CN114452672B - Based on CO 2 Concentrated solution manufacturing device and method for phase change balance regulation and control - Google Patents
Based on CO 2 Concentrated solution manufacturing device and method for phase change balance regulation and control Download PDFInfo
- Publication number
- CN114452672B CN114452672B CN202110290869.4A CN202110290869A CN114452672B CN 114452672 B CN114452672 B CN 114452672B CN 202110290869 A CN202110290869 A CN 202110290869A CN 114452672 B CN114452672 B CN 114452672B
- Authority
- CN
- China
- Prior art keywords
- concentration
- pressure
- temperature
- liquid material
- tank
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 230000008859 change Effects 0.000 title claims abstract description 77
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title abstract description 28
- 230000033228 biological regulation Effects 0.000 title description 7
- 239000013078 crystal Substances 0.000 claims abstract description 85
- 238000003756 stirring Methods 0.000 claims abstract description 85
- 239000011344 liquid material Substances 0.000 claims abstract description 73
- 230000001105 regulatory effect Effects 0.000 claims abstract description 52
- 238000002425 crystallisation Methods 0.000 claims abstract description 33
- 230000008025 crystallization Effects 0.000 claims abstract description 33
- 230000012010 growth Effects 0.000 claims abstract description 23
- 238000001816 cooling Methods 0.000 claims abstract description 20
- 230000001276 controlling effect Effects 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 239000012141 concentrate Substances 0.000 claims description 52
- 230000007423 decrease Effects 0.000 claims description 29
- 239000007788 liquid Substances 0.000 claims description 17
- 238000012544 monitoring process Methods 0.000 claims description 4
- 238000013019 agitation Methods 0.000 claims description 3
- 230000003698 anagen phase Effects 0.000 claims description 2
- 230000003247 decreasing effect Effects 0.000 claims 1
- 239000000243 solution Substances 0.000 description 63
- 230000001954 sterilising effect Effects 0.000 description 51
- 238000004659 sterilization and disinfection Methods 0.000 description 51
- 235000011389 fruit/vegetable juice Nutrition 0.000 description 22
- 244000183278 Nephelium litchi Species 0.000 description 15
- 239000011229 interlayer Substances 0.000 description 14
- 238000009833 condensation Methods 0.000 description 13
- 230000005494 condensation Effects 0.000 description 13
- 230000007246 mechanism Effects 0.000 description 13
- 150000008442 polyphenolic compounds Chemical class 0.000 description 13
- 235000013824 polyphenols Nutrition 0.000 description 13
- 238000005057 refrigeration Methods 0.000 description 11
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 10
- 239000000796 flavoring agent Substances 0.000 description 10
- 235000019634 flavors Nutrition 0.000 description 10
- 230000014759 maintenance of location Effects 0.000 description 9
- 239000000463 material Substances 0.000 description 9
- 238000002360 preparation method Methods 0.000 description 9
- 239000007787 solid Substances 0.000 description 9
- 244000005700 microbiome Species 0.000 description 8
- 238000004064 recycling Methods 0.000 description 8
- 238000003860 storage Methods 0.000 description 8
- 230000007704 transition Effects 0.000 description 7
- 235000019082 Osmanthus Nutrition 0.000 description 6
- 241000333181 Osmanthus Species 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 229910002092 carbon dioxide Inorganic materials 0.000 description 5
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 4
- 240000001008 Dimocarpus longan Species 0.000 description 4
- 235000000235 Euphoria longan Nutrition 0.000 description 4
- 235000015197 apple juice Nutrition 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 238000005265 energy consumption Methods 0.000 description 4
- 229940087559 grape seed Drugs 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- 238000002844 melting Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 238000012546 transfer Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 235000013305 food Nutrition 0.000 description 3
- 235000021579 juice concentrates Nutrition 0.000 description 3
- 230000000813 microbial effect Effects 0.000 description 3
- 230000006911 nucleation Effects 0.000 description 3
- 238000010899 nucleation Methods 0.000 description 3
- 235000015205 orange juice Nutrition 0.000 description 3
- 230000001737 promoting effect Effects 0.000 description 3
- 238000005086 pumping Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 2
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 description 2
- 229930003268 Vitamin C Natural products 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 229910002091 carbon monoxide Inorganic materials 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000011265 semifinished product Substances 0.000 description 2
- 235000019154 vitamin C Nutrition 0.000 description 2
- 239000011718 vitamin C Substances 0.000 description 2
- 238000005411 Van der Waals force Methods 0.000 description 1
- 238000005273 aeration Methods 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000001143 conditioned effect Effects 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 235000012041 food component Nutrition 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000002147 killing effect Effects 0.000 description 1
- 235000021056 liquid food Nutrition 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- NMJORVOYSJLJGU-UHFFFAOYSA-N methane clathrate Chemical compound C.C.C.C.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O NMJORVOYSJLJGU-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- SNICXCGAKADSCV-UHFFFAOYSA-N nicotine Chemical compound CN1CCCC1C1=CC=CN=C1 SNICXCGAKADSCV-UHFFFAOYSA-N 0.000 description 1
- 150000007965 phenolic acids Chemical class 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000011550 stock solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0004—Crystallisation cooling by heat exchange
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L2/00—Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation
- A23L2/02—Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation containing fruit or vegetable juices
- A23L2/08—Concentrating or drying of juices
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/005—Selection of auxiliary, e.g. for control of crystallisation nuclei, of crystal growth, of adherence to walls; Arrangements for introduction thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0063—Control or regulation
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/14—Thermal energy storage
Landscapes
- Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Nutrition Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Polymers & Plastics (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Non-Alcoholic Beverages (AREA)
- Physical Water Treatments (AREA)
Abstract
The invention relates to a method based on CO 2 A phase-change balance-regulated concentrated solution manufacturing method and a device for realizing the method. The method comprises the following steps: pre-cooling the liquid material, and controlling the temperature of the inner cavity of the concentration processor to be consistent with the pre-cooling temperature of the liquid material; the precooled liquid material is sent into the concentration processor; feeding CO into the inner cavity of the concentration processor 2 And the diameter of the air bubble is regulated and controlled by an air bubble generator, wherein the diameter of the air bubble is 10 2 ～10 7 nm; stirring the liquid material after the pressure in the inner cavity of the concentration processor is 50-150 bar, and simultaneously maintaining the pressure in the inner cavity of the concentration processor; after the liquid material is stirred for a period of time, reducing the temperature of the inner cavity of the concentration processor to 0.5-10 ℃, and regulating the pressure of the inner cavity of the concentration processor to 20-90 bar; the liquid material undergoes a phase change crystallization reaction, and hydrate crystals and concentrated solution are formed after the liquid material undergoes a phase change stage and a crystal growth stage.
Description
Technical Field
The invention relates to the technical field of concentrated liquid materials in the fields of biological pharmacy, food, chemical synthesis and the like, in particular to a liquid material based on CO 2 Concentrated solution manufacturing device based on phase change balance regulation and control and CO (carbon monoxide) 2 Phase change balance regulating and controlling concentrationA method for producing condensed liquid.
Background
The concentrated solution is widely circulated in the fields of biological pharmacy and food processing as a semi-finished product or a product, and a high-efficiency, high-quality and low-cost concentration means is always an urgent need of the concentration industry.
The hydrate method concentration is a concentration method that guest gas water molecules and host water molecules in solution form cage-shaped structural substances similar to ice crystals under certain pressure and temperature, and concentrated solution is obtained after solid-liquid separation; similar to the presently recognized relatively optimal effect of freeze concentration, the method also has similar problems of crystal entrainment solute loss, but lower energy consumption than the method without subzero low temperature. Therefore, the formation speed, shape and size of the hydrate crystal are effectively regulated and controlled, and stable, more and pure hydrate crystals are obtained, so that concentrated solution with high concentration rate and low entrainment rate is obtained, and the method is an important guarantee for promoting the technical popularization of the liquid food concentrated by a hydrate method.
The formation of hydrate includes two stages of crystal nucleation and crystal growth, in the early stage of nucleation, gas molecules enter the solution, gas bubbles gradually become smaller along with the progress of gas-liquid mass transfer, gas molecules enter the cage-shaped pore structure formed by main water molecules gradually, nucleation occurs, main guest molecules are mutually related through Van der Waals force, stable cages are formed continuously in a gathering mode, and finally crystallization is completed.
The concentrated solution is a common semi-finished product or product in the industries of biological pharmacy, food and the like, and common concentration modes comprise membrane concentration, evaporation concentration and freeze concentration, wherein the concentration quality of the freeze concentration is optimal, but the application of the concentrated solution is relatively limited due to high energy consumption. At present, the gas hydrate concentration technology, which is comparable with the freeze concentration technology, can keep the material quality to the greatest extent. But simultaneously, similar to freeze concentration, solution solutes are easy to be entrained and even embedded in the process of crystal formation (forming cage-shaped structural materials), and the entrainment rate of the hydrate is one of main factors limiting popularization and application.
Thus, the current concentration technology has some defects, mainly expressed as:
(1) In the prior art, the concentration efficiency is high, and the heat-sensitive functional and nutritional components in the materials are seriously damaged.
(2) The relatively high quality of freeze concentration requires high energy consumption and long time for concentration due to the low freezing temperature condition, and the finished concentrated juice can be stored for a long time only by sterilization treatment.
(3) The single hydrate is concentrated, the sterilization effect on materials is limited, the phenomenon of microorganism subdeath occurs, and the materials can be stored for a long time only by auxiliary sterilization treatment.
Disclosure of Invention
Based on this, the object of the invention is to provide a CO-based system 2 Concentrated solution manufacturing device based on phase change balance regulation and control and CO (carbon monoxide) 2 The phase change balance regulating and controlling concentrated solution manufacturing method is realized by the concentrated solution manufacturing device, so that high-quality concentrated solution can be obtained, the concentrated solution is safe, and the storage quality is ensured.
Based on CO 2 A method of manufacturing a phase change equilibrium conditioned concentrate, the method comprising:
pre-cooling the liquid material, and controlling the temperature of the inner cavity of the concentration processor to be consistent with the pre-cooling temperature of the liquid material;
the precooled liquid material is sent into the concentration processor;
feeding CO into the inner cavity of the concentration processor 2 And the diameter of the air bubble is regulated and controlled by an air bubble generator, wherein the diameter of the air bubble is 10 2～ 10 7 nm；
Stirring the liquid material after the pressure in the inner cavity of the concentration processor is 50-150 bar, and simultaneously maintaining the pressure in the inner cavity of the concentration processor;
after the liquid material is stirred for a period of time, reducing the temperature of the inner cavity of the concentration processor to 0.5-10 ℃, and regulating the pressure of the inner cavity of the concentration processor to 20-90 bar;
the liquid material undergoes a phase change crystallization reaction, and hydrate crystals and concentrated solution are formed after the liquid material undergoes a phase change stage and a crystal growth stage.
Compared with the prior art, the invention is based on CO 2 The phase change balance regulating and controlling concentrated solution manufacturing method can regulate and control the diameter of bubbles and the treatment time according to the concentration of initial materials in the early phase of the phase change of the concentrated solution, promote the contact of air and liquid, enhance the heat and mass transfer effect, promote the phase change of the next step and achieve the aim of sterilization.
Further, the concentration of the liquid material is 4-20 degrees brix; precooling the liquid material to 15-20 ℃; after the pressure in the inner cavity of the concentration processor is 50-150 bar, stirring the liquid material, and setting the stirring speed to be 500-1500 rpm/min; the relationship among the concentration of the liquid material, the diameter of the bubbles, the pressure before cooling the concentration processor and the stirring speed when the pressure of the inner cavity of the concentration processor is 50-150 bar is as follows:
the concentration is 4-10 DEG brix, the diameter is 10 DEG brix 2～ 10 3 nm, the pressure is 50-90 bar, and the stirring rotation speed is 500-900 rpm/min;
the concentration is 10-15 DEG brix, the diameter is 10 3～ 10 5 nm, the pressure is 90-120 bar, and the stirring rotation speed is 900-1200 rpm/min;
the concentration is 15-20 DEG brix, the diameter is 10 DEG 5～ 10 7 nm, the pressure is 120-150 bar, and the stirring rotation speed is 1200-1500 rpm/min.
Further, after the pressure of the inner cavity of the concentration processor is 50-150 bar, stirring the liquid material, and simultaneously maintaining the pressure of the inner cavity of the concentration processor for 5-15 min; aeration is continued as the pressure drops during agitation to maintain the pressure within the concentrating processor chamber.
Further, the phase change phase refers to: after the continuous inflation is finished, the system pressure is reduced for the first time, the temperature of the liquid material starts to rise to be a starting point, and the temperature of the liquid material keeps stable or falls to be a starting point to be a terminal point, wherein the phase is a phase change phase and is obtained by an online temperature and pressure monitoring curve.
Further, the crystal growth stage refers to: after the phase change phase is finished, the system temperature starts to continuously decrease or the system temperature starts to decrease from the starting point temperature of the phase change phase, the pressure also continuously decreases until the pressure is not changed any more, and the pressure is kept constant for a period of time, and the phase is a crystal growth phase.
Further, the phase change stage and the crystal growth stage are both carried out under stirring conditions, and the stirring speed in the phase change stage and the crystal growth stage is 800-1500 rpm/min; the relationship among the concentration of the liquid material, the diameter of the bubbles, the pressure before cooling the concentration processor, the stirring speed when the pressure of the inner cavity of the concentration processor is 50-150 bar, and the stirring speed in the phase-change stage and the crystal growth stage is as follows:
the concentration is 4-10 DEG brix, the diameter is 10 DEG brix 2～ 10 3 nm, the pressure is 50-90 bar, the stirring speed is 500-900 rpm/min, and the stirring speed is 1300-1500 rpm/min;
the concentration is 10-15 DEG brix, the diameter is 10 3～ 10 5 nm, the pressure is 90-120 bar, the stirring speed is 900-1200 rpm/min, and the stirring speed is 1000-1300 rpm/min;
the concentration is 15-20 DEG brix, the diameter is 10 DEG 5～ 10 7 The pressure is 120-150 bar, the stirring speed is 1200-1500 rpm/min, and the stirring speed is 800-1500 rpm/min.
Further, the hydrate crystal enters a hydrate crystal tank, and the concentrated solution enters a concentrated solution tank; adjusting the temperature of the hydrate crystal tank to 40-60 ℃, stirring the hydrate crystal, dissolving out gas from the hydrate crystal, and introducing the dissolved gas into the concentrated liquid tank to sterilize the concentrated liquid; regulating the pressure of the concentrated solution tank to 50-150 bar, stirring concentrated solution in the concentrated solution tank, and setting the stirring rotating speed to 1500-2500 rpm/min; the gas in the concentrated liquid tank firstly enters the bubble generator and then enters the concentration processor.
Based on CO 2 Phase-change balance-regulated concentrated solution manufacturing device, which comprises a concentration processor and CO 2 Dewar, hydrate crystal tank, concentrate tank, condensation circulation system, thermal circulation system, storage tank, the concentration treater is used for liquid material takes place the phase transition crystallization reaction to produce concentrate and hydrate crystal, CO 2 The gas outlet of dewar bottle is linked together with the air inlet of concentrated treater through a bubble generator, the feed inlet of hydrate crystal jar with the hydrate export of concentrated treater is linked together, the feed inlet of concentrate jar with the concentrate export of concentrated treater is linked together, the air inlet of concentrate jar with the gas outlet of hydrate crystal jar is linked together, the gas outlet of concentrate jar with the air inlet of bubble generator is linked together, condensation circulation system is used for concentrating the treater refrigeration, thermal circulation system is used for the hydrate crystal jar heats, the feed inlet of storage tank with the discharge gate of concentrate jar is linked together.
Further, the device performs the above-mentioned CO-based 2 A method for preparing concentrated solution for regulating phase change balance.
Further, the device also comprises a feeding tank, wherein the feeding tank is used for storing liquid materials, and a discharge port of the feeding tank is communicated with a feed port of the concentration processor; a feed pump is arranged between the discharge port of the feed tank and the feed port of the concentration processor; at the CO 2 A booster pump or a compressor is arranged between the air outlet of the dewar and the bubble generator; the concentrating processor comprises an outer shell, an inner shell and a stirring device, wherein the inner shell is arranged in the outer shell, a shell interlayer is arranged between the inner shell and the outer shell, the shell interlayer is communicated with the condensation circulating system, the stirring device is arranged in the inner shell, and the stirring device is used for stirring liquid materials in the concentrating processor; a K-type thermocouple positioned in the interlayer of the shell is arranged in the inner cavity of the shell; a transparent observation window is also arranged on the inner shell; also in the inner cavity of the inner shellA high-speed camera is arranged; a pressure sensor is also arranged in the inner cavity of the inner shell; a K-type thermocouple is also arranged in the inner cavity of the inner shell; the hydrate crystal tank comprises an outer tank body, an inner tank body and a stirrer, wherein the inner tank body is arranged in the outer tank body, a tank body interlayer is arranged between the inner tank body and the outer tank body, the tank body interlayer is communicated with the thermal circulation system, the stirrer is arranged in the inner tank body, and the stirrer is used for stirring hydrate crystals in the hydrate crystal tank; k-type thermocouples are arranged in the inner cavities of the interlayer of the tank body and the inner tank body; a K-type thermocouple is arranged in the inner cavity of the concentrated liquid tank; a pressure sensor is also arranged in the inner cavity of the concentrated liquid tank; and a stirring mechanism for stirring the concentrated solution is also arranged in the concentrated solution tank.
For a better understanding and implementation, the present invention is described in detail below with reference to the drawings.
Drawings
FIG. 1 is a schematic view of a CO-based system according to the present invention 2 Schematic structural diagram of a concentrated solution manufacturing device with phase change balance regulation;
FIG. 2 is a schematic diagram of a concentrating processor according to the present invention;
FIG. 3 is a schematic diagram of a hydrate crystal tank according to the present invention;
FIG. 4 is a schematic view of the structure of the concentrate tank according to the present invention;
reference numerals:
10. a feed tank; 11. a feed pump; 20. a concentrating processor; 21. a housing; 22. an inner case; 23. a stirring device; 24. a shell interlayer; 30. CO 2 A dewar; 31. a bubble generator; 40. a hydrate crystal tank; 41. an outer can; 42. an inner tank; 43. a stirrer; 44. a tank interlayer; 50. a concentrate tank; 51. a stirring mechanism; 60. a condensation circulation system; 70. a thermal circulation system; 80. storage tank.
Detailed Description
Based on CO 2 A method for manufacturing a concentrated solution for regulating phase change balance, see fig. 1, which comprises the following steps:
s1, obtaining liquid materials with the concentration of 4-20 degrees brix, pre-cooling the liquid materials to 15-20 degrees, and simultaneously controlling the temperature of the inner cavity of the feeding tank 10 and the temperature of the inner cavity of the concentration processor 20 to be consistent with the pre-cooling temperature of the liquid materials;
s2, loading the precooled liquid material into a feed tank 10, and pumping the precooled liquid material from the feed tank 10 into an inner cavity of a concentration processor 20;
s3, feeding CO into the inner cavity of the concentration processor 20 2 And CO is regulated by the bubble generator 31 2 Is 10 in diameter 2～ 10 7 nm；
S4, after the pressure of the inner cavity of the concentration processor 20 is 50-150 bar, stirring the liquid material, setting the stirring speed to be 500-500 rpm/min, and simultaneously maintaining the pressure of the inner cavity of the concentration processor 20 for 5-15 min; continuing to inflate as the pressure decreases during agitation to maintain the pressure within the internal chamber of the concentrating processor 20;
s5, after the liquid material is stirred for a period of time, stirring is continuously performed, the stirring speed is set to be 800-1500 rpm/min, the temperature of the inner cavity of the concentration processor 20 is reduced to 0.5-10 ℃, and the concentration processor 20 is inflated or deflated to control the pressure of the inner cavity of the concentration processor 20 to 20-90 bar, the liquid material undergoes a phase change crystallization reaction, and hydrate crystals and concentrated solution are formed after the liquid material undergoes a phase change stage and a crystal growth stage;
s6, after the pressure in the inner cavity of the concentration processor 20 is stable for a period of time, the obtained hydrate crystal enters a hydrate crystal tank 40, and the concentrated solution enters a concentrated solution tank 50;
s7, adjusting the temperature of the hydrate crystal tank 40 to 40-60 ℃, dissolving out gas from the hydrate crystal, and feeding the dissolved gas into the concentrated liquid tank 50;
s8, regulating the pressure of the concentrated solution tank 50 to 50-150 bar, stirring the concentrated solution, setting the stirring rotation speed to 1500-2500 rpm/min, and performing secondary sterilization on the concentrated solution;
s9, after the concentrated solution is subjected to secondary sterilization treatment for a period of time, the gas in the concentrated solution tank 50 reenters the concentration processor 20 from the bubble generator 31 and enters the next cyclic utilization;
s10, after secondary sterilization is completed, the concentrated solution enters a storage tank 80 from a concentrated solution tank 50;
s11, carrying out sterile split charging on the concentrated solution, and storing in a refrigeration house.
In the practical implementation process, according to different material viscosities and concentrations, the bubble diameters are regulated and controlled, and meanwhile, the temperature, the corresponding pressure and the stirring rate are regulated and controlled, so that the contact of air and liquid can be effectively promoted, the heat and mass transfer is enhanced, and the formation and sterilization effects of hydrate crystals are promoted.
Thus, for step S3, the relationship between the concentration of the liquid material, the diameter of the bubbles is:
the concentration of the liquid material is 4-10 DEG brix, and the diameter of the bubble is 10 2～ 10 3 nm；
The concentration of the liquid material is 10-15 DEG brix, and the diameter of the bubble is 10 3～ 10 5 nm；
The concentration of the liquid material is 15-20 DEG brix, and the diameter of the air bubble is 10 5～ 10 7 nm。
For step S4, the relationship between the concentration of the liquid material, the pressure in the inner chamber of the concentration processor 20, and the stirring speed when the pressure in the inner chamber of the concentration processor 20 is 50-150 bar is:
the concentration of the liquid material is 4-10 degrees brix, the pressure is 50-90 bar, and the stirring speed is 500-900 rpm/min;
the concentration of the liquid material is 10-15 degrees brix, the pressure is 90-120 bar, and the stirring speed is 900-1200 rpm/min;
the concentration of the liquid material is 15-20 degrees brix, the pressure is 120-150 bar, and the stirring speed is 1200-1500 rpm/min.
For step S5, the relationship between the concentration of the liquid material, the stirring speed in the phase transition stage and the crystal growth stage is:
the concentration of the liquid material is 4-10 degrees brix, and the stirring speed is 1300-1500 rpm/min;
the concentration of the liquid material is 10-15 DEG brix, and the stirring speed is 1000-1300 rpm/min;
the concentration of the liquid material is 15-20 degrees brix, and the stirring speed is 800-1500 rpm/min.
Specifically, in step S5, the phase transition phase refers to that after the inflation is continued, the system pressure decreases for the first time, the temperature of the liquid material starts to increase to a starting point, and the temperature of the liquid material keeps stable or decreases to the starting point to an end point, where the phase transition phase is obtained from an online temperature-pressure monitoring curve. The crystal growth stage refers to a stage in which after the phase change stage is finished, the system temperature starts to continuously decrease or the system temperature starts to decrease from the starting point temperature of the phase change stage, and the pressure also continues to decrease until no change occurs and the temperature is kept constant for a certain period of time.
Specifically, in step S7, the hydrate crystals may be stirred, thereby promoting melting of the hydrate crystals.
Specifically, in step S9, the treatment time for performing the secondary sterilization treatment on the concentrated solution is determined according to the sterilization effect of the concentrated solution of different materials.
Compared with the prior art, the invention is based on CO 2 The phase change balance regulating and controlling concentrated solution manufacturing method has the following beneficial effects:
(1) In the early stage of the concentrated phase transition, the diameter, the temperature, the corresponding pressure and the treatment time of bubbles can be regulated and controlled according to the concentration of the initial material, so that the contact of air and liquid can be effectively promoted, the heat and mass transfer effect can be enhanced, the next phase transition can be promoted, and the aim of sterilization can be achieved;
(2) The high-density carbon dioxide sterilization principle is utilized in the early stage of concentration and the stage of obtaining the concentrated solution, so that the microorganism killing effect is achieved;
(3) And the gas from the crystal melting is utilized to perform secondary sterilization on the concentrated solution, and after sterilization is finished, the concentrated solution is recycled again to perform concentrated phase change, so that the energy consumption is effectively saved, and additional sterilization treatment is not needed.
(4) Compared with single hydrate concentration treatment, the invention can increase the sterilization rate by more than 30 percent;
(5) Compared with the single hydrate concentration treatment which is cooperated with the traditional sterilization treatment, the method can save more than 15% of time and improve more than 20% of quality.
In order to automatically realize the concentrated solution manufacturing method based on the CO2 phase change balance regulation, the invention also provides a concentrated solution manufacturing device based on the CO2 phase change balance regulation. Referring to fig. 1 to 4, the apparatus comprises a feed tank 10, a concentration processor 20, CO 2 Dewar 30, hydrate crystal tank 40, concentrate tank 50, condensate circulation system 60, thermal circulation system 70, and storage tank 80. Wherein, the feed tank 10 is used for storing liquid materials, and the discharge port of the feed tank 10 is communicated with the feed port of the concentration processor 20; a feed pump 11 is provided between a discharge port of the feed tank 10 and a feed port of the concentration processor 20, and liquid material in the feed tank 10 is conveyed into the concentration processor 20 by the feed pump 11. CO 2 Dewar 30 for storing CO 2 Gas, CO 2 The air outlet of the dewar 30 is communicated with the air inlet of the concentration processor 20; a bubble generator 31 is arranged between the air outlet of the CO2 Dewar bottle 30 and the air inlet of the concentration processor 20, and CO is regulated and controlled by the bubble generator 31 2 The diameter of the air bubble; in CO 2 A booster pump or a compressor is arranged between the air outlet of the dewar 30 and the bubble generator 31, and CO is pumped by the booster pump or the compressor 2 To the bubble generator 31. The concentration processor 20 is used to produce a concentrate and hydrate crystals. The hydrate crystal tank 40 is used for storing hydrate crystals, a feed inlet of the hydrate crystal tank 40 is communicated with a hydrate outlet of the concentration processor 20, and an air outlet of the hydrate crystal tank 40 is communicated with an air inlet of the concentration liquid tank 50. The concentrate tank 50 is used for storing concentrate, the feed inlet of the concentrate tank 50 is communicated with the concentrate outlet of the concentrate processor 20, and the air outlet of the concentrate tank 50 is communicated with the air inlet of the bubble generator 31. The condensing circulation system 60 is used to cool the feed tank 10 and the concentration processor 20. The thermal cycle system 70 is used to heat the hydrate crystal tank 40. The storage tank 80 is used for storing the concentrated solution after sterilization, and a feed inlet of the storage tank 80 is communicated with a discharge outlet of the concentrated solution tank 50.
Specifically, the concentration processor 20 includes an outer casing 21, an inner casing 22, and a stirring device 23. Wherein the inner shell 22 is disposed within the outer shell 21, and a shell interlayer 24 is disposed between the inner shell 22 and the outer shell 21, the shell interlayer 24 being in communication with the condensation circulation system 60. The stirring device 23 is disposed in the inner cavity of the inner shell 22, the stirring device 23 is used for stirring the liquid material in the concentrating processor 20, and as for the specific structure of the stirring device 23, reference may be made to chinese patent No. CN212236048U, which is not limited herein.
In addition, a type K thermocouple is installed in the inner cavity of the housing 21, and the type K thermocouple is located in the case interlayer 24, and the temperature of the inner cavity of the housing 21 is collected by the type K thermocouple. A transparent viewing window is also provided on the inner housing 22 to facilitate the user's view of the operation within the concentrating processor 20. A high speed camera is also provided in the interior of the inner housing 22, through which the operation of the concentrating processor 20 is collected. A pressure sensor is also installed in the inner cavity of the inner case 22, and the pressure of the inner cavity of the inner case 22 is detected using the pressure sensor. A type K thermocouple is also installed in the inner cavity of the inner housing 22, and the temperature of the inner cavity of the inner housing 22 is collected by using the type K thermocouple. The K-type thermocouple and the pressure sensor are used for realizing on-line monitoring of pressure and temperature and measuring the temperature of a sample and the pressure change of a system, namely the phase change condition, so that the sterilization and concentration process is regulated.
Specifically, the hydrate crystal tank 40 includes an outer tank 41, an inner tank 42, and a stirrer 43. The inner tank 42 is disposed in the outer tank 41, and a tank interlayer 44 is disposed between the inner tank 42 and the outer tank 41, and the tank interlayer 44 is communicated with the thermal circulation system 70. An agitator 43 is provided in the inner cavity of the inner tank 42, the agitator 43 being for agitating the hydrate crystals in the hydrate crystal tank 40 for promoting melting of the hydrate crystals. In addition, a K-type thermocouple is provided in each of the inner cavities of the tank body interlayer 44 and the inner tank body 42, and the temperature of the hydrate crystal is observed by the K-type thermocouple, so that the degree of melting is determined.
Specifically, a type K thermocouple is installed in the inner cavity of the concentrate tank 50, and the temperature of the concentrate is observed by the type K thermocouple. A pressure sensor is also installed in the inner cavity of the concentrate tank 50, and the pressure of the concentrate tank 50 is detected by the pressure sensor. The use of a type K thermocouple and pressure sensor may be used to determine the physical condition of the carbon dioxide within the concentrate tank 50 for further sterilization process adjustments. Further, a stirring mechanism 51 is provided in the concentrate tank 50, and the concentrate in the concentrate tank 50 is stirred by the stirring mechanism 51.
Example 1
A preparation method of litchi concentrated juice adopts the CO-based method of the invention 2 The phase change balance regulating and controlling concentrated solution manufacturing method specifically comprises the following steps:
extracting to obtain litchi vitamin C extract with solid content of 4 degrees brix, and pre-cooling to 15 ℃. The condensing circulation system 60 is opened to cool so that the temperature of the feed tank 10 and the concentration processor 20 is consistent with the temperature of the liquid material pre-cooling. Pumping 2.5L of pre-cooled extracting solution from the feeding tank 10 into the inner cavity of the concentration processor 20; turning on CO 2 Dewar 30 with a regulated bubble diameter of 10 2 After the pressure reaches 50bar at nm, simultaneously turning on a stirring device 23 of the concentration processor 20, setting the rotating speed to be 500rpm/min, and processing for 10min; regulating condensation circulation, reducing the temperature of the concentration processor 20 to 2 ℃, and performing phase-change crystallization reaction by deflating treatment to ensure that the pressure in the concentration processor 20 is 70bar and the rotating speed is 1300rpm/min; the phase change stage and the crystal growth stage are judged according to the pressure and temperature change curves, the pressure drop is detected for the first time, the point of temperature rise is a crystallization point, and the subsequent period of time when the temperature is kept constant is the phase change stage; the temperature starts to continuously decrease, and the pressure also continuously decreases until the pressure is unchanged and is constant for a period of time, and the crystallization stage is adopted; and meanwhile, the temperature of the hydrate crystal tank 40 is increased to 45 ℃, dissolved gas enters the concentrate tank 50, a stirring mechanism 51 of the concentrate tank 50 is opened, and after treatment for 10min, the gas is circulated to the bubble generator 31 again and enters the next recycling. And finally, sterile split charging and storing in a refrigeration house. The obtained vitamin C concentrate has a concentration rate of 40%, a polyphenol and Vc retention rate of 95%, and a microorganism quantity of about 10% lower than that of the stock solution 6 The color is not changed, compared with the single hydrate concentration and the heat sterilization or non-heat sterilization before or after the conventional concentration, the sterilization concentration treatment time is shortened by 20 percent; compared with the concentration treatment of the hydrate alone, the sterilization rate is improved by 20 percent.
Example two
A preparation method of litchi concentrated juice adopts the CO-based method of the invention 2 The phase change balance regulating and controlling concentrated solution manufacturing method specifically comprises the following steps:
litchi juice (longan flavor) with a solid content of 10 DEG brix, and precooling to 15 ℃. The condensing circulation system 60 is opened to cool so that the temperature of the feed tank 10 and the concentration processor 20 is consistent with the temperature of the liquid material pre-cooling. 2.5L of pre-cooled osmanthus flavored juice is pumped into the inner cavity of the concentration processor 20 from the feeding tank 10; turning on CO 2 Dewar 30 with a regulated bubble diameter of 10 3 After the pressure reaches 90bar at nm, simultaneously turning on a stirring device 23 of the concentration processor 20, setting the rotating speed to be 500rpm/min, and processing for 10min; regulating condensation circulation, reducing the temperature of the concentration processor 20 to 6 ℃, and performing phase-change crystallization reaction by deflating treatment to ensure that the pressure in the concentration processor 20 is 50bar and the rotating speed is 1300rpm/min; the phase change stage and the crystal growth stage are judged according to the pressure and temperature change curves, the pressure drop is detected for the first time, the point of temperature rise is a crystallization point, and the subsequent period of time when the temperature is kept constant is the phase change stage; the temperature starts to continuously decrease, and the pressure also continuously decreases until the pressure is unchanged and is constant for a period of time, and the crystallization stage is adopted; and meanwhile, the temperature of the hydrate crystal tank 40 is increased to 45 ℃, dissolved gas enters the concentrate tank 50, a stirring mechanism 51 of the concentrate tank 50 is opened, and after 15 minutes of treatment, the gas is circulated to the bubble generator 31 again and enters the next recycling. And finally, sterile split charging and storing in a refrigeration house. The obtained osmanthus concentrated juice has a concentration rate of 35%, a polyphenol and Vc retention rate of 94%, and a microorganism quantity of about 10% lower than that of the original juice 8 The flavor characteristic value is not changed, the original flavor and color are maintained, and compared with the single hydrate concentration and the heat sterilization or non-heat sterilization before or after the conventional concentration, the sterilization concentration treatment time is shortened by 15%; compared with the concentration treatment of the hydrate alone, the sterilization rate is improved by 40 percent.
Example III
A preparation method of litchi concentrated juice adopts the CO-based method of the invention 2 The phase change balance regulating and controlling concentrated solution manufacturing method specifically comprises the following steps:
litchi juice (longan flavor), solid content 15 DEG brix, precooling to 15 ℃. The condensing circulation system 60 is opened to cool so that the temperature of the feed tank 10 and the concentration processor 20 is consistent with the temperature of the liquid material pre-cooling. 2.5L of pre-cooled osmanthus flavored juice is pumped into the inner cavity of the concentration processor 20 from the feeding tank 10; turning on CO 2 Dewar 30 with a regulated bubble diameter of 10 5 After the pressure reaches 120bar, the stirring device 23 of the concentration processor 20 is simultaneously turned on, the rotating speed is set to 1200rpm/min, and the treatment is carried out for 10min; regulating condensation circulation, reducing the temperature of the concentration processor 20 to 4 ℃, and performing phase-change crystallization reaction by deflating treatment to ensure that the pressure in the concentration processor 20 is 50bar and the rotating speed is 1000 rpm/min; the phase change stage and the crystal growth stage are judged according to the pressure and temperature change curves, the pressure drop is detected for the first time, the point of temperature rise is a crystallization point, and the subsequent period of time when the temperature is kept constant is the phase change stage; the temperature starts to continuously decrease, and the pressure also continuously decreases until the pressure is unchanged and is constant for a period of time, and the crystallization stage is adopted; and meanwhile, the temperature of the hydrate crystal tank 40 is increased to 45 ℃, dissolved gas enters the concentrate tank 50, a stirring mechanism 51 of the concentrate tank 50 is opened, and after 20 minutes of treatment, the gas is circulated to the bubble generator 31 again and enters the next recycling. And finally, sterile split charging and storing in a refrigeration house. The obtained osmanthus concentrated juice has a concentration rate of 35%, a polyphenol and Vc retention rate of 94%, and a microorganism quantity of about 10% lower than that of the original juice 8 The flavor characteristic value is not changed, the original flavor and color are maintained, and compared with the single hydrate concentration and the heat sterilization or non-heat sterilization before or after the conventional concentration, the sterilization concentration treatment time is shortened by 15%; compared with the concentration treatment of the hydrate alone, the sterilization rate is improved by 40 percent.
Example IV
A preparation method of litchi concentrated juice adopts the CO-based method of the invention 2 The phase change balance regulating and controlling concentrated solution manufacturing method specifically comprises the following steps:
litchi juice (black leaf), solid content20°brix, precooled to 20 ℃. The condensing circulation system 60 is opened to cool so that the temperature of the feed tank 10 and the concentration processor 20 is consistent with the temperature of the liquid material pre-cooling. Taking 2.5L of precooled black She Guozhi and pumping the precooled black She Guozhi into the inner cavity of the concentration processor 20 from the feed tank 10; turning on CO 2 Dewar 30 with a regulated bubble diameter of 10 7 After the pressure reaches 150bar, setting the rotating speed to 1500rpm/min, and simultaneously turning on the stirring device 23 of the concentration processor 20 for 15min; regulating condensation circulation, setting the rotating speed to 800rpm/min, reducing the temperature of the concentration processor 20 to 5 ℃, and performing gas release treatment to ensure that the pressure in the concentration processor 20 is 60bar to perform phase change crystallization reaction; the phase change stage and the crystal growth stage are judged according to the pressure and temperature change curves, the pressure drop is detected for the first time, the point of temperature rise is a crystallization point, and the subsequent period of time when the temperature is kept constant is the phase change stage; the temperature starts to continuously decrease, and the pressure also continuously decreases until the pressure is unchanged and is constant for a period of time, and the crystallization stage is adopted; and meanwhile, the temperature of the hydrate crystal tank 40 is increased to 50 ℃, dissolved gas enters the concentrate tank 50, a stirring mechanism 51 of the concentrate tank 50 is opened, and after 25 minutes of treatment, the gas is circulated to the bubble generator 31 again and enters the next recycling. And finally, sterile split charging and storing in a refrigeration house. The obtained litchi juice concentrate has a concentration rate of 55%, a retention rate of polyphenol content and Vc content of 94%, and a microbial count of about 10% lower than that of the original extract 6 The chroma is good, compared with the concentration of single hydrate, the concentration sterilization treatment time is shortened by 29% by non-thermal sterilization, and the sterilization rate is improved by 34% compared with the concentration treatment of single hydrate.
Example five
A preparation method of litchi concentrated juice adopts the CO-based method of the invention 2 The phase change balance regulating and controlling concentrated solution manufacturing method specifically comprises the following steps:
litchi juice (longan flavor) with a solid content of 20 DEG brix, and precooling to 20 ℃. The condensing circulation system 60 is opened to cool so that the temperature of the feed tank 10 and the concentration processor 20 is consistent with the temperature of the liquid material pre-cooling. 2.5L of pre-cooled osmanthus flavored juice is pumped from a feed tank 10 into a concentration processor 20 in the inner cavity of the tube; turning on CO 2 Dewar 30 with a regulated bubble diameter of 10 7 After the pressure reaches 150bar, setting the rotating speed to 1500rpm/min, and simultaneously turning on the stirring device 23 of the concentration processor 20 for 15min; regulating condensation circulation, setting the rotating speed to 800rpm/min, reducing the temperature of the concentration processor 20 to 0.5 ℃, and performing gas release treatment to ensure that the pressure in the concentration processor 20 is 20bar to perform phase change crystallization reaction; the phase change stage and the crystal growth stage are judged according to the pressure and temperature change curves, the pressure drop is detected for the first time, the point of temperature rise is a crystallization point, and the subsequent period of time when the temperature is kept constant is the phase change stage; the temperature starts to continuously decrease, and the pressure also continuously decreases until the pressure is unchanged and is constant for a period of time, and the crystallization stage is adopted; and meanwhile, the temperature of the hydrate crystal tank 40 is increased to 50 ℃, dissolved gas enters the concentrate tank 50, a stirring mechanism 51 of the concentrate tank 50 is opened, and after 25 minutes of treatment, the gas is circulated to the bubble generator 31 again and enters the next recycling. And finally, sterile split charging and storing in a refrigeration house. The obtained litchi juice concentrate has a concentration rate of 55%, a retention rate of polyphenol content and Vc content of 94%, and a microbial count of about 10% lower than that of the original extract 6 The chroma is good, compared with the concentration of single hydrate, the concentration sterilization treatment time is shortened by 29% by non-thermal sterilization, and the sterilization rate is improved by 34% compared with the concentration treatment of single hydrate.
Example six
A preparation method of litchi concentrated juice adopts the CO-based method of the invention 2 The phase change balance regulating and controlling concentrated solution manufacturing method specifically comprises the following steps:
litchi juice (longan flavor) with a solid content of 20 DEG brix, and precooling to 20 ℃. The condensing circulation system 60 is opened to cool so that the temperature of the feed tank 10 and the concentration processor 20 is consistent with the temperature of the liquid material pre-cooling. 2.5L of pre-cooled osmanthus flavored juice is pumped into the inner cavity of the concentration processor 20 from the feeding tank 10; turning on CO 2 Dewar 30 with a regulated bubble diameter of 10 7 After the pressure reaches 150bar, setting the rotating speed to 1500rpm/min, and simultaneously turning on the stirring device 23 of the concentration processor 20 for 15min; regulating the condensing cycleThe ring is set at 800rpm/min, the temperature of the concentration processor 20 is reduced to 10 ℃, and the pressure in the concentration processor 20 is 90bar through the deflation treatment, so that the phase-change crystallization reaction occurs; the phase change stage and the crystal growth stage are judged according to the pressure and temperature change curves, the pressure drop is detected for the first time, the point of temperature rise is a crystallization point, and the subsequent period of time when the temperature is kept constant is the phase change stage; the temperature starts to continuously decrease, and the pressure also continuously decreases until the pressure is unchanged and is constant for a period of time, and the crystallization stage is adopted; and meanwhile, the temperature of the hydrate crystal tank 40 is increased to 50 ℃, dissolved gas enters the concentrate tank 50, a stirring mechanism 51 of the concentrate tank 50 is opened, and after 25 minutes of treatment, the gas is circulated to the bubble generator 31 again and enters the next recycling. And finally, sterile split charging and storing in a refrigeration house. The obtained litchi juice concentrate has a concentration rate of 55%, a retention rate of polyphenol content and Vc content of 94%, and a microbial count of about 10% lower than that of the original extract 6 The chroma is good, compared with the concentration of single hydrate, the concentration sterilization treatment time is shortened by 29% by non-thermal sterilization, and the sterilization rate is improved by 34% compared with the concentration treatment of single hydrate.
Example seven
A preparation method of grape seed polyphenol concentrate adopts the CO-based method of the invention 2 The phase change balance regulating and controlling concentrated solution manufacturing method specifically comprises the following steps:
the grape seed polyphenol extract liquid has a solid content of 4 degrees brix and is precooled to 15 ℃. The condensing circulation system 60 is opened to cool so that the temperature of the feed tank 10 and the concentration processor 20 is consistent with the temperature of the liquid material pre-cooling. 2L of precooled grape seed polyphenol extracting solution is pumped into the inner cavity of the concentration processor 20 from the feeding tank 10; turning on CO 2 Dewar 30 with a regulated bubble diameter of 10 2 After the pressure reaches 70bar, setting the rotating speed to 500rpm/min, and simultaneously turning on the stirring device 23 of the concentration processor 20 for 15min; regulating condensation circulation, reducing the temperature of the concentration processor 20 to 4 ℃, and performing phase-change crystallization reaction by deflating treatment to ensure that the pressure in the concentration processor 20 is 50bar and the rotating speed is 1500rpm/min; in which phase transition phase and crystal growthThe judgment of the phase is that according to the pressure and temperature change curve, the pressure drop is detected for the first time, the point of temperature rise is a crystallization point, and the subsequent period of temperature holding is a phase change phase; the temperature starts to continuously decrease, and the pressure also continuously decreases until the pressure is unchanged and is constant for a period of time, and the crystallization stage is adopted; and meanwhile, the temperature of the hydrate crystal tank 40 is increased to 40 ℃, dissolved gas enters the concentrate tank 50, a stirring mechanism 51 of the concentrate tank 50 is opened, and after 8 minutes of treatment, the gas is circulated to the bubble generator 31 again and enters the next recycling. And finally, sterile split charging and storing in a refrigeration house. The obtained grape seed polyphenol concentrated solution has a concentration rate of 40%, a polyphenol antioxidant activity retention rate of 96%, and a microorganism quantity reduced by about 10% compared with the original extract 4 The chroma is good, compared with the concentration shrinkage of single hydrate, the concentration sterilization treatment time is shortened by 20% by non-thermal sterilization, and the sterilization rate is improved by 30% compared with the concentration treatment of single hydrate.
Example eight
The invention relates to a preparation method of apple juice concentrate, which adopts the CO-based method 2 The phase change balance regulating and controlling concentrated solution manufacturing method specifically comprises the following steps:
apple juice, solid content 10 DEG brix, is pre-cooled to 18 ℃. The condensing circulation system 60 is opened to cool so that the temperature of the feed tank 10 and the concentration processor 20 is consistent with the temperature of the liquid material pre-cooling. 2L of pre-cooled apple juice extracting solution is pumped into the inner cavity of the concentration processor 20 from the feeding tank 10; turning on CO 2 Dewar 30 with a regulated bubble diameter of 10 3 After the pressure reaches 90bar, setting the rotating speed to 900rpm/min, and simultaneously turning on the stirring device 23 of the concentration processor 20 for 15min; regulating condensation circulation, setting the rotating speed to 1300rpm/min, reducing the temperature of the concentration processor 20 to 6 ℃, and performing gas release treatment to ensure that the pressure in the concentration processor 20 is 45bar to perform phase change crystallization reaction; the phase change stage and the crystal growth stage are judged according to the pressure and temperature change curves, the pressure drop is detected for the first time, the point of temperature rise is a crystallization point, and the subsequent period of time when the temperature is kept constant is the phase change stage; the temperature starts to drop continuously and the pressure is maintainedContinuing to decrease until the pressure is unchanged for a constant period of time, wherein the stage is a crystallization stage; and meanwhile, the temperature of the hydrate crystal tank 40 is increased to 50 ℃, dissolved gas enters the concentrate tank 50, a stirring mechanism 51 of the concentrate tank 50 is opened, and after 20 minutes of treatment, the gas is circulated to the bubble generator 31 again and enters the next recycling. And finally, sterile split charging and storing in a refrigeration house. The obtained apple juice concentrate has a concentration rate of 45%, a polyphenol content and phenolic acid retention rate of 92%, and a microorganism quantity reduced by about 10% compared with the original extract 5 The chroma is good, compared with the concentration shrinkage of single hydrate, the concentration sterilization treatment time is shortened by 25% by non-thermal sterilization, and the sterilization rate is improved by 28% compared with the concentration treatment of single hydrate.
Example nine
The preparation method of the orange juice concentrate adopts the CO-based method 2 The phase change balance regulating and controlling concentrated solution manufacturing method specifically comprises the following steps:
orange juice with a solids content of 10 DEG brix is pre-cooled to 15 ℃. The condensing circulation system 60 is opened to cool so that the temperature of the feed tank 10 and the concentration processor 20 is consistent with the temperature of the liquid material pre-cooling. 2.5L of pre-cooled orange juice is pumped from the feed tank 10 into the inner cavity of the concentration processor 20; turning on CO 2 Dewar 30 with a regulated bubble diameter of 10 3 After the pressure reaches 90bar at nm, simultaneously turning on a stirring device 23 of the concentration processor 20, setting the rotating speed to be 500rpm/min, and processing for 10min; regulating condensation circulation, reducing the temperature of the concentration processor 20 to 6 ℃, and performing phase-change crystallization reaction by deflating treatment to ensure that the pressure in the concentration processor 20 is 50bar and the rotating speed is 1300rpm/min; the phase change stage and the crystal growth stage are judged according to the pressure and temperature change curves, the pressure drop is detected for the first time, the point of temperature rise is a crystallization point, and the subsequent period of time when the temperature is kept constant is the phase change stage; the temperature starts to continuously decrease, and the pressure also continuously decreases until the pressure is unchanged and is constant for a period of time, and the crystallization stage is adopted; simultaneously, the temperature of the hydrate crystal tank 40 is increased to 45 ℃, dissolved gas enters the concentrate tank 50, the stirring mechanism 51 of the concentrate tank 50 is opened, after 15min of treatment,the gas is recirculated to the bubble generator 31 for the next cycle. And finally, sterile split charging and storing in a refrigeration house. The obtained concentrated juice has concentration rate up to 45%, polyphenol and Vc retention rate up to 90%, and microorganism amount reduced by about 10% compared with original juice 6 The flavor characteristic value is not changed, the original flavor and color are maintained, and compared with the single hydrate concentration and the heat sterilization or non-heat sterilization before or after the conventional concentration, the sterilization concentration treatment time is shortened by 25%; compared with the concentration treatment of the hydrate alone, the sterilization rate is improved by 30 percent.
The above examples illustrate only a few embodiments of the invention, which are described in detail and are not to be construed as limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention.
Claims (1)
1. Based on CO 2 The phase change balance regulating and controlling concentrated solution manufacturing method is characterized by comprising the following steps:
pre-cooling the liquid material to 15-20 ℃, wherein the concentration of the liquid material is 4-20 DEG C o brix, controlling the temperature of the inner cavity of the concentration processor (20) to be consistent with the precooling temperature of the liquid material;
feeding the precooled liquid material into the concentration processor (20);
feeding CO into the interior of the concentration processor (20) 2 And the diameter of the air bubble is regulated by a bubble generator (31), the diameter of the air bubble is 10 2 ~10 7 nm；
After the pressure of the inner cavity of the concentration processor (20) is 50-150 bar, stirring the liquid material, setting the stirring speed to be 500-1500 rpm/min, and simultaneously maintaining the pressure of the inner cavity of the concentration processor (20) for 5-15 min;
after the liquid material is stirred for a period of time, reducing the temperature of the inner cavity of the concentration processor (20) to 0.5-10 ℃, and regulating the pressure of the inner cavity of the concentration processor (20) to 20-90 bar;
the liquid material undergoes a phase-change crystallization reaction, and hydrate crystals and concentrated solution are formed after the liquid material undergoes a phase-change stage and a crystal growth stage, wherein the phase-change stage and the crystal growth stage are both carried out under stirring conditions, and the stirring speed in the phase-change stage and the crystal growth stage is 800-1500 rpm/min;
continuing to aerate while the pressure is decreasing during agitation to maintain the pressure in the internal chamber of the concentrating processor (20);
the hydrate crystals enter a hydrate crystal tank (40), and the concentrated solution enters a concentrated solution tank (50); adjusting the temperature of the hydrate crystal tank (40) to 40-60 ℃, stirring the hydrate crystal, dissolving out gas from the hydrate crystal, and introducing the dissolved gas into the concentrated liquid tank (50) to sterilize the concentrated liquid; the pressure of the concentrate tank (50) is regulated to be 50-150 bar, concentrate in the concentrate tank (50) is stirred, and the stirring rotating speed is set to be 1500-2500 rpm/min; the gas in the concentrated liquid tank (50) firstly enters the bubble generator (31) and then enters the concentrated processor (20);
the relationship among the concentration of the liquid material, the diameter of the bubbles, the pressure before cooling the concentration processor (20), the stirring speed when the pressure of the inner cavity of the concentration processor (20) is 50-150 bar, and the stirring speed in the phase-change stage and the crystal growth stage is as follows:
the concentration is 4-10 o brix of said diameter of 10 2 ~10 3 The pressure is 50-90 bar, the stirring speed is 500-900 rpm/min, and the stirring speed is 1300-1500 rpm/min;
the concentration is 10-15 o brix of said diameter of 10 3 ~10 5 The pressure is 90-120 bar, the stirring speed is 900-1200 rpm/min, and the stirring speed is 1000-1300 rpm/min;
the concentration is 15-20 o brix of said diameter of 10 5 ~10 7 nm, the pressure is 120-150 bar, and the stirring rotation speed is the same as that of the former1200-1500 rpm/min, the latter stirring speed being 800-1500 rpm/min;
the phase change phase refers to: after the continuous inflation is finished, the system pressure is reduced for the first time, the temperature of the liquid material starts to rise to be a starting point, and the temperature of the liquid material keeps stable or falls to be a starting point to be a finishing point, wherein the phase is a phase change phase and is obtained by an online temperature-pressure monitoring curve;
the crystal growth stage refers to: after the phase change phase is finished, the system temperature starts to continuously decrease or the system temperature starts to decrease from the starting point temperature of the phase change phase, the pressure also continuously decreases until the pressure is not changed any more, and the pressure is kept constant for a period of time, and the phase is a crystal growth phase.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110290869.4A CN114452672B (en) | 2021-03-18 | 2021-03-18 | Based on CO 2 Concentrated solution manufacturing device and method for phase change balance regulation and control |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110290869.4A CN114452672B (en) | 2021-03-18 | 2021-03-18 | Based on CO 2 Concentrated solution manufacturing device and method for phase change balance regulation and control |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114452672A CN114452672A (en) | 2022-05-10 |
| CN114452672B true CN114452672B (en) | 2023-06-16 |
Family
ID=81406196
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110290869.4A Active CN114452672B (en) | 2021-03-18 | 2021-03-18 | Based on CO 2 Concentrated solution manufacturing device and method for phase change balance regulation and control |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114452672B (en) |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3953615A (en) * | 1971-08-03 | 1976-04-27 | The Coca-Cola Co. | Hydration drying of coffee, tea, or juice concentrate by means of anhydrous dextrose |
| JPH03278801A (en) * | 1990-03-27 | 1991-12-10 | Toyo Eng Works Ltd | Pressure type freezing concentrator |
| JP2003138281A (en) * | 2001-08-23 | 2003-05-14 | National Institute Of Advanced Industrial & Technology | Separating agent for gas, and method and apparatus for separating and concentrating gas |
| CN1617919A (en) * | 2002-09-11 | 2005-05-18 | 杰富意工程股份有限公司 | Method and apparatus for producing gas clathrate |
| CN110050914A (en) * | 2018-12-24 | 2019-07-26 | 广东省农业科学院蚕业与农产品加工研究所 | A kind of electric field-assisted improves the method and device of hydrate inspissated juice quality |
| CN212236048U (en) * | 2020-03-18 | 2020-12-29 | 广东省农业科学院蚕业与农产品加工研究所 | Gas hydrate concentrating device |
| CN112244184A (en) * | 2020-09-30 | 2021-01-22 | 广东省农业科学院蚕业与农产品加工研究所 | Device and method for concentrating liquid food by hydrate under assistance of frequency conversion ultrasound |
| CN215137037U (en) * | 2021-03-18 | 2021-12-14 | 广东省农业科学院蚕业与农产品加工研究所 | Concentrated solution manufacturing installation based on CO2 phase transition balance regulation and control |
-
2021
- 2021-03-18 CN CN202110290869.4A patent/CN114452672B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3953615A (en) * | 1971-08-03 | 1976-04-27 | The Coca-Cola Co. | Hydration drying of coffee, tea, or juice concentrate by means of anhydrous dextrose |
| JPH03278801A (en) * | 1990-03-27 | 1991-12-10 | Toyo Eng Works Ltd | Pressure type freezing concentrator |
| JP2003138281A (en) * | 2001-08-23 | 2003-05-14 | National Institute Of Advanced Industrial & Technology | Separating agent for gas, and method and apparatus for separating and concentrating gas |
| CN1617919A (en) * | 2002-09-11 | 2005-05-18 | 杰富意工程股份有限公司 | Method and apparatus for producing gas clathrate |
| CN110050914A (en) * | 2018-12-24 | 2019-07-26 | 广东省农业科学院蚕业与农产品加工研究所 | A kind of electric field-assisted improves the method and device of hydrate inspissated juice quality |
| CN212236048U (en) * | 2020-03-18 | 2020-12-29 | 广东省农业科学院蚕业与农产品加工研究所 | Gas hydrate concentrating device |
| CN112244184A (en) * | 2020-09-30 | 2021-01-22 | 广东省农业科学院蚕业与农产品加工研究所 | Device and method for concentrating liquid food by hydrate under assistance of frequency conversion ultrasound |
| CN215137037U (en) * | 2021-03-18 | 2021-12-14 | 广东省农业科学院蚕业与农产品加工研究所 | Concentrated solution manufacturing installation based on CO2 phase transition balance regulation and control |
Non-Patent Citations (2)
| Title |
|---|
| 《果汁冷冻浓缩加工技术和设备研究进展》;吴继军;《现代农业装备》;20200630;第78-81页 * |
| 气/液态氮在食品加工技术中的应用机制和研究进展;程丽娜等;《食品与发酵工业》;20200409(第13期);全文 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114452672A (en) | 2022-05-10 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US20220264912A1 (en) | Reduced calorie beverage or food product and process and apparatus for making same | |
| CN100482106C (en) | Active peptide fruity beer and its preparing method | |
| CN101664214B (en) | Ultrasonic synergetic crystal growing fruit juice freezing and concentrating method and equipment thereof | |
| CN105682762B (en) | Using the manufacturing method of membrane concentration method and the concentrated product of freeze concentration method | |
| CN215137037U (en) | Concentrated solution manufacturing installation based on CO2 phase transition balance regulation and control | |
| SE459098B (en) | PROCEDURES FOR PREPARING ALCOHOLIC REDUCED WINE | |
| CZ291236B6 (en) | Process for preparing a fermented malt beverage | |
| CN114452672B (en) | Based on CO 2 Concentrated solution manufacturing device and method for phase change balance regulation and control | |
| CN111134217A (en) | Processing method of cold-extracted fresh leaf instant tea concentrated solution | |
| JP4238312B2 (en) | Incense vinegar | |
| CN112244184B (en) | Device and method for concentrating liquid food by hydrate under assistance of frequency conversion ultrasound | |
| CN203138087U (en) | Carbonic water preparing device | |
| CN106987608A (en) | A kind of crystallization in motion of calcium gluconae | |
| CN105658293A (en) | Production method for concentrated product using freeze-concentration method | |
| WO2019049644A1 (en) | Dissolved gas-containing ice production device and production method | |
| US2559204A (en) | Method of freeze dehydration of liquid bearing substances | |
| US3285022A (en) | Concentration of extracts by freezing | |
| US1997277A (en) | Crystallization apparatus | |
| Jusoh et al. | Progressive freeze concentration of coconut water | |
| Dette et al. | Freeze concentration of black currant juice | |
| JPH11130195A (en) | Energy-saving system for recycling waste heat at manufacturing factory of carbonated beverage including beer | |
| CN212236048U (en) | Gas hydrate concentrating device | |
| US3389567A (en) | Method of crystallizing fluids | |
| CN215653903U (en) | Durene crystallization device | |
| JP6121661B2 (en) | Interface forward freeze concentration apparatus and interface forward freeze concentration method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |