202210968665.6A CN202210968665A CN115160386A CN 115160386 A CN115160386 A CN 115160386A CN 202210968665 A CN202210968665 A CN 202210968665A CN 115160386 A CN115160386 A CN 115160386A
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- 239000013078 crystal Substances 0.000 title claims abstract description 123
- LKDRXBCSQODPBY-JDJSBBGDSA-N D-allulose Chemical compound OCC1(O)OC[C@@H](O)[C@@H](O)[C@H]1O LKDRXBCSQODPBY-JDJSBBGDSA-N 0.000 title claims abstract description 107
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 48
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- 230000008025 crystallization Effects 0.000 claims abstract description 177
- 238000010438 heat treatment Methods 0.000 claims abstract description 139
- 239000011552 falling film Substances 0.000 claims abstract description 98
- 239000007788 liquid Substances 0.000 claims abstract description 92
- 239000013067 intermediate product Substances 0.000 claims abstract description 56
- 238000001816 cooling Methods 0.000 claims description 99
- 210000004243 sweat Anatomy 0.000 claims description 79
- 230000007246 mechanism Effects 0.000 claims description 77
- 239000000463 material Substances 0.000 claims description 36
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- 238000001914 filtration Methods 0.000 claims description 28
- 239000007921 spray Substances 0.000 claims description 24
- 238000003860 storage Methods 0.000 claims description 24
- 238000005520 cutting process Methods 0.000 claims description 23
- 239000003507 refrigerant Substances 0.000 claims description 19
- 238000007599 discharging Methods 0.000 claims description 16
- 230000035900 sweating Effects 0.000 claims description 16
- 238000004891 communication Methods 0.000 claims description 14
- 238000002844 melting Methods 0.000 claims description 10
- 230000008018 melting Effects 0.000 claims description 10
- 238000011084 recovery Methods 0.000 claims description 4
- 239000000126 substance Substances 0.000 abstract description 25
- 238000000034 method Methods 0.000 description 36
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- 230000008569 process Effects 0.000 description 19
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- BJHIKXHVCXFQLS-PUFIMZNGSA-N D-psicose Chemical compound OC[C@@H](O)[C@@H](O)[C@@H](O)C(=O)CO BJHIKXHVCXFQLS-PUFIMZNGSA-N 0.000 description 13
- 230000000694 effects Effects 0.000 description 13
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- BJHIKXHVCXFQLS-ZXEDONINSA-N L-psicose Chemical compound OC[C@H](O)[C@H](O)[C@H](O)C(=O)CO BJHIKXHVCXFQLS-ZXEDONINSA-N 0.000 description 10
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H3/00—Compounds containing only hydrogen atoms and saccharide radicals having only carbon, hydrogen, and oxygen atoms
- C07H3/02—Monosaccharides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0018—Evaporation of components of the mixture to be separated
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0059—General arrangements of crystallisation plant, e.g. flow sheets
-
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- Biotechnology (AREA)
- General Health & Medical Sciences (AREA)
- Genetics & Genomics (AREA)
- Molecular Biology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention belongs to the technical field of chemical industry, and particularly relates to a production method and a production system of psicose crystals, wherein the production method comprises the following steps: s1, sending the allulose solution into a tubular falling film crystallizer for crystallization, then heating to melt the obtained crystals into liquid state to obtain an intermediate product, and S2, precooling the intermediate product, and then sending the precooled intermediate product into a plate-type falling film crystallizer for crystallization to obtain allulose crystals.
Description
Technical Field
The invention belongs to the technical field of chemical industry, and particularly relates to a production method and a production system of allulose crystals.
Background
With the improvement of living standard, people are increasingly concerned about the problems of food safety and the like, especially various functional additives. Allulose is a popular low-calorie sweetener in the food industry because it has a high sweetness and is not easily digested. In the field of medicine, psicose also has the effects of reducing in vivo fat accumulation, inhibiting the increase in blood glucose concentration, improving insulin sensitivity and glucose tolerance, and the like. However, allulose is contained in a very small amount in nature, is difficult to meet market demands, and generally needs to be artificially synthesized.
Psicose belongs to hexulose, is a six-carbon sugar, and is an epimer corresponding to the third carbon of D-fructose. The synthetic method of the psicose comprises a chemical synthesis method and a biological enzyme method. The chemical synthesis method for producing the psicose has the following defects: 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 application. Compared with a chemical synthesis method, the enzymatic synthesis method for the psicose has great advantages: 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, biotransformation of psicose is the focus and focus of current research.
However, commercial psicose is basically a liquid product or a powdery solid product, when the psicose is at a high degree of supersaturation, crystals grow faster than crystals, fine crystals are easily generated, the solution viscosity is increased, and the growth of large crystals is not facilitated, if the psicose is subjected to multiple heating concentration and cooling crystallization processes, the production process is complex and is not easy to operate, and the granularity of the generated psicose crystals is small, so that the yield of the psicose crystals is only about 20-30%, and the production economy of the psicose crystal products is seriously affected.
In the related technology, 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 consumption is long, the energy consumption is high, the actual production economy is poor, the prepared product crystals are granular, the crystals are small, and the yield is low.
Disclosure of Invention
In view of the above disadvantages of the prior art, the present invention aims to provide a method and a system for producing psicose crystals, which are used to solve the technical problems of complicated process flow, long time consumption, high energy consumption, poor economical efficiency of actual production, granular crystal of the prepared product, small crystal and low yield in producing psicose crystals by using the existing equipment and method.
In a first aspect, the present application provides a method for producing allulose crystals, comprising the steps of:
s1, feeding the allulose solution into a tubular falling film crystallizer for crystallization, and then heating to melt the obtained crystals into liquid to obtain an intermediate product;
s2, precooling the intermediate product, and then sending the intermediate product into a plate-type falling film crystallizer for crystallization to obtain the psicose crystal.
It should be noted that the "psicose crystal" referred to herein means a D-psicose crystal, an L-psicose crystal or a D-psicose crystal/L-psicose crystal mixed crystal, i.e., the production system of the present application is applicable to the production of a D-psicose crystal, an L-psicose crystal or a D-psicose crystal/L-psicose crystal mixed crystal.
Optionally, in step S1, the allulose solution has a concentration of 70wt% to 80wt%, preferably 75wt% to 80wt%.
Optionally, in step S1, the temperature of the allulose solution is 80-120 ℃, preferably 100-120 ℃.
Optionally, in step S1, the crystallizing comprises: firstly, cooling to 40-45 ℃ at the speed of 3-5 ℃/min, preferably to 42-45 ℃ at the speed of 4-5 ℃/min; then cooling to 30-35 deg.C at a rate of 0.5-1 deg.C/min, preferably to 30-32 deg.C at a rate of 0.6-1 deg.C/min; then crystallizing at 30-35 deg.C for 90-100min.
Optionally, in step S1, a sweating step is further included after the crystallization and before the melting.
Optionally, in step S1, the melting comprises: heating to 115-125 deg.C at a rate of 0.5-1 deg.C/min, preferably to 120-125 deg.C at a rate of 0.6-1 deg.C/min; then preserving heat for 30-40min at the temperature of 115-125 ℃ to obtain an intermediate product, and then preserving heat for 30-40min at the temperature of 120-125 ℃.
Optionally, the sweating comprises: heating to 80-90 deg.C at 3-5 deg.C/min, preferably heating to 85-90 deg.C at 4-5 deg.C/min; then heating to 105-110 ℃ at the speed of 0.5-1 ℃/min, preferably heating to 105-110 ℃ at the speed of 0.6-1 ℃/min; then preserving heat at 105-110 deg.C for 40-50min to obtain sweat.
Optionally, the production method further comprises: and (2) enriching the mother liquor and/or sweat obtained in the step (S1), and feeding the enriched and recovered mother liquor and/or sweat into a tubular falling film crystallizer for crystallization.
Optionally, in step S2, the intermediate product is cooled to 60-80 ℃, preferably 60-75 ℃.
Optionally, in step S2, the crystallizing comprises: firstly, cooling to 30-40 ℃, preferably 30-35 ℃; then crystallizing at 30-40 deg.C.
Optionally, in step S2, a sweating step is further included after the crystallization.
Optionally, in step S2, the sweating comprises: heating to 80-90 deg.C at 3-5 deg.C/min, heating to 105-110 deg.C at 0.5-1 deg.C/min, preferably heating to 85-90 deg.C at 4-5 deg.C/min, heating to 105-110 deg.C at 0.6-1 deg.C/min, and maintaining at 105-110 deg.C for 40-50min; then preserving heat at 105-110 deg.C for 40-50min to obtain sweat.
Optionally, the production method further comprises: and (3) enriching and recovering the mother liquor obtained in the step (S2), and feeding the enriched and recovered mother liquor into a tubular falling film crystallizer for crystallization.
Optionally, the production method further comprises: and (3) enriching and recovering the sweat obtained in the step (S2), and feeding the sweat after enrichment and recovery into a plate-type falling film crystallizer for crystallization.
In another aspect, the invention further provides a production system adopted by the production method of the psicose crystal, 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 cooling and heating medium inlet, a first cooling and heating medium outlet, a first feeding hole and a first discharging hole, the plate-type falling-film crystallizer comprises a shell, the top of the shell is provided with a second feeding hole and a gas outlet, the bottom of the shell is provided with a second discharging hole and a gas inlet, the second feeding hole is flat, a crystallization plate arranged in the vertical direction is arranged in the shell, 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 feeding hole through a feeding pipe, the heat exchange cavity is located in an adjacent area of the crystallization groove, the lower part of the shell is provided with a second cooling and heating medium inlet communicated with the heat exchange cavity, the upper part of the shell is provided with a second cooling and heating medium outlet communicated with the heat exchange cavity, the top of the shell and the bottom of the shell are respectively provided with a gas inlet and a gas outlet, and the gas inlet is located below the crystallization plate.
Optionally, the first discharge port is communicated with a mother liquor tank and/or a sweat tank, and the mother liquor tank and/or the sweat tank are communicated with the first feed port.
Optionally, the first discharge hole is communicated with the feed inlet through a first material circulating pipeline, and a circulating pump is arranged on the first material circulating pipeline.
The first cooling and heating medium outlet is communicated with the first cooling and heating medium inlet through a first cooling and heating medium circulating pipeline, and a circulating pump, a refrigerant cooler and a heating medium heat exchanger are arranged on the Leng Di heating medium circulating pipeline.
Optionally, the crystallization plate is provided with a plurality of crystallization grooves along the vertical direction.
Optionally, 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 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 position, close to the filtering mechanism, of the shell.
Optionally, a pipeline for communicating the heat exchange cavity with the cold and hot medium inlet and/or a pipeline part for communicating the heat exchange cavity with the cold and hot medium outlet extends into the heat exchange cavity.
Optionally, the second discharge hole is communicated with the second feed inlet through a second material circulating pipeline, and a circulating pump is arranged on the second material circulating pipeline.
Optionally, the second cooling medium outlet is communicated with the second cooling medium inlet through a second cooling medium circulation pipeline, and a circulation pump, a cooling medium cooler and a heating medium heat exchanger are arranged on the second heating medium circulation pipeline.
Optionally, the crystallization plate is further provided with a heat exchange groove, the refrigerant heat exchange groove is located in an area adjacent to the crystallization groove, and the heat exchange groove is communicated with the second refrigerant inlet and the second refrigerant outlet.
Optionally, the second discharge port is further communicated with a residual liquid tank and/or a sweat storage tank, the residual liquid tank is communicated with the first feed port, and the sweat storage tank is communicated with the second feed port.
Optionally, the inside push rod subassembly that still sets up of board-like falling film crystallizer, the push rod subassembly is located crystallization plate top, the push rod subassembly include a 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 the crystallization material in the crystallization tank and push away from the crystallization tank wall, the push rod sets up along vertical direction.
Optionally, plate-type falling film crystallizer still includes the mechanism of surely making, surely make mechanism fixed mounting in shells inner wall, surely make the mechanism follow the subtend setting of crystallizer tank, surely make the mechanism be provided with the cutter and be used for the drive the flexible second actuating mechanism of cutter, the cutter along with crystallizer tank vertically direction sets up.
Optionally, the plate-type falling film crystallizer further comprises a spray head, the spray head is located 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.
Optionally, the second discharge port is further communicated with a residual liquid tank and/or a sweat storage tank, and a liquid outlet end of the residual liquid tank and/or the sweat storage tank is communicated with the second feed port.
Optionally, the cutting mechanism is provided with a plurality of cutters, and all the cutters are arranged in parallel along a direction perpendicular to the crystallization tank.
Optionally, the spray head is a rotary spray head.
Optionally, the push rod is matched with the crystallization groove.
Optionally, a pipeline for communicating the heat exchange groove with the second cooling medium inlet and/or a pipeline part for communicating the heat exchange groove with the second cooling medium outlet extends into the heat exchange groove.
Optionally, the allulose crystal production system further comprises a solvent tank in communication with the bottom of the housing via a pipe.
Optionally, the gas outlet is communicated with the solvent tank through a pipeline, and a condenser is arranged on the communication pipeline between the gas outlet and the solvent tank.
The invention has the beneficial effects that:
the method combines a tubular falling film crystallizer and a plate falling film crystallizer to produce the allulose crystal product, and the crystallization rate reaches 99.99%.
According to the method, the allulose crystal product is produced by combining the tubular falling film crystallizer and the plate type falling film crystallizer, the purity of the obtained allulose crystal product is high, and the requirements of food-grade and medical-grade application can be met.
The allulose crystal product produced by the method is blocky, and the technical problems that the crystal of the product is granular and the crystal is small when the allulose crystal is produced by the existing method and equipment are solved.
The psicose crystal product produced by the method can meet the requirements without carrying out decoloring treatment, so that the decoloring process step is omitted, the process flow is reduced, the process time is shortened, the yield is improved, and the cost is reduced.
The allulose crystal product produced by the method has the advantages of short process time, low energy consumption and high utilization rate of raw materials.
The method for producing the psicose crystal product has the advantages of simple process flow, easy industrial realization and high economical efficiency.
Drawings
Fig. 1 is a schematic structural view of an psicose crystal production system of example 1;
fig. 2 is a schematic structural view of a plate-type falling film crystallizer in fig. 1;
FIG. 3 is a schematic structural view of the crystallization plate of FIG. 2;
FIG. 4 is a perspective view of the cutting mechanism of FIG. 2 in cooperation with a crystallization plate;
fig. 5 is a schematic structural view of a push rod assembly of a falling film crystallizer of the psicose crystal production system of example 5;
fig. 6 is an assembly view of a crystallization plate and a shell of a falling film crystallizer of the allulose crystal preparation system of example 6;
fig. 7 is a schematic structural view of the psicose crystal production system of example 7.
Reference numerals
1-plate falling film crystallizer; 101-a housing; 102-second feed inlet, 1021-feed pipe, 1022-feed manifold, 1023-blocking element; 103-crystallization plate, 1031-crystallization tank, 1032-heat exchange cavity and 1033-heat exchange tank; 104-a push rod assembly, 1041-a push rod, 1042-a first driving mechanism, 1043-a push block; 105-filter mechanism, 1051-opening; 106-a cutting mechanism, 1061-a cutter, 1062-a second driving mechanism; 107-air inlet; 108-a second discharge port; 109-a spray head; 1010-air outlet; 1012-a second cooling and heating medium inlet, 10121-a cooling and heating medium inlet pipe; 1013-a second cooling medium outlet, 10131-a cooling medium outlet pipe;
2-tubular falling film crystallizer;
3-intermediate product tank;
4-a cooler;
5-mother liquor tank;
6-a sweat tank;
7-a raw material tank;
8-a residue tank;
9-a sweat storage tank;
10-a circulating pump;
11-a centrifugal pump;
12-a switching valve;
13-a refrigerant cooler;
14-heat medium heat exchanger;
15-solvent tank;
16-a condenser.
Detailed Description
The following embodiments of the present invention are provided by way of specific examples, and other advantages and effects of the present invention will be readily apparent to those skilled in the art from the disclosure herein. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention.
It should be noted that the drawings provided in the present embodiment are only for illustrating the basic idea of the present invention, and the components related to the present invention are only shown in the drawings rather than drawn according to the number, shape and size of the components in actual implementation, and the type, quantity and proportion of the components in actual implementation may be changed freely, and the layout of the components may be more complicated. The structures, proportions, sizes, and other dimensions shown in the drawings and described in the specification are for understanding and reading the present disclosure, and are not intended to limit the scope of the present disclosure, which is defined in the claims, and are not essential to the art, and any structural modifications, changes in proportions, or adjustments in size, which do not affect the efficacy and attainment of the same are intended to fall within the scope of the present disclosure. Meanwhile, the terms such as "upper", "lower", "top", "bottom", "vertical", and the like, referred to in the present specification, are used for clarity of description only, and are not used to limit the scope of the invention, and the relative relationship between the terms may be changed or adjusted without substantial technical change. It should be understood that the terms "inner and outer" are used herein to refer to the interior and exterior relative to the profile of the respective component itself.
In the description of the present invention, it should be understood that the terms "first", "second", etc. are used to define the components, and are used only for the convenience of distinguishing the corresponding components, and if not otherwise stated, the terms have no special meaning, and thus, should not be construed as limiting the scope of the present invention.
The application provides a production method of psicose crystals, which comprises the following steps:
s1, feeding a 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 ℃; subsequently sweating is carried out, specifically: heating to 80-90 deg.C at a rate of 3-5 deg.C/min, heating to 105-110 deg.C at a rate of 0.5-1 deg.C/min, and maintaining at 105-110 deg.C for 40-50min to obtain sweat; then melting is carried out, specifically: heating to 115-125 deg.C at a rate of 0.5-1 deg.C/min, maintaining at 115-125 deg.C for 30-40min to obtain intermediate product, and maintaining at 120-125 deg.C for 30-40min to obtain liquid intermediate product; enriching and recovering mother liquor generated in the crystallization process and sweat obtained in the sweating process, and sending the mother liquor and the sweat obtained by enrichment and recovery into a tubular falling film crystallizer for crystallization;
s2, precooling the intermediate product to 60-80 ℃, and then sending the intermediate product into a plate-type falling film crystallizer for crystallization, wherein the method specifically comprises the following steps: firstly, cooling to 30-40 ℃, and then crystallizing at the temperature of 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 for 40-50min at the temperature of 105-110 ℃; then preserving heat for 40-50min at 105-110 ℃ to obtain sweat; and (3) sending the 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 the 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-type falling-film crystallizer which are sequentially communicated;
the tubular falling film crystallizer is provided with a first feed inlet, a first discharge outlet, a first cooling and heating medium inlet and a first cooling and heating medium outlet, 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 are communicated with the first feed inlet, the first discharge outlet is communicated with the first feed inlet through a first material circulating pipeline, the first material circulating pipeline is provided with a circulating pump, the first cooling and heating medium outlet is communicated with the first cooling and heating medium inlet through the first cooling and heating medium circulating pipeline, and the first cooling and heating medium circulating pipeline is provided with a circulating pump, a cooling medium cooler and a heating medium heat exchanger;
the plate-type falling film crystallizer comprises a shell, wherein a second feed port and a gas outlet are formed in the top of the shell, the second feed port is flat, a second discharge port and a gas inlet are formed in the bottom of the shell, the second discharge port is communicated with the second feed port through a second material circulating pipeline, and a push rod assembly, a crystallization plate, a filtering 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 grooves, a plurality of heat exchange cavities and a plurality of heat exchange grooves along the vertical direction, the crystallization grooves are communicated with a feed inlet through a feed pipe, the heat exchange cavities are positioned in the adjacent areas of the crystallization grooves, the lower part of the shell is provided with a second cooling and heating medium inlet communicated with the heat exchange cavities, the upper part of the shell is provided with a second cooling and heating medium outlet communicated with the heat exchange cavities, the second cooling and heating medium outlet is communicated with a second cooling and heating medium inlet through a second cooling and heating medium circulation pipeline, and the second cooling and heating medium circulation pipeline is provided with a circulation pump, a cooling medium cooler and a heating medium heat exchanger;
the top of the shell 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 cooling and heating medium inlet and the second cooling and heating medium outlet; a pipeline for communicating the heat exchange cavity with the second cooling and heating medium inlet and/or a pipeline part for communicating the heat exchange cavity with the second cooling and heating medium outlet extend into the heat exchange cavity; a pipeline for communicating the heat exchange groove with the second cooling and heating medium inlet and/or a pipeline part for communicating the heat exchange groove with the second cooling and heating medium outlet extends 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 can push the crystallized substances crystallized in the crystallization grooves down from the wall surfaces of the crystallization grooves, and the push rods are arranged along the vertical direction;
the plate-type falling film crystallizer also comprises a cutting mechanism, the cutting mechanism is fixedly arranged on the inner wall of the shell and is arranged along the opposite direction of the crystallization tank, the cutting mechanism is provided with a plurality of cutters and a second driving mechanism for driving the cutters to stretch, and all the cutters are arranged in parallel along the direction vertical to the crystallization tank;
the plate-type falling film crystallizer also comprises a spray head, 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 are communicated with the second feed port.
In another embodiment of the application, the bottom of the shell is also communicated with a solvent tank, the solvent tank is communicated with the air outlet through a pipeline, and a condenser is arranged on a communication pipeline between the air outlet and the solvent tank.
In another embodiment of the present application, the push rod is matched to the crystallization groove.
The present invention will be described in detail below with reference to specific exemplary embodiments. It should also be understood that the following examples are illustrative only and are not to be construed as limiting the scope of the invention, and that numerous insubstantial modifications and adaptations of the invention described above will occur to those skilled in the art. The specific process parameters and the like of the following examples are also only one example of suitable ranges, i.e., those skilled in the art can select the appropriate ranges through the description herein, and are not limited to the specific values exemplified below. In the present invention, "wt%" means a mass content unless otherwise specified.
In the present application, the method for calculating the crystallization rate is as follows: crystallization rate = crystal mass in final product/final product mass;
in the present application, the yield is calculated by the following formula:
in the application, the purity is detected by referring to a Chinese and foreign standard method in Q/CBL 0009S-2016D-psicose Enterprise Standard, and it is noted that when the raw material is L-psicose solution, D-psicose in the Standard needs to be replaced by L-psicose.
Example 1
Referring to fig. 1, fig. 1 is a schematic structural diagram of an psicose crystal production system of the present embodiment, which is used for producing an psicose crystal product.
As shown in fig. 1, the allulose crystal preparation system of the present embodiment includes a tubular falling film crystallizer 2, a cooler 4, and a plate-type falling film crystallizer 1, which are connected in sequence.
With continued reference to fig. 1, the tube-type falling film crystallizer 1 is a crystallization apparatus with crystallization tubes as crystallization elements. The bottom of the tubular falling film crystallizer 2 is provided with a first feeding hole (not shown) and a first discharging hole (not shown), the upper part of the tubular falling film crystallizer 2 is provided with a first cooling and heating medium inlet (not shown), and the lower part of the tubular falling film crystallizer 2 is provided with a first cooling and heating medium outlet (not shown).
Referring to fig. 1, the first discharge hole is connected to the first feed hole through a first material circulation pipeline, and a circulation pump 10 is disposed on the first material circulation pipeline. The circulating pump is prior art and is not described in detail herein.
Specifically, the first discharge hole is communicated with the first feed inlet through the first material circulating pipeline, so that uncrystallized liquid in the material to be purified can be circulated and then sent into the tubular falling film crystallizer 2 for crystallization, and the yield of the psicose crystal product is further improved.
With reference to fig. 1, the first cooling and heating medium inlet is used to introduce cooling and heating media (cooling water may be used as the cooling medium, and heat transfer oil may be used as the heating medium) into the tubular falling film crystallizer 2, and the first cooling and heating medium outlet is used to discharge the cooling and heating media 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.
Referring to fig. 1, the cooling medium cooler 13 is used for cooling the cooling medium (cooling water may be used as the cooling medium) with a raised temperature after heat exchange (crystallization stage), so that the cooling medium is sent into the tubular falling film crystallizer 2 again to exchange heat with the material to be purified that is not crystallized, and the material to be purified that is primarily crystallized is recrystallized again, thereby increasing the yield of the psicose crystals. The heat medium heat exchanger 14 is configured to heat a heat medium (the heat medium may be heat exchange oil or the like) having a reduced temperature after heat exchange (at a sweating and melting stage), so that the heat medium is introduced into the tubular falling film crystallizer 2 again through the first cooling-heating medium circulation pipeline to exchange heat with a crystal substance obtained again on a wall of the crystallization tube, thereby improving the purity of the psicose crystal. The refrigerant cooler 13 may be a tube cooler, a plate 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. Tube falling film crystallizer, switch valve, centrifugal pump, tube type cooler, plate cooler, air-cooled cooler, dividing wall type heat exchanger, hybrid heat exchanger, regenerative heat exchanger, etc. are prior art, and are not described herein again.
Particularly, the first cooling and heating medium outlet is communicated with the first cooling and heating medium inlet through the first cooling and heating medium circulating pipeline, and the second cooling and heating medium circulating pipeline is provided with the circulating pump, the refrigerant cooler and the heating medium heat exchanger, so that the cooling and heating media can be recycled, the utilization rate of the cooling and heating media is improved, and the production cost is reduced.
Referring to fig. 1, the first feed inlet is connected to a material tank 7, and a connection pipe between the material tank 7 and the first feed inlet is provided with a centrifugal pump 11 and a switch valve 12. The raw material tank 7 is used as a storage place for a crystallization raw material to be purified, namely, an psicose solution, and the psicose solution with the concentration of 70wt% -80wt% is stored in the raw material tank 7. And a communicating pipeline between the raw material tank 7 and the first feed inlet is provided with a switch valve 12 and a centrifugal pump 11.
With continued reference to fig. 1, the first outlet is connected to a mother liquor tank 5 and a sweat tank 6. The mother liquor tank 5 and the 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 communicated with the first discharge port through a pipeline, and the communicating pipeline between the first discharge port and the mother liquid tank 5 and the communicating pipeline between the first discharge port and the sweat tank 6 are provided with switch valves 12. A 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 inlet is provided with a switch valve 12 and a centrifugal pump 11.
Referring to fig. 1, a sealing valve (not shown) is disposed at the first discharge port, and the mother liquor tank 5 and the sweat tank 6 are respectively storage containers of mother liquor (residual solution after crystallization, mother liquor containing a small amount of psicose) and sweat (liquid discharged during the heating and sweating stage, sweat containing a large amount of psicose) obtained after treatment by the tube-type 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 both communicated with the first feed inlet. The communicating pipelines between the liquid outlet end of the mother liquid tank 5 and the first feed inlet and the liquid outlet end of the sweat tank 6 are both provided with a switch valve 12 and a centrifugal pump 11.
Specifically, the mother liquor tank 5 and the sweat tank 6 are communicated with the first discharge hole and the first feed inlet, so that the mother liquor and sweat discharged from the first discharge hole can be sent into the tubular falling film crystallizer 2 again for crystallization, allulose in the mother liquor and sweat can be recovered, and the yield of allulose crystal products can be improved.
Referring to fig. 1, the first discharge port is connected to the plate-type falling film crystallizer 1 through a pipeline, a cooler 4 and an intermediate product tank 3 are disposed on a connecting pipeline between the first discharge port and the plate-type falling film crystallizer 1, a switching valve 12 is disposed on a connecting pipeline between the first discharge port and the intermediate product tank 3, a switching valve 12 and a centrifugal pump 11 are disposed on a connecting pipeline between the intermediate product tank 3 and the cooler 4, and a switching valve 12 and a centrifugal pump 11 are disposed on a connecting pipeline between the cooler 4 and the plate-type falling film crystallizer 1.
With reference to fig. 1, the intermediate product tank 3 is a storage container for the liquid intermediate product obtained by preliminary purification, which is the liquid 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 melted, and the intermediate product tank 3 is located below the tubular falling film crystallizer 2.
Referring to fig. 1, the cooler 4 is used for cooling the liquid intermediate product discharged after the temperature rise, and the cooler 4 may be a tube cooler, a plate cooler, an air-cooled cooler, or the like. Tube coolers, plate coolers and air-cooled coolers are prior art and will not be described in detail herein.
Referring to fig. 2, the plate-type falling film crystallizer includes a housing 101, a second feeding hole 102 and an air outlet 1010 are formed at the top of the housing 101, a second discharging hole 108 and an air inlet are formed at the bottom of the housing 101, a second cooling and heating medium outlet 1013 is formed at the upper part of the housing 101, and a second cooling and heating medium inlet 1012 and an air inlet 107 are formed at the lower part of the housing 101.
Referring 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 connected to the cooler 4. The inner diameter of the communication pipe between the cooler 4 and the second inlet 102, which is close to the second inlet 102, is gradually reduced, and the communication pipe is flat. The second inlet 102 is used for feeding the liquid intermediate product after the preliminary purification into the shell 101. A sealing valve (not shown) is arranged at the second discharging port 102.
Specifically, the inner diameter of the part of the communication pipeline between the cooler 4 and the second feed inlet 102, which is close to the second feed inlet 102, is gradually reduced and is flat, so that the liquid intermediate product can enter the shell 101 in a film form instead of a strand form, the technical problem of poor crystallization effect caused by the flow of the liquid intermediate product in the strand form is solved, and the crystallization effect is improved; by arranging the feed inlet 102 to be flat, the liquid intermediate product can enter the shell 101 in a film form instead of a strand form, so that the technical problem of poor crystallization effect caused by the flow of the liquid intermediate product in the strand form is avoided, and the crystallization effect is improved.
Referring to fig. 2, the second discharge port is connected to the second feed port 102 via a second material circulation pipeline, and the second material circulation pipeline is provided with a circulation pump 10.
Specifically, the second discharge port is communicated with the second feed port 102 through the second material circulating pipeline, so that the uncrystallized liquid in the intermediate product can be recycled and then sent into the plate-type falling film crystallizer again for crystallization, and the yield of the allulose crystal product is further improved.
Referring to fig. 2, the second cooling and heating medium outlet 1013 is connected to the second cooling and heating medium inlet 1012 through a second cooling and heating medium circulation pipeline, and the second cooling and heating medium circulation pipeline is provided with a circulation pump 10, a cooling medium cooler 13 and a heating medium heat exchanger 14.
Specifically, the second cooling and heating medium outlet 1013 is communicated with the second cooling and heating medium inlet 1012 through the second cooling and heating medium circulation pipeline, and the second cooling and heating medium circulation pipeline is provided with the circulating pump, the refrigerant cooler and the heating medium heat exchanger, so that the cooling and heating media can be recycled, the utilization rate of the cooling and heating media is improved, and the production cost is reduced.
Referring to fig. 2, the gas inlet 107 is used for introducing high-pressure gas such as high-pressure nitrogen gas, inert gas, etc. into the casing 101.
Specifically, by additionally arranging the gas inlet 107, high-pressure gas such as high-pressure nitrogen, inert gas and the like 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 rate 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; meanwhile, volatile substances in the material to be purified can escape and be discharged to the atmosphere through the gas outlet 1010.
With reference to fig. 2, the push rod assembly 104, the crystallization plate 103 and the filtering structure 105 are sequentially disposed from top to bottom inside the housing 101, and a liquid collecting chamber 1014 is disposed between the filtering structure 105 and the discharging hole 108. The cross section of the part of the liquid collecting cavity 10104 close to the discharge hole 108 is V-shaped. A sealing valve (not shown) is arranged at the discharge port 108, the liquid collecting cavity 1014 is communicated with the discharge port 108, and the liquid collecting cavity 1014 is positioned above the discharge port 108.
Specifically, by setting the cross section of the part of the liquid collection chamber 10104 close to the discharge port 108 to be V-shaped, as much material as possible can be discharged through the discharge port, and the situation that the material cannot be completely discharged from the casing 101 is avoided.
Referring to fig. 3, the crystallization plate 103 is disposed along a vertical direction, the crystallization plate 103 is located above the gas inlet 107, and a plurality of crystallization grooves 1031, a plurality of heat exchange chambers 1032 and a plurality of heat exchange grooves 1033 are disposed in the vertical direction of the crystallization plate 103.
Specifically, by forming the crystallization plate 103 with the plurality of crystallization tanks 1031 in the vertical direction, crystallization can be performed simultaneously in the plurality of crystallization tanks 1031, thereby improving the production efficiency. 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 with liquid intermediate product simultaneously, be favorable to liquid intermediate product rapid cooling, further improve the crystallization effect.
With continued reference to FIGS. 2-3, the crystallization bath 1031 is connected to the feed inlet 102 via a feed pipe, and the crystallization bath 1031, the heat exchange chamber 1032 and the heat exchange tank 1033 all penetrate the crystallization plate 103. The feed pipe 1021 is provided with a plurality of parallel blocking elements 1023 along the material flowing direction, and the blocking elements 1023 are used for dividing the material entering the feed pipe 1021 into a plurality of branches, so that the material enters different crystallizing tanks 1031 through different branch feed pipes 1022 respectively. The branch feeding pipes 1022 correspond to the crystallization tanks 1031 one by one, and the cross section of the branch feeding pipe 1022 of the pipe section near the crystallization tanks 1031 is arc-shaped. The heat exchange chamber 1032 and the heat exchange slots 1033 are located adjacent to the crystallization slots 1031. The blocking element 1023 can be made of a blocking element 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 flowing direction and arranging the cross section of the feeding branch pipe 1022 close to the pipe section of the crystallizing tank 1031 to be arc-shaped, the liquid intermediate product can be shunted, and then the liquid intermediate product enters the inside of the housing 101 in a film shape instead of a strand shape, so that the technical problem that the crystallization effect is poor due to the flow of the liquid intermediate product in the strand shape 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 bath 1031, and the heat exchange bath 1033 is located at the side of the adjacent region of the crystallization bath 1031. The heat exchange cavity 1032 is communicated with a second cooling medium inlet 1012 through a cooling medium inlet pipe 10121, and the heat exchange cavity 1032 is communicated with a second cooling medium outlet 1013 through a cooling medium outlet pipe 10131.
In particular, by arranging the heat exchange chamber 1032 at the back of the crystallization tank 1031 and arranging the heat exchange tank 1033 at the side of the adjacent region of the crystallization tank 1031, the better heat exchange between the cold medium entering the heat exchange chamber and the liquid intermediate product flowing along the crystallization tank is facilitated, so that the psicose in the intermediate product is better crystallized on the wall of the crystallization tank 1031.
Referring to fig. 1, the cooling and heating medium inlet pipe includes a cooling and heating medium inlet main pipe (not shown) and a plurality of cooling and heating medium inlet branch pipes (not shown) communicating with the cooling and heating medium inlet main pipe. The second cooling and heating medium outlet pipe includes a cooling and heating medium outlet main pipe (not shown) and a plurality of cooling and heating medium outlet branch pipes (not shown) communicated with the cooling and heating medium outlet main pipe. The cold and heat medium inlet branch pipe and the cold and heat medium outlet branch pipe are communicated with the heat exchange cavity 1032 and the heat exchange groove 1033, and the cold and heat medium inlet branch pipe and/or the cold and heat 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 grooves 1033 are closed bottom walls, and through holes (not shown) for inserting cooling and heating medium inlet branch pipes are formed in the bottom walls of the heat exchange cavity 1032 and the heat exchange grooves 1033.
Particularly, through inserting cold and hot medium import pipe 1021 and/or cold and hot medium outlet pipe 1031 part in heat transfer chamber 1032 heat transfer groove 1032, can shorten the stroke of cold medium, and then improve the heat transfer effect between cold medium and the liquid intermediate product to guarantee the crystallization effect (guarantee crystal thickness) of the allulose crystal on the crystallization tank, avoid because of the problem that the crystal thickness that the heat transfer effect is not good leads to is thinner.
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, that is, the positions of the push rods 1041 correspond to the positions of the crystallization tanks 1031 one by one. The push rod 1041 is arranged along the vertical direction, the shape of the push rod 1041 is matched with the shape of the crystal tank 1031, and the width of the push rod 1041 is slightly smaller than the width of the crystal 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 crystallized substance off the wall surface of the crystallizing tank 1031. The first driving mechanism 1042 may be a hydraulic machine, a pneumatic machine, a driving machine, or the like. The hydraulic press, pneumatic press and drive machine are prior art and will not be described here.
Specifically, by additionally arranging the push rod assembly 4, the allulose crystal substance can be pushed down from the wall surface of the crystallization tank 1031, and the yield of the allulose crystal product is further improved. By setting the push rod 1041 to match with the crystallization tank 1031, more psicose crystal products can be pushed off from the wall surface of the crystallization tank 31, and the yield of the psicose crystal products is improved.
Referring to fig. 2, the filter mechanism 105 is detachably fixed on the inner wall of the housing 101, and the detachable fixing manner can be realized by bolt fastening, hanging, and the like. The filtering mechanism 105 is positioned between the second feeding port 102 and the second discharging port 108, and the filtering mechanism 105 is positioned below the crystallization plate 103. The filter mechanism 105 is a filter net, and an opening 1051 is provided in the housing 101 near the filter mechanism 105. Opening 1051 is used to manually remove filter mechanism 105 through 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 the inner wall of the housing 101, the cutting mechanism 106 is disposed along the opposite direction of the crystallization tank 1031, the cutting mechanism 106 is provided with a plurality of cutting blades 1061 and a second driving mechanism 1062 for driving the cutting blades 1061 to extend and retract, the cutting blades 1061 are disposed in parallel along a direction perpendicular to the crystallization tank 1032, that is, the cutting blades 1061 are disposed along a direction perpendicular to the bottom wall of the crystallization tank 1032. The drive shaft of the second drive mechanism 1062 is connected to a connecting block to which all the cutters 1061 are connected. The second driving mechanism 1062 may be a hydraulic machine, a pneumatic machine, a driving machine, or the like. The cutter 1061 may be a dicing blade or the like. The hydraulic press, the pneumatic press, the driver and the dicing cutter are prior art and are not described herein.
By additionally arranging the cutting machine 106 arranged oppositely along the crystallization tank 1031, the crystallized substance can be cut, so that the psicose crystal substance is easier to fall off from the wall surface of the crystallization tank 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 sets up along the direction parallel arrangement perpendicular with crystallizer 1031, can cut allulose crystal substance through a plurality of cutters 1061 simultaneously to make allulose crystal product more easily drop from crystallizer 131 wall, further improve the yield of allulose crystal product.
With continued reference to fig. 2, the falling film crystallizer further includes a spray head 109. The spray head 109 is fixedly arranged on the inner wall of the shell 11, the spray head 109 is positioned above the crystallizing tank 1031, and the spray head 109 is communicated with a high-pressure air inlet pipe (not shown) and/or a high-pressure liquid inlet pipe (not shown). Specifically, in this embodiment, the spray head 109 is a rotary spray head.
Specifically, the nozzle 109 is communicated with the high-pressure air inlet pipe, so that when sweat is separated in a sweating stage, the sweat can be blown off by high-pressure gas (particularly suitable for viscous materials), and the purity of the obtained allulose crystal product is improved; by communicating the nozzle 109 with the high-pressure liquid inlet pipe, when the crystallization tank 1031 and the filtering mechanism 105 need to be cleaned, the crystallization tank 1031 and the filtering mechanism 105 can be washed by high-pressure liquid, so that the psicose crystal substances remaining on the wall surface 1031 of the crystallization tank 1031 fall off, the yield of the psicose crystal product is improved, and the filtering mechanism 105 is cleaned. By setting the spray head 109 to adopt a rotary spray head, high-pressure gas and/or high-pressure liquid can sweep the crystallization tank 1031 and the filtering mechanism 105 at different angles simultaneously, so that the yield of the psicose crystal product is further improved, and a better cleaning effect on the filtering mechanism 105 is achieved.
With continued reference to fig. 1, the second discharge port 108 is connected to the residue tank 8 and/or the sweat storage tank 9, and the residue tank 5 and the sweat storage tank 6 are located below the plate-type falling film crystallizer 1.
With continuing reference to fig. 1, the raffinate tank 8 and the sweat storage tank 9 are storage containers for raffinate (residual solution after crystallization, which contains a small amount of psicose) and sweat (liquid discharged during the warming and sweating stage, which contains a large amount of psicose) obtained after treatment in the plate-type falling film crystallizer 1. The liquid outlet end of the residual liquid tank 5 is communicated with the first feeding hole, the liquid outlet end of the sweat storage tank 6 is communicated with the second feeding hole 102, and a communicating pipeline between the residual liquid tank 5 and the first feeding hole and a communicating pipeline between the liquid outlet end of the sweat storage tank 6 and the second feeding hole 102 are both provided with a switch valve 12 and a centrifugal pump 11. Through communicating the liquid outlet ends of the residual liquid tank 8 and the sweat storage tank 9 with the second feed inlet 102, residual liquid and sweat discharged from the second discharge port 108 can be respectively fed into the tubular falling film crystallizer 2 and the plate-type falling film crystallizer 1 for crystallization, so that allulose in the residual liquid and the sweat can be recovered, and the yield of allulose crystal products can be improved.
Example 2
The D-psicose crystal was prepared using the psicose crystal production system of example 1, and the specific steps were as follows:
d-psicose solution with the temperature of 80 ℃ and the concentration of 80wt% is sent into a raw material tank 7, and then the psicose solution is pumped 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 cooling and heating medium circulating pipeline and a cooling medium cooler 13, feeding cooling medium cooling water into the tubular falling film crystallizer 2, conveying a D-psicose solution to a first feed inlet by the circulating pump 10, cooling the psicose solution to 40 ℃ at the speed of 3 ℃/min, then slowly cooling the psicose solution to 30 ℃ at the cooling speed of 0.5 ℃/min, and then carrying out heat preservation treatment at the temperature of 30 ℃ by a cooling medium to carry out circulating falling film crystallization for 100min; then opening a switch valve 12 on a pipeline between the mother liquor tank 5 and the first discharge hole, discharging the mother liquor to the mother liquor tank 5, and weighing and sampling;
enriching and recovering mother liquor accumulated in multiple falling film crystallization, opening a switch valve 12 and a centrifugal pump 11 on a communication pipeline between a mother liquor tank 5 and a first feed inlet, and pumping the mother liquor obtained by enrichment and recovery to the bottom of the 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 ℃ at the heating rate of 3 ℃/min by a heating medium, the temperature of the internal environment of the tubular falling film crystallizer 2 is raised to 105 ℃ at the heating rate of 0.5 ℃/min, and then the temperature is preserved for 40min at 105 ℃; 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 after being heated to sweat, the psicose and the impurities in the melted sweat are redistributed and enriched, the sweat contains more impurities, and the sweat is gradually discharged out of the crystal layer under the push of heat transfer and mass transfer, so that the content of the psicose in the crystal layer is increased;
in the process, high-pressure nitrogen is fed into the nozzle 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 the viscous sweat is blown off;
then opening a switch valve 12 on a pipeline between the sweat tank 6 and the first discharge port and a sealing valve at 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 be used as a raw material of the next batch of crystallization, and closing a sealing valve at the first discharge port;
heating to 115 ℃ at a heating rate of 0.5 ℃/min, carrying out heat preservation treatment at the temperature of 115 ℃ for melting for 30min, opening a switching valve 12 and a centrifugal pump 11 on a communication pipeline between the intermediate product tank 3 and the first discharge port after the melting is finished, and conveying liquid (namely the intermediate product) to the intermediate product tank 3 for temporary storage;
the centrifugal pump 11 and the on-off valve 12 on the piping between the intermediate product tank 3 and the cooler 4 are opened, and the cooler 4 is started. The intermediate product is pumped by the centrifugal pump 11 to the cooler 4 and pre-cooled by the cooler 4 to 60 ℃.
Subsequently, the centrifugal pump 11 and the on-off 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 crystallizing tank 1031 in a film form through the feed pipe 1021;
starting a circulating pump 10 and a refrigerant cooler 13 on a second refrigerant and heat medium circulating pipeline for precooling, and keeping the internal environment temperature of the shell 1 at 30 ℃;
after all the materials enter the plate-type falling film crystallizer 1, starting a circulating pump 10 on a second material circulating pipeline, and keeping the temperature in the shell 101 at 30 ℃ to continue crystallizing; 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 rate of the intermediate product is reduced, and the psicose crystallized substance is better crystallized on the wall surface of the crystallizing tank 1031; meanwhile, volatile substances in the intermediate product are released and exhausted to the atmosphere through the air outlet 1010;
after the crystallization is finished, opening a switch valve 12 on a pipeline between the residual liquid tank 8 and a second discharge port 108, discharging the mother liquid to the residual liquid tank 8, weighing and sampling;
enriching and recovering residual liquid accumulated by multiple falling film crystallization; opening a switching valve 12 and a centrifugal pump 11 on a communication pipeline between the residual liquid tank 8 and the first feed inlet, and pumping the 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 heat medium circulating pipeline of the plate-type falling film crystallizer 1 to heat, raising the temperature of the crystals to 80 ℃ at the rate of 3 ℃/min through a heat medium, raising the internal environment temperature of the shell 101 to 105 ℃ at the rate of 0.5 ℃/min, and then preserving the heat at the temperature of 105 ℃ for 40min; 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 psicose and the impurities in the melted sweat are redistributed and enriched, the sweat contains more impurities, and the sweat is gradually discharged out of the crystal layer under the push of heat transfer and mass transfer, so that the content of the psicose in the crystal layer is increased;
in the process, high-pressure nitrogen is fed into the nozzle 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 crystallizing tank 1031 along different angles, so that the viscous sweat is blown off;
then opening the switch valve 12 on the pipeline between the sweat storage tank 9 and the second discharge hole 108 and the sealing valve at the second discharge hole 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 a second discharge port 108;
starting a cutting mechanism 16, cutting the psicose crystal substance on the wall surface of the crystal tank 1031 of the tubular falling film crystallizer 2 into blocks by driving a cutting knife 1061 through a second driving mechanism 1062, and then starting a first driving mechanism 1042 to drive a push rod 1041 to move towards the direction of the crystal tank 1031, so that the crystal block is pushed down from the wall surface of the crystal tank 1031, and the crystal block falls to a filtering mechanism 105;
after the filtering mechanism 15 filters the crystal substance mixed with the liquid substance, the solid substance such as crystal block is retained on the filtering mechanism 15, and the impurities such as liquid substance fall into the liquid collecting cavity 1014 due to the gravity;
the outlet 1051 is opened, the filter mechanism 105 is taken out, the crystallized substances on the filter mechanism 105 are taken down from the filter mechanism 105, the product of the psicose crystal is obtained, and the product is weighed and sampled.
Feeding high-pressure water into the nozzle 109 through a high-pressure liquid inlet pipe, and washing the crystallization tank 1031 and the filtering mechanism 105 with the high-pressure water;
the sealing valve at the second discharge port 108 is opened to discharge impurities such as liquid substances in the liquid collection chamber 1014 to the outside from the second discharge port 108.
Through detection, the D-psicose crystal produced by the method of the embodiment has the crystallization rate of 100%, the yield of 85.2% and the purity of the prepared D-psicose crystal of 99.8%.
Example 3
The present embodiment is different from embodiment 2 in that:
the raw material adopts an L-psicose solution, the temperature of the L-psicose solution is 120 ℃, and the concentration is 70wt%;
cooling the psicose solution to 45 ℃ at the speed of 5 ℃/min, then slowly cooling the psicose solution to 35 ℃ at the speed of 1 ℃/min, and then carrying out heat preservation treatment at the temperature of 35 ℃ by a cooling medium to circularly falling film crystallization for 90min;
heating the temperature of crystals on the wall surface of a crystallization tube of the tubular falling film crystallizer 2 to 90 ℃ by heating medium at the heating rate of 3 ℃/min, then heating the temperature of the internal environment of the tubular falling film crystallizer 2 to 110 ℃ at the heating rate of 1 ℃/min, and then preserving the heat for 50min at the temperature of 110 ℃;
heating to 125 deg.C at a rate of 1 deg.C/min, and melting at 125 deg.C for 30-40min;
the cooler 4 is started and the intermediate product is pumped by the centrifugal pump 11 to the cooler 4 and pre-cooled by the cooler 4 to 80 ℃.
Starting a circulating pump 10 and a refrigerant cooler 13 on a second refrigerant and heat medium circulating pipeline for precooling, and keeping the internal environment temperature of the shell 1 at 40 ℃;
keeping the internal temperature of the shell 101 at 30 ℃ and continuing crystallization;
after raising the crystal temperature to 90 c at a rate of 5 c/min by the heating medium, the internal ambient temperature of the housing 101 is raised to 110 c at a rate of 1 c/min, followed by holding at 110 c for 50min.
Through detection, the L-psicose crystal produced by the method of the embodiment has the crystallization rate of 100%, the yield of 84.5% and the purity of the prepared L-psicose crystal of 99.5%.
Example 4
The present embodiment is different from embodiment 2 in that:
the temperature of the raw material D-psicose solution is 100 ℃, and the concentration is 75wt%;
cooling the psicose solution to 42 ℃ at the speed of 4 ℃/min, then slowly cooling the psicose solution to 32 ℃ at the cooling speed of 0.8 ℃/min, and then carrying out heat preservation treatment at the temperature of 32 ℃ by using a cooling medium to realize circulating falling film crystallization for 95min;
heating the temperature of crystals on the wall surface of a crystallization tube of the tubular falling film crystallizer 2 to 85 ℃ at a heating rate of 4 ℃/min by using a heating medium, then heating the internal environment temperature of the tubular falling film crystallizer 2 to 108 ℃ at a heating rate of 0.8 ℃/min, and then preserving the temperature for 45min at the temperature of 108 ℃;
heating to 120 deg.C at a rate of 0.8 deg.C/min, and melting at 120 deg.C for 30-40min;
the cooler 4 is started and the intermediate product is pumped by the centrifugal pump 11 to the cooler 4 and pre-cooled by the cooler 4 to 70 ℃.
Starting a circulating pump 10 and a refrigerant cooler 13 on a second refrigerant circulating pipeline of the plate-type falling film crystallizer 1 for precooling, so that the internal environment temperature of the shell 1 is kept at 35 ℃;
keeping the internal temperature of the shell 101 at 35 ℃ to continue crystallization;
after raising the crystal temperature to 90 ℃ at a rate of 4 ℃/min by means of a heating medium, the internal ambient temperature of the housing 101 is raised to 108 ℃ at a rate of 0.8 ℃/min, and then the temperature is maintained at 108 ℃ for 45min.
Through detection, the D-psicose crystal produced by the embodiment has the crystallization rate of 100%, the yield of 84.9% and the purity of the prepared D-psicose crystal of 99.6%.
Example 5
As shown in fig. 5, the present embodiment is different from embodiment 1 in that: the push rod assembly 104 comprises 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 crystallizing bath 1031. The driving mechanism 1042 is used to drive the push rod 1041 and the push block 1043 to move in the direction of the crystallization tank 1031, so that the push rod 142 pushes the crystal substance crystallized in the crystallization tank 1031 down from the wall surface of the crystallization tank 31.
Example 6
As shown in fig. 6, the present embodiment is different from embodiment 1 in the assembly of the crystallization plate and the housing: 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 cavity 1032 and a heat exchange slot 1033.
Example 7
As shown in fig. 7, the allulose crystal production system of the present embodiment further includes a solvent tank 15 and a condenser 16.
Referring 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 pipeline, the solvents such as ethanol can be fed into the shell 101, so that the solvents such as ethanol can dissolve the non-crystallized liquid in the intermediate product, the flow rate of the non-crystallized liquid in the intermediate product is increased, the problem that effective circulation crystallization cannot be performed due to the fact that the viscosity of the non-crystallized liquid in the intermediate product is too high is solved, and the yield of the psicose crystal product is further increased.
With reference to fig. 7, the condenser 16 is used to cool the solvent, such as ethanol, discharged from the plate-type falling film crystallizer 1 and transformed into a gas state after being heated, so that the solvent, such as ethanol, is transformed into a liquid state after being cooled, and is pumped into the solvent tank 15 by the centrifugal pump 11, so as to recycle the solvent, such as ethanol. The condenser 16 may employ a water-cooled condenser, an air-cooled condenser, a water-air cooled condenser, or the like. Water cooled condensers, air cooled condensers and water-air cooled condensers are prior art and will not be described in detail 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 increased;
this embodiment is also different from embodiment 1 in that: pumping the absolute ethanol stored in the solvent tank 15 to a crystallization tank 1031 by using a centrifugal pump 11, dissolving the psicose by the absolute ethanol, and promoting the psicose which is difficult to fall and is remained on the wall surface of the crystallization tank 1031 to flow at a certain speed so as to crystallize, so that the yield of the psicose crystal product is further improved; in the sweating stage, due to the rise of the internal environment temperature of the casing 101, the absolute ethyl alcohol is volatilized into gas, is discharged from the gas outlet 1010, enters the condenser 16, is processed by the condenser 16, is converted into liquid absolute ethyl alcohol, and then flows into the solvent tank 15 through a pipeline.
It should be understood that, without being limited thereto, the crystallization plate may be provided with only the heat exchange chamber or the heat exchange slot, and not with both the heat exchange chamber and the heat exchange slot. The first feed inlet can also be arranged at the upper part of the tubular falling film crystallizer.
It should be noted that, in the non-application, the upper portion of the casing may be provided with a second cooling and heating medium inlet communicated with the heat exchange cavity, and the lower portion of the casing may be provided with a second cooling and heating medium outlet communicated with the heat exchange cavity.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (10)
1. A method for producing allulose crystals, comprising the steps of:
s1, feeding the allulose solution into a tubular falling film crystallizer for crystallization, and then heating to melt the obtained crystals into a liquid state to obtain an intermediate product;
s2, precooling the intermediate product, and then sending the intermediate product into a plate-type falling film crystallizer for crystallization to obtain the psicose crystal.
2. The production method according to claim 1, wherein in step S1, the concentration of the psicose solution is 70wt% to 80wt%;
and/or, in step S1, the temperature of the allulose solution is 80-120 ℃;
and/or, in step S1, the crystallization comprises: cooling to 40-45 deg.C at a rate of 3-5 deg.C/min, cooling to 30-35 deg.C at a rate of 0.5-1 deg.C/min, and crystallizing at 30-35 deg.C for 90-100min;
and/or in step S1, a sweating step is further included after crystallization and before melting;
and/or, in step S1, the melting comprises: heating to 115-125 deg.C at a rate of 0.5-1 deg.C/min, and maintaining at 115-125 deg.C for 30-40min to obtain intermediate product.
3. The production method according to claim 2, wherein the sweating comprises: heating to 80-90 deg.C at 3-5 deg.C/min, heating to 105-110 deg.C at 0.5-1 deg.C/min, and maintaining at 105-110 deg.C for 40-50min to obtain sweat.
4. The production method according to claim 3, further comprising: and (2) enriching and recovering the mother liquor and/or sweat obtained in the step (S1), and feeding the enriched and recovered mother liquor and/or sweat into a tubular falling film crystallizer for crystallization.
5. The production method according to claim 1, wherein in step S2, the intermediate product is cooled to 60 to 80 ℃;
and/or, in step S2, the crystallization comprises: firstly, cooling to 30-40 ℃, and then crystallizing at the temperature of 30-40 ℃;
and/or, in the step S2, a sweating step is further included after the crystallization.
6. The production method according to claim 5, wherein in step S2, the sweating includes: heating to 80-90 deg.C at 3-5 deg.C/min, heating to 105-110 deg.C at 0.5-1 deg.C/min, and maintaining at 105-110 deg.C for 40-50min to obtain sweat;
and/or, further comprising: enriching and recovering the mother liquor obtained in the step S2, and feeding the enriched and recovered mother liquor into a tubular falling film crystallizer for crystallization;
and/or, further comprising: and (3) enriching and recovering the sweat obtained in the step (S2), and feeding the sweat after enrichment and recovery into a plate-type falling film crystallizer for crystallization.
7. The allulose crystal production system is characterized by comprising a tubular falling film crystallizer, a cooler and a plate falling film crystallizer which are sequentially communicated, wherein the tubular falling film crystallizer is provided with a first cooling and heating medium inlet, a first cooling and heating medium outlet, a first feeding hole and a first discharging hole, the plate falling film crystallizer comprises a shell, a second feeding hole and a gas outlet are formed in the top of the shell, the second feeding hole is flat, a second discharging hole and a gas 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 groove and a heat exchange cavity are formed in the crystallization plate in the vertical direction, the crystallization groove is communicated with the second feeding hole through a feeding pipe, the heat exchange cavity is located in an area adjacent to the crystallization groove, a second cooling and heating medium inlet which is communicated with the heat exchange cavity is formed in the lower portion of the shell, a second cooling and heating medium outlet which is communicated with the heat exchange cavity is formed in the upper portion of the shell, the top of the shell and the bottom of the shell are respectively provided with the gas inlet and the gas outlet which is located below the crystallization plate.
8. An allulose crystal production system as recited in claim 7, 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;
and/or the first material outlet is communicated with the first material circulating inlet through a first material circulating pipeline, and a circulating pump is arranged on the first material circulating pipeline;
and/or the first cooling and heating medium outlet is communicated with the first cooling and heating medium inlet through a first cooling and heating medium circulating pipeline, and a circulating pump, a refrigerant cooler and a heating medium heat exchanger are arranged on the Leng Di heating medium circulating pipeline;
and/or the crystallization plate is provided with a plurality of crystallization grooves along the vertical direction;
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 shell, close to the filtering mechanism;
and/or a pipeline for communicating the heat exchange cavity with the second cooling and heating medium inlet and/or a pipeline part for communicating the heat exchange cavity with the second cooling and heating medium outlet extends into the heat exchange cavity;
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 cooling medium outlet is communicated with the second cooling medium inlet through a second cooling medium circulating pipeline, and a circulating pump, a refrigerant cooler and a heating medium heat exchanger are arranged on the second heating medium circulating pipeline;
and/or the crystallization plate is also provided with a heat exchange groove, the refrigerant heat exchange groove is positioned in the adjacent area of the crystallization groove, and the heat exchange groove is communicated with the second cooling medium inlet and the second cooling medium outlet;
and/or the second discharge port is also communicated with a residual liquid tank and/or a sweat storage tank, the residual liquid tank is communicated with the first feed port, and the sweat storage tank is communicated with the second feed port.
9. An allulose crystal production system according to claim 7, wherein a push rod assembly is further disposed inside the plate-type falling film crystallizer, the push rod assembly is located above the crystallization plate, the push rod assembly includes a first driving mechanism and a push rod corresponding to the crystallization tank, the driving mechanism is configured to drive the push rod so that the push rod pushes the crystallized material off the wall surface of the crystallization tank, and the push rod is disposed in a 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 and 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, and the cutter is arranged along the direction vertical to the crystallization groove;
and/or the plate-type falling film crystallizer further comprises a spray head, 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 device also comprises a solvent tank which is communicated with the bottom of the shell through a pipeline.
10. An allulose crystal production system according to claim 9, 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 groove;
and/or a pipeline for communicating the heat exchange groove with the second cooling and heating medium inlet and/or a pipeline part for communicating the heat exchange groove with the second cooling and heating medium outlet extends into the heat exchange groove;
and/or the gas outlet is communicated with the solvent tank through a pipeline, and a condenser is arranged on a communication pipeline between the gas outlet and the solvent tank.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210968665.6A CN115160386A (en) | 2022-08-12 | 2022-08-12 | Production method and production system of psicose crystals |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210968665.6A CN115160386A (en) | 2022-08-12 | 2022-08-12 | Production method and production system of psicose crystals |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN115160386A true CN115160386A (en) | 2022-10-11 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210968665.6A Withdrawn CN115160386A (en) | 2022-08-12 | 2022-08-12 | Production method and production system of psicose crystals |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115160386A (en) |
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2022
- 2022-08-12 CN CN202210968665.6A patent/CN115160386A/en not_active Withdrawn
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