CN215137037U - Concentrated solution manufacturing installation based on CO2 phase transition balance regulation and control - Google Patents
Concentrated solution manufacturing installation based on CO2 phase transition balance regulation and control Download PDFInfo
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- CN215137037U CN215137037U CN202120560245.5U CN202120560245U CN215137037U CN 215137037 U CN215137037 U CN 215137037U CN 202120560245 U CN202120560245 U CN 202120560245U CN 215137037 U CN215137037 U CN 215137037U
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Abstract
The utility model relates to a based on CO2The phase-change balance controlled concentrated liquid producing apparatus includes concentrating processor and CO2The device comprises a Dewar flask, a hydrate crystal tank, a concentrated liquid tank, a condensation circulation system and a heat circulation system, wherein the concentration processor is used for carrying out phase change crystallization reaction on liquid materials to generate concentrated liquid and hydrate crystals, CO2The gas outlet of the Dewar flask is communicated with the gas inlet of the concentration processor through a bubble generator, the feed inlet of the hydrate crystal tank is communicated with the hydrate outlet of the concentration processor, and the feed inlet of the concentrate tank is communicated with the hydrate outlet of the concentration processorThe gas outlet of the concentrated liquid tank is communicated with the gas outlet of the hydrate crystal tank, the gas outlet of the concentrated liquid tank is communicated with the gas inlet of the bubble generator, the condensation circulating system is used for refrigerating the concentrated processor, and the heat circulating system is used for heating the hydrate crystal tank.
Description
Technical Field
The utility model relates to a concentrated liquid material technical field in fields such as bio-pharmaceuticals, food, chemical synthesis especially relates to one kind and is based on CO2A phase-change balance control concentrated solution manufacturing device.
Background
The concentrated solution is widely distributed in the fields of biological pharmacy and food processing as a semi-finished product or product, and the concentration means with high efficiency, high quality and low cost is always the urgent need of the concentration industry.
The hydrate method concentration is a concentration method for obtaining concentrated solution after solid-liquid separation, wherein under certain pressure and temperature, guest gas water molecules and host water molecules in the solution form a cage-shaped structure substance similar to ice crystals; similar to the effect of the currently accepted relatively optimal freeze concentration, there is a similar problem of solute loss in the crystals, but with lower energy consumption than if a sub-zero low temperature is not required. Therefore, the forming speed, the shape and the size of the hydrate crystal are effectively regulated and controlled, and the stable, abundant and pure hydrate crystal is obtained, so that the 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 hydrate method concentrated liquid food.
The formation of the hydrate comprises two stages of crystal nucleation and crystal growth, gas molecules enter the solution at the early stage of nucleation, gas bubbles gradually become small along with the gas-liquid mass transfer, the gas molecules enter a cage-shaped hole structure formed by water molecules of a main body, the nucleation phenomenon occurs, the main and object molecules are mutually associated through Van der Waals force and are continuously gathered to slowly form a stable cage, and finally, the 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 freeze concentration is limited to a relative extent due to high energy consumption. Currently, the gas hydrate concentration technology, which is a concentration technology comparable to freeze concentration, can maximally retain the quality of materials. But also similar to the freeze concentration, the solute of the solution is easy to be entrained and even embedded in the crystal forming process (forming cage-shaped structural substances), and the entrainment rate of the hydrate is one of the main factors limiting the popularization and the application of the hydrate.
Therefore, the existing concentration technology has some defects, which are mainly represented as follows:
(1) in the existing concentration technology, evaporation concentration with high concentration efficiency seriously damages heat-sensitive functional and nutritional ingredients in materials.
(2) The requirements of relatively high quality freeze concentration and low freezing temperature thereof cause high energy consumption and long time for concentration, and in addition, sterilization treatment is still required to store the finished concentrated juice for a long time.
(3) The single hydrate is concentrated, the sterilization effect on materials is limited, the phenomenon of sublethal microorganism occurs, and the long-term storage can be realized only by auxiliary sterilization treatment.
SUMMERY OF THE UTILITY MODEL
Based on this, the utility model aims at providing a based on CO2The phase-change balance regulation and control concentrated solution manufacturing device can obtain high-quality concentrated solution, is safe and ensures the storage quality.
Based on CO2The phase-change equilibrium controlled concentrated solution manufacturing device comprises a concentration processor and CO2The device comprises a Dewar flask, a hydrate crystal tank, a concentrated liquid tank, a condensation circulation system and a heat circulation system, wherein the concentration processor is used for carrying out phase change crystallization reaction on liquid materials to generate concentrated liquid and hydrate crystals, and the CO is2The gas outlet of the Dewar flask is communicated with the gas inlet of the concentration processor through a bubble generator, and the feed inlet of the hydrate crystal tank is communicated with the gas inlet of the concentration processorThe hydrate outlet of the concentration processor is communicated, the feed inlet of the concentrated liquid tank is communicated with the concentrated liquid outlet of the concentration processor, the air inlet of the concentrated liquid tank is communicated with the air outlet of the hydrate crystal tank, the air outlet of the concentrated liquid tank is communicated with the air inlet of the bubble generator, the condensation circulating system is used for refrigerating the concentration processor, and the heat circulating system is used for heating the hydrate crystal tank.
Further, a feeding pump is arranged between the discharge hole of the feeding tank and the feeding hole of the concentration processor.
Further, in the CO2A booster pump or a compressor is arranged between the air outlet of the Dewar flask and the bubble generator.
Further, the concentration 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 the liquid material in the concentration processor.
Further, a K-type thermocouple positioned in the interlayer of the shell body is arranged in the inner cavity of the shell body; a transparent observation window is also arranged on the inner shell; a high-speed camera is also arranged in the inner cavity of the inner shell; a pressure sensor is also arranged in the inner cavity of the inner shell; and a K-type thermocouple is also arranged in the inner cavity of the inner shell.
Further, 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 heat circulation system, the stirrer is arranged in the inner tank body, and the stirrer is used for stirring the hydrate crystals in the hydrate crystal tank.
Furthermore, K-type thermocouples are arranged in the tank body interlayer and the inner cavity of the inner tank body.
Further, 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.
Further, still include the feeding jar, the feeding jar is used for storing liquid material, the discharge gate of feeding jar with the feed inlet of concentrated treater is linked together.
Further, still include the storage tank, the feed inlet of storage tank with the discharge gate of concentrate jar is linked together.
For a better understanding and an implementation, the present invention is described in detail below with reference to the accompanying drawings.
Drawings
FIG. 1 shows that the present invention is based on CO2The structure schematic diagram of a phase-change balance-controlled concentrated solution manufacturing device;
fig. 2 is a schematic structural diagram of a concentration processor according to the present invention;
fig. 3 is a schematic structural diagram of a hydrate crystal tank according to the present invention;
fig. 4 is a schematic structural diagram of the concentrated liquid tank of the present invention;
reference numerals:
10. a feed tank; 11. a feed pump; 20. a concentration processor; 21. a housing; 22. an inner shell; 23. a stirring device; 24. a housing interlayer; 30. CO22A dewar flask; 31. a bubble generator; 40. a hydrate crystal tank; 41. an outer tank body; 42. an inner tank body; 43. a stirrer; 44. a tank body interlayer; 50. a concentrated liquid tank; 51. a stirring mechanism; 60. a condensation circulation system; 70. a heat cycle system; 80. a material storage tank.
Detailed Description
Based on CO2The preparation method of the phase-change equilibrium-regulated concentrated solution is shown in figure 1 and comprises the following steps:
s1, obtaining a liquid material with the concentration of 4-20 degrees brix, pre-cooling the liquid material to 15-20 ℃, 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 material;
s2, filling the pre-cooled liquid material into a feeding tank 10, and pumping the pre-cooled liquid material into an inner cavity of a concentration processor 20 from the feeding tank 10;
s3, feeding CO into the inner cavity of the concentration processor 202And CO is regulated by the bubble generator 312The diameter of the bubble of (2), the diameter of the bubble being 102～107nm；
S4, stirring the liquid material after the pressure of the inner cavity of the processor 20 to be concentrated is 50-150 bar, setting the stirring speed to be 500-500 rpm/min, and simultaneously maintaining the pressure of the inner cavity of the processor 20 to be concentrated for 5-15 min; during the stirring period, when the pressure is reduced, the aeration is continued to maintain the pressure of the inner cavity of the concentration processor 20;
s5, after the liquid material is stirred for a period of time, not only is the stirring continuously carried out, the stirring speed is set to be 800-1500 rpm/min, but also 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 be 20-90 bar, the liquid material is subjected to phase change crystallization reaction, and the liquid material forms hydrate crystals and concentrated liquid after undergoing a phase change stage and a crystal growth stage;
s6, after the pressure in the inner cavity of the processor 20 to be concentrated is stabilized 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 ℃, melting out gas from the hydrate crystal, and feeding the melted gas into the concentrated liquid tank 50;
s8, adjusting the pressure of the concentrated liquid tank 50 to 50-150 bar, stirring the concentrated liquid, setting the stirring speed to be 1500-2500 rpm/min, and performing secondary sterilization on the concentrated liquid;
s9, after the concentrated solution is sterilized for a period of time for the second time, the gas in the concentrated solution tank 50 enters the concentration processor 20 again from the bubble generator 31 and enters the next cycle for utilization;
s10, after the secondary sterilization is finished, the concentrated solution enters the storage tank 80 from the concentrated solution tank 50;
and S11, performing sterile subpackage on the concentrated solution, and storing in a refrigeration house.
In the practical implementation process, according to different viscosity and concentration of materials, the diameter of the bubbles is regulated, and simultaneously, the gas-liquid contact can be effectively promoted, the heat and mass transfer is enhanced, and the formation and sterilization effects of hydrate crystals are promoted by combining the regulation of temperature, the regulation of corresponding pressure and the regulation of stirring speed.
Thus, for step S3, the relationship between the concentration of the liquid material and the diameter of the bubble is:
the concentration of the liquid material is 4-10 degrees brix, and the diameter of the air bubble is 102～103nm；
The concentration of the liquid material is 10-15 degrees brix, and the diameter of the air bubble is 103～105nm；
The concentration of the liquid material is 15-20 degrees brix, and the diameter of the air bubble is 105～107nm。
For step S4, the relationship among the concentration of the liquid material, the pressure in the inner cavity of the concentration processor 20, and the stirring speed when the pressure in the inner cavity of the concentration processor 20 is 50 to 150bar is as follows:
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 degrees 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 change phase refers to that after the continuous inflation is finished, the system pressure first drops, the temperature of the liquid material starts to rise to the starting point, and the temperature of the liquid material remains stable or drops to the starting point as the end point, which is the phase change phase and is obtained from the online temperature and pressure monitoring curve. The crystal growth phase refers to that after the phase change phase is finished, the temperature of the system begins to continuously decrease or the temperature begins to decrease from the initial point of the phase change phase, the pressure also continues to decrease until the pressure does not change, and the pressure is kept constant for a period of time, and the phase is the crystal growth phase.
Specifically, in step S7, the hydrate crystals may be stirred, thereby promoting the melting of the hydrate crystals.
Specifically, in step S9, the processing time for performing the secondary sterilization process on the concentrated solution depends on the sterilization effect of the concentrated solution of different materials.
Compared with the prior art, the device based on CO2The preparation method of the phase-change balance-controlled concentrated solution has the following beneficial effects:
(1) in the early stage of the concentration phase change, the diameter, the temperature, the corresponding pressure and the processing time of bubbles can be regulated and controlled according to the concentration of the initial material, so that not only can the gas-liquid contact be effectively promoted and the heat and mass transfer effects be enhanced, but also the next phase change can be promoted and the sterilization purpose 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 microbial lethal effect is achieved;
(3) the gas generated by the melt crystallization is utilized to carry out secondary sterilization on the concentrated solution, and after the sterilization is finished, the concentrated solution is recycled again to carry out concentrated phase change, so that the energy consumption is effectively saved, and no additional sterilization treatment is needed.
(4) Compared with single hydrate concentration treatment, the utility model can increase the sterilization rate by more than 30%;
(5) for the concentrated processing of single hydrate traditional germicidal treatment in coordination, the utility model discloses can save time more than 15%, the quality improves more than 20%.
For automatically realizing the above concentrated solution manufacturing method based on CO2 phase-change balance regulation, the utility model also provides a concentrated solution system based on CO2 phase-change balance regulationAnd (5) manufacturing a device. Referring to fig. 1 to 4, the apparatus comprises a feed tank 10, a concentration processor 20, CO2Dewar 30, hydrate crystal jar 40, concentrate liquid jar 50, condensation circulation system 60, heat cycle system 70, storage tank 80. Wherein, the feeding tank 10 is used for storing liquid materials, and a discharge hole of the feeding tank 10 is communicated with a feed hole of the concentration processor 20; a feed pump 11 is provided between the discharge port of the feed tank 10 and the feed port of the concentration processor 20, and the liquid material in the feed tank 10 is transported to the concentration processor 20 by the feed pump 11. CO22Dewar 30 for storing CO2Gas, CO2The air outlet of the Dewar flask 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 flask 30 and the air inlet of the concentration processor 20, and the CO is regulated and controlled by the bubble generator 312The diameter of the bubble; in CO2A booster pump or compressor is provided between the air outlet of the dewar 30 and the bubble generator 31, and CO is supplied by the booster pump or compressor2To 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 concentrated liquid tank 50. The concentrated solution tank 50 is used for storing concentrated solution, a feed inlet of the concentrated solution tank 50 is communicated with a concentrated solution outlet of the concentration processor 20, and an air outlet of the concentrated solution tank 50 is communicated with an air inlet of the bubble generator 31. The condensing cycle system 60 is used to refrigerate the feed tank 10 and the concentration processor 20. The heat cycle system 70 is used to heat the hydrate crystal tank 40. The storage tank 80 is used for storing the sterilized concentrated solution, 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 comprises an outer shell 21, an inner shell 22 and a stirring device 23. Wherein, the inner shell 22 is arranged in the outer shell 21, a shell interlayer 24 is arranged between the inner shell 22 and the outer shell 21, and the shell interlayer 24 is communicated with the condensation circulating system 60. The stirring device 23 is disposed in the inner cavity of the inner casing 22, the stirring device 23 is used for stirring the liquid material in the concentration 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 K-type thermocouple is installed in the inner cavity of the outer shell 21, the K-type thermocouple is located in the shell interlayer 24, and the temperature of the inner cavity of the outer shell 21 is collected by the K-type thermocouple. A transparent viewing window is also provided in the inner housing 22 to allow a user to view the operation of the concentrator/processor 20. A high-speed camera is also arranged in the inner cavity of the inner shell 22, and the working condition in the concentration processor 20 is collected through the high-speed camera. A pressure sensor is also installed in the inner cavity of the inner casing 22, and the pressure sensor is used to detect the pressure of the inner cavity of the inner casing 22. A K-type thermocouple is also installed in the inner cavity of the inner shell 22, and the temperature of the inner cavity of the inner shell 22 is collected by the K-type thermocouple. The pressure and temperature can be monitored on line by the K-type thermocouple and the pressure sensor, and the pressure and temperature can be used for 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 can be adjusted.
Specifically, the hydrate crystal tank 40 includes an outer tank 41, an inner tank 42, and a stirrer 43. Wherein, the inner tank 42 is arranged in the outer tank 41, a tank interlayer 44 is arranged between the inner tank 42 and the outer tank 41, and the tank interlayer 44 is communicated with the heat cycle system 70. The stirrer 43 is disposed in the inner cavity of the inner tank 42, and the stirrer 43 is used for stirring the hydrate crystals in the hydrate crystal tank 40 and promoting the melting of the hydrate crystals. Further, K-type thermocouples are provided in the inner cavities of both the tank sandwich 44 and the inner tank 42, and the temperature of the hydrate crystal is observed by the K-type thermocouples to determine the degree of melting.
Specifically, a K-type thermocouple is installed in the inner cavity of the concentrate tank 50, and the temperature of the concentrate is observed by the K-type thermocouple. A pressure sensor is further 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 K-type thermocouple and pressure sensor can be used to determine the physical state of the carbon dioxide in the concentrate tank 50 for further adjustment of the sterilization process. Further, a stirring mechanism 51 is provided in the concentrated liquid tank 50, and the concentrated liquid in the concentrated liquid tank 50 is stirred by the stirring mechanism 51.
Example one
The invention relates to a preparation method of litchi concentrated juice, which adopts the concentrated juice based on CO2The preparation method of the phase change balance regulating and controlling concentrated solution specifically comprises the following steps:
extracting to obtain litchi vitamin C extract with solid content of 4obrix, and precooling to 15 ℃. The condensing circulation system 60 is opened for cooling, so that the temperature of the feeding tank 10 and the concentration processor 20 is consistent with the precooling temperature of the liquid material. Pumping pre-cooled 2.5L of extractive solution from the feed tank 10 into the inner cavity of the concentration processor 20; opening of CO2A Dewar flask 30 with bubble diameter of 102When the pressure reaches 50bar, simultaneously opening a stirring device 23 of the concentration processor 20, setting the rotating speed at 500rpm/min, and processing for 10 min; adjusting condensation circulation, reducing the temperature of the concentration processor 20 to 2 ℃, and performing gas discharge treatment to ensure that the pressure in the concentration processor 20 is 70bar and the rotating speed is adjusted to 1300rpm/min to perform phase change crystallization reaction; wherein, the phase transition stage and the crystal growth stage are judged according to the pressure and temperature change curves, the first time of detecting the pressure drop, the temperature rising point is the crystallization point, and the subsequent period of constant temperature is the phase transition stage; the temperature begins to continuously decrease, the pressure also continuously decreases until the pressure is not changed and is constant for a period of time, and the period is a crystallization period; and meanwhile, the temperature of the hydrate crystal tank 40 is increased to 45 ℃, the dissolved gas enters the concentrated solution tank 50, the stirring mechanism 51 of the concentrated solution tank 50 is opened, and after 10min of treatment, the gas is circulated to the bubble generator 31 again and enters the next cycle for utilization. Finally, aseptically subpackaging and storing in a refrigeration house. The concentration rate of the obtained vitamin C concentrated solution reaches 40 percent, the retention rate of polyphenol and Vc reaches 95 percent, and the number of microorganisms is reduced by about 10 percent compared with that of the original solution6The color and luster are not changed, and the sterilization and concentration treatment time is shortened by 20 percent compared with the single hydrate concentration and the heat sterilization or non-heat sterilization before or after the conventional concentration; compared with the concentration treatment of single hydrate, the sterilization rate is improved by 20 percent.
Example two
The invention relates to a preparation method of litchi concentrated juice, which adopts the concentrated juice based on CO2Preparation of concentrated solution for phase change balance regulationThe method specifically comprises the following steps:
the litchi juice (osmanthus flavor) with the solid content of 10 degrees brix is pre-cooled to 15 ℃. The condensing circulation system 60 is opened for cooling, so that the temperature of the feeding tank 10 and the concentration processor 20 is consistent with the precooling temperature of the liquid material. Pumping 2.5L of pre-cooled Osmanthus-flavored fruit juice from a feed tank 10 into the inner cavity of a concentration processor 20; opening of CO2A Dewar flask 30 with bubble diameter of 103When the pressure reaches 90bar, simultaneously opening a stirring device 23 of the concentration processor 20, setting the rotating speed at 500rpm/min, and processing for 10 min; adjusting condensation circulation, reducing the temperature of the concentration processor 20 to 6 ℃, and performing gas discharge treatment to ensure that the pressure in the concentration processor 20 is 50bar and the rotating speed is adjusted to 1300rpm/min to perform phase change crystallization reaction; wherein, the phase transition stage and the crystal growth stage are judged according to the pressure and temperature change curves, the first time of detecting the pressure drop, the temperature rising point is the crystallization point, and the subsequent period of constant temperature is the phase transition stage; the temperature begins to continuously decrease, the pressure also continuously decreases until the pressure is not changed and is constant for a period of time, and the period is a crystallization period; and meanwhile, the temperature of the hydrate crystal tank 40 is increased to 45 ℃, the dissolved gas enters the concentrated solution tank 50, the stirring mechanism 51 of the concentrated solution tank 50 is opened, and after the gas is treated for 15min, the gas is circulated to the bubble generator 31 again and enters the next cycle for utilization. Finally, aseptically subpackaging and storing in a refrigeration house. The obtained fructus Cinnamomi concentrated juice has concentration rate of 35%, polyphenol and Vc retention rate of 94%, and microorganism amount reduced by 10% compared with original juice8The flavor characteristic value is not changed, the original flavor and color are retained, and compared with single hydrate concentration and heat sterilization or non-heat sterilization before or after conventional concentration, the sterilization concentration processing time is shortened by 15%; compared with the concentration treatment of single hydrate, the sterilization rate is improved by 40 percent.
EXAMPLE III
The invention relates to a preparation method of litchi concentrated juice, which adopts the concentrated juice based on CO2The preparation method of the phase change balance regulating and controlling concentrated solution specifically comprises the following steps:
the litchi juice (osmanthus flavor) with the solid content of 15 degrees brix is pre-cooled to 15 ℃. Open condensationThe circulation system 60 cools the feed tank 10 and the concentration processor 20 to a temperature consistent with the pre-cooling temperature of the liquid material. Pumping 2.5L of pre-cooled Osmanthus-flavored fruit juice from a feed tank 10 into the inner cavity of a concentration processor 20; opening of CO2A Dewar flask 30 with bubble diameter of 105When the pressure reaches 120bar, simultaneously opening a stirring device 23 of the concentration processor 20, and setting the rotating speed to 1200rpm/min for processing for 10 min; adjusting condensation circulation, reducing the temperature of the concentration processor 20 to 4 ℃, and performing gas discharge treatment to ensure that the pressure in the concentration processor 20 is 50bar and the rotating speed is adjusted to 1000rpm/min to perform phase change crystallization reaction; wherein, the phase transition stage and the crystal growth stage are judged according to the pressure and temperature change curves, the first time of detecting the pressure drop, the temperature rising point is the crystallization point, and the subsequent period of constant temperature is the phase transition stage; the temperature begins to continuously decrease, the pressure also continuously decreases until the pressure is not changed and is constant for a period of time, and the period is a crystallization period; and meanwhile, the temperature of the hydrate crystal tank 40 is increased to 45 ℃, the dissolved gas enters the concentrated solution tank 50, the stirring mechanism 51 of the concentrated solution tank 50 is opened, and after 20min of treatment, the gas is circulated to the bubble generator 31 again and enters the next cycle for utilization. Finally, aseptically subpackaging and storing in a refrigeration house. The obtained fructus Cinnamomi concentrated juice has concentration rate of 35%, polyphenol and Vc retention rate of 94%, and microorganism amount reduced by 10% compared with original juice8The flavor characteristic value is not changed, the original flavor and color are retained, and compared with single hydrate concentration and heat sterilization or non-heat sterilization before or after conventional concentration, the sterilization concentration processing time is shortened by 15%; compared with the concentration treatment of single hydrate, the sterilization rate is improved by 40 percent.
Example four
The invention relates to a preparation method of litchi concentrated juice, which adopts the concentrated juice based on CO2The preparation method of the phase change balance regulating and controlling concentrated solution specifically comprises the following steps:
litchi juice (black leaf) with solid content of 20 degree brix, precooled to 20 ℃. The condensing circulation system 60 is opened for cooling, so that the temperature of the feeding tank 10 and the concentration processor 20 is consistent with the precooling temperature of the liquid material. Taking 2.5L of pre-cooled black leaf juiceThe charging bucket 10 is pumped into the inner cavity of the concentration processor 20; opening of CO2A Dewar flask 30 with bubble diameter of 107Setting the rotating speed to be 1500rpm/min after the pressure reaches 150bar, and simultaneously opening a stirring device 23 of the concentration processor 20 for processing for 15 min; adjusting condensation circulation, setting the rotation speed to be 800rpm/min, reducing the temperature of the concentration processor 20 to be 5 ℃, and performing gas discharge treatment to ensure that the pressure in the concentration processor 20 is 60bar to perform phase change crystallization reaction; wherein, the phase transition stage and the crystal growth stage are judged according to the pressure and temperature change curves, the first time of detecting the pressure drop, the temperature rising point is the crystallization point, and the subsequent period of constant temperature is the phase transition stage; the temperature begins to continuously decrease, the pressure also continuously decreases until the pressure is not changed and is constant for a period of time, and the period is a crystallization period; and meanwhile, the temperature of the hydrate crystal tank 40 is increased to 50 ℃, the dissolved gas enters the concentrated solution tank 50, the stirring mechanism 51 of the concentrated solution tank 50 is opened, and after the treatment for 25min, the gas is circulated to the bubble generator 31 again and enters the next cycle for utilization. Finally, aseptically subpackaging and storing in a refrigeration house. The concentration rate of the obtained litchi juice concentrated solution reaches 55%, the retention rate of polyphenol content and Vc content reaches 94%, and the number of microorganisms is reduced by about 10% compared with the original extracting solution6The color is good, the time of concentrated sterilization is shortened by 29% compared with the method of concentrating a single hydrate and assisting non-thermal sterilization, and the sterilization rate is improved by 34% compared with the method of concentrating a single hydrate.
EXAMPLE five
The invention relates to a preparation method of litchi concentrated juice, which adopts the concentrated juice based on CO2The preparation method of the phase change balance regulating and controlling concentrated solution specifically comprises the following steps:
litchi juice (cinnamon flavor) with a solid content of 20 degrees brix, and precooling to 20 ℃. The condensing circulation system 60 is opened for cooling, so that the temperature of the feeding tank 10 and the concentration processor 20 is consistent with the precooling temperature of the liquid material. Pumping 2.5L of pre-cooled Osmanthus-flavored fruit juice from a feed tank 10 into the inner cavity of a concentration processor 20; opening of CO2A Dewar flask 30 with bubble diameter of 107nm, after the pressure reaches 150bar, setting the rotating speed to be 1500rpm/min, simultaneously opening the stirring device 23 of the concentration processor 20,treating for 15 min; adjusting condensation circulation, setting the rotation speed to be 800rpm/min, reducing the temperature of the concentration processor 20 to be 0.5 ℃, and performing gas discharge treatment to ensure that the pressure in the concentration processor 20 is 20bar to perform phase change crystallization reaction; wherein, the phase transition stage and the crystal growth stage are judged according to the pressure and temperature change curves, the first time of detecting the pressure drop, the temperature rising point is the crystallization point, and the subsequent period of constant temperature is the phase transition stage; the temperature begins to continuously decrease, the pressure also continuously decreases until the pressure is not changed and is constant for a period of time, and the period is a crystallization period; and meanwhile, the temperature of the hydrate crystal tank 40 is increased to 50 ℃, the dissolved gas enters the concentrated solution tank 50, the stirring mechanism 51 of the concentrated solution tank 50 is opened, and after the treatment for 25min, the gas is circulated to the bubble generator 31 again and enters the next cycle for utilization. Finally, aseptically subpackaging and storing in a refrigeration house. The concentration rate of the obtained litchi juice concentrated solution reaches 55%, the retention rate of polyphenol content and Vc content reaches 94%, and the number of microorganisms is reduced by about 10% compared with the original extracting solution6The color is good, the time of concentrated sterilization is shortened by 29% compared with the method of concentrating a single hydrate and assisting non-thermal sterilization, and the sterilization rate is improved by 34% compared with the method of concentrating a single hydrate.
EXAMPLE six
The invention relates to a preparation method of litchi concentrated juice, which adopts the concentrated juice based on CO2The preparation method of the phase change balance regulating and controlling concentrated solution specifically comprises the following steps:
litchi juice (cinnamon flavor) with a solid content of 20 degrees brix, and precooling to 20 ℃. The condensing circulation system 60 is opened for cooling, so that the temperature of the feeding tank 10 and the concentration processor 20 is consistent with the precooling temperature of the liquid material. Pumping 2.5L of pre-cooled Osmanthus-flavored fruit juice from a feed tank 10 into the inner cavity of a concentration processor 20; opening of CO2A Dewar flask 30 with bubble diameter of 107Setting the rotating speed to be 1500rpm/min after the pressure reaches 150bar, and simultaneously opening a stirring device 23 of the concentration processor 20 for processing for 15 min; adjusting condensation circulation, setting the rotation speed to be 800rpm/min, reducing the temperature of the concentration processor 20 to be 10 ℃, and performing gas discharge treatment to ensure that the pressure in the concentration processor 20 is 90bar and phase change crystallization reaction occurs; in which the phase change stage and the crystalThe judgment of the growth stage of the body is that according to the pressure and temperature change curve, the pressure drop is detected for the first time, the temperature rising point is a crystallization point, and the subsequent period of constant temperature is a phase change stage; the temperature begins to continuously decrease, the pressure also continuously decreases until the pressure is not changed and is constant for a period of time, and the period is a crystallization period; and meanwhile, the temperature of the hydrate crystal tank 40 is increased to 50 ℃, the dissolved gas enters the concentrated solution tank 50, the stirring mechanism 51 of the concentrated solution tank 50 is opened, and after the treatment for 25min, the gas is circulated to the bubble generator 31 again and enters the next cycle for utilization. Finally, aseptically subpackaging and storing in a refrigeration house. The concentration rate of the obtained litchi juice concentrated solution reaches 55%, the retention rate of polyphenol content and Vc content reaches 94%, and the number of microorganisms is reduced by about 10% compared with the original extracting solution6The color is good, the time of concentrated sterilization is shortened by 29% compared with the method of concentrating a single hydrate and assisting non-thermal sterilization, and the sterilization rate is improved by 34% compared with the method of concentrating a single hydrate.
EXAMPLE seven
The preparation method of the grape seed polyphenol concentrated solution adopts the method based on CO2The preparation method of the phase change balance regulating and controlling concentrated solution specifically comprises the following steps:
and (3) precooling the grape seed polyphenol extract with solid content of 4 degrees brix to 15 ℃. The condensing circulation system 60 is opened for cooling, so that the temperature of the feeding tank 10 and the concentration processor 20 is consistent with the precooling temperature of the liquid material. Pumping 2L of pre-cooled grape seed polyphenol extracting solution from a feeding tank 10 into an inner cavity of a concentration processor 20; opening of CO2A Dewar flask 30 with bubble diameter of 102Setting the rotating speed to be 500rpm/min after the pressure reaches 70bar, and simultaneously opening a stirring device 23 of the concentration processor 20 for processing for 15 min; adjusting condensation circulation, reducing the temperature of the concentration processor 20 to 4 ℃, and performing gas discharge treatment to ensure that the pressure in the concentration processor 20 is 50bar and the rotating speed is adjusted to 1500rpm/min to perform phase change crystallization reaction; wherein, the phase transition stage and the crystal growth stage are judged according to the pressure and temperature change curves, the first time of detecting the pressure drop, the temperature rising point is the crystallization point, and the subsequent period of constant temperature is the phase transition stage; temperature start holdingContinuously reducing the pressure until the pressure is not changed and is constant for a period of time, wherein the period is a crystallization period; and meanwhile, the temperature of the hydrate crystal tank 40 is increased to 40 ℃, the dissolved gas enters the concentrated solution tank 50, the stirring mechanism 51 of the concentrated solution tank 50 is opened, and after the gas is treated for 8min, the gas is circulated to the bubble generator 31 again and enters the next cycle for utilization. Finally, aseptically subpackaging and storing in a refrigeration house. The obtained grape seed polyphenol concentrated solution has concentration rate of 40%, polyphenol antioxidant activity retention rate of 96%, and microorganism amount reduced by 10% compared with the original extractive solution4The color is good, the time of concentrated sterilization is shortened by 20% compared with the single hydrate concentrated concentration and concentrated sterilization assisted by non-thermal sterilization, and the sterilization rate is improved by 30% compared with the single hydrate concentrated sterilization.
Example eight
The preparation method of the apple juice concentrated solution adopts the method based on CO2The preparation method of the phase change balance regulating and controlling concentrated solution specifically comprises the following steps:
clear apple juice with solid content of 10 degrees brix, precooling to 18 ℃. The condensing circulation system 60 is opened for cooling, so that the temperature of the feeding tank 10 and the concentration processor 20 is consistent with the precooling temperature of the liquid material. Pumping 2L of the pre-cooled apple clear juice extracting solution from the feeding tank 10 into the inner cavity of the concentration processor 20; opening of CO2A Dewar flask 30 with bubble diameter of 103Setting the rotating speed to 900rpm/min after the pressure reaches 90bar, and simultaneously opening a stirring device 23 of the concentration processor 20 for processing for 15 min; adjusting condensation circulation, setting the rotation speed at 1300rpm/min, reducing the temperature of the concentration processor 20 to 6 ℃, and performing gas discharge treatment to ensure that the pressure in the concentration processor 20 is 45bar and phase change crystallization reaction occurs; wherein, the phase transition stage and the crystal growth stage are judged according to the pressure and temperature change curves, the first time of detecting the pressure drop, the temperature rising point is the crystallization point, and the subsequent period of constant temperature is the phase transition stage; the temperature begins to continuously decrease, the pressure also continuously decreases until the pressure is not changed and is constant for a period of time, and the period is a crystallization period; simultaneously, the temperature of the hydrate crystal tank 40 is increased to 50 ℃, the dissolved gas enters the concentrated solution tank 50, and the concentration is openedAfter the stirring mechanism 51 of the liquid tank 50 is treated for 20min, the gas is circulated to the bubble generator 31 again and enters the next cycle. Finally, aseptically subpackaging and storing in a refrigeration house. The obtained concentrated apple juice has concentration rate of 45%, polyphenol content and phenolic acid retention rate of 92%, and microorganism amount reduced by 10% compared with the original extractive solution5The color is good, the time of concentrated sterilization is shortened by 25% compared with the single hydrate concentrated concentration and concentrated sterilization assisted by non-thermal sterilization, and the sterilization rate is improved by 28% compared with the single hydrate concentrated sterilization.
Example nine
A method for preparing orange juice concentrate using the CO-based concentrate of the present invention2The preparation method of the phase change balance regulating and controlling concentrated solution specifically comprises the following steps:
orange juice with solid content of 10 degrees brix, precooled to 15 ℃. The condensing circulation system 60 is opened for cooling, so that the temperature of the feeding tank 10 and the concentration processor 20 is consistent with the precooling temperature of the liquid material. Pumping 2.5L of pre-cooled orange juice from the feed tank 10 into the inner cavity of the concentration processor 20; opening of CO2A Dewar flask 30 with bubble diameter of 103When the pressure reaches 90bar, simultaneously opening a stirring device 23 of the concentration processor 20, setting the rotating speed at 500rpm/min, and processing for 10 min; adjusting condensation circulation, reducing the temperature of the concentration processor 20 to 6 ℃, and performing gas discharge treatment to ensure that the pressure in the concentration processor 20 is 50bar and the rotating speed is adjusted to 1300rpm/min to perform phase change crystallization reaction; wherein, the phase transition stage and the crystal growth stage are judged according to the pressure and temperature change curves, the first time of detecting the pressure drop, the temperature rising point is the crystallization point, and the subsequent period of constant temperature is the phase transition stage; the temperature begins to continuously decrease, the pressure also continuously decreases until the pressure is not changed and is constant for a period of time, and the period is a crystallization period; and meanwhile, the temperature of the hydrate crystal tank 40 is increased to 45 ℃, the dissolved gas enters the concentrated solution tank 50, the stirring mechanism 51 of the concentrated solution tank 50 is opened, and after the gas is treated for 15min, the gas is circulated to the bubble generator 31 again and enters the next cycle for utilization. Finally, aseptically subpackaging and storing in a refrigeration house. The concentrated orange juice has concentration rate up to 45%, polyphenol and Vc retention rate up to 90%, and has low content of vitamin CThe amount of organism is reduced by about 10% compared with original juice6The flavor characteristic value is not changed, the original flavor and color are retained, and compared with single hydrate concentration and heat sterilization or non-heat sterilization before or after conventional concentration, the sterilization concentration processing time is shortened by 25%; compared with the concentration treatment of single hydrate, the sterilization rate is improved by 30 percent.
The above-mentioned embodiments only represent some embodiments of the present invention, and the description thereof is specific and detailed, but not to be construed as limiting the scope of the present invention. It should be noted that, for those skilled in the art, without departing from the spirit of the present invention, several variations and modifications can be made, which are within the scope of the present invention.
Claims (10)
1. Based on CO2Phase transition balance regulation and control's concentrate manufacturing installation which characterized in that:
the apparatus comprises a concentration processor (20), CO2The system comprises a Dewar flask (30), a hydrate crystal tank (40), a concentrated liquid tank (50), a condensation circulating system (60) and a heat circulating system (70), wherein the concentration processor (20) is used for enabling liquid materials to undergo a phase change crystallization reaction to generate concentrated liquid and hydrate crystals, and the CO is2The gas outlet of dewar bottle (30) is linked together through a bubble generator (31) in order to be linked together with the air inlet of concentrated treater (20), the feed inlet of hydrate crystal growing tank (40) with the hydrate export of concentrated treater (20) is linked together, the feed inlet of concentrated liquid jar (50) with the concentrate export of concentrated treater (20) is linked together, the air inlet of concentrated liquid jar (50) with the gas outlet of hydrate crystal growing tank (40) is linked together, the gas outlet of concentrated liquid jar (50) with the air inlet of bubble generator (31) is linked together, condensation circulation system (60) are used for doing concentrated treater (20) refrigeration, heat circulation system (70) are used for doing hydrate crystal growing tank (40) heats.
2. CO-based according to claim 12Phase transition balance regulation and control's concentrate manufacturing installation which characterized in that: the device also comprises a feeding tank(10) And a feeding pump (11) is arranged between the discharge hole of the feeding tank (10) and the feeding hole of the concentration processor (20).
3. CO-based according to claim 12Phase transition balance regulation and control's concentrate manufacturing installation which characterized in that: in the CO2A booster pump or a compressor is arranged between the air outlet of the Dewar flask (30) and the bubble generator (31).
4. CO-based according to claim 12Phase transition balance regulation and control's concentrate manufacturing installation which characterized in that: the concentration processor (20) comprises an outer shell (21), an inner shell (22) and a stirring device (23), wherein the inner shell (22) is arranged in the outer shell (21), a shell interlayer (24) is arranged between the inner shell (22) and the outer shell (21), the shell interlayer (24) is communicated with the condensation circulating system (60), the stirring device (23) is arranged in the inner shell (22), and the stirring device (23) is used for stirring liquid materials in the concentration processor (20).
5. CO-based according to claim 42Phase transition balance regulation and control's concentrate manufacturing installation which characterized in that:
a K-type thermocouple positioned in the shell interlayer (24) is arranged in the inner cavity of the shell (21);
a transparent observation window is also arranged on the inner shell (22);
a high-speed camera is also arranged in the inner cavity of the inner shell (22);
a pressure sensor is also arranged in the inner cavity of the inner shell (22);
a K-type thermocouple is also arranged in the inner cavity of the inner shell (22).
6. CO-based according to claim 12Phase transition balance regulation and control's concentrate manufacturing installation which characterized in that: the hydrate crystal tank (40) comprises an outer tank body (41), an inner tank body (42) and a stirrer (43), wherein the inner tank body (42) is arranged in the outer tank body (41)A tank interlayer (44) is arranged between the inner tank body (42) and the outer tank body (41), the tank interlayer (44) is communicated with the heat circulation system (70), the stirrer (43) is arranged in the inner tank body (42), and the stirrer (43) is used for stirring the hydrate crystals in the hydrate crystal tank (40).
7. CO-based according to claim 62Phase transition balance regulation and control's concentrate manufacturing installation which characterized in that: k-type thermocouples are arranged in the inner cavities of the tank body interlayer (44) and the inner tank body (42).
8. CO-based according to claim 12Phase transition balance regulation and control's concentrate manufacturing installation which characterized in that:
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.
9. CO-based according to claim 12Phase transition balance regulation and control's concentrate manufacturing installation which characterized in that: still include feed tank (10), feed tank (10) are used for the storage liquid material, the discharge gate of feed tank (10) with the feed inlet of concentrated treater (20) is linked together.
10. CO-based according to claim 12Phase transition balance regulation and control's concentrate manufacturing installation which characterized in that: still include storage tank (80), storage tank (80) are used for the storage to disinfect the concentrate after accomplishing, the feed inlet of storage tank (80) with the discharge gate of concentrate jar (50) is linked together.
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| CN114452672B (en) * | 2021-03-18 | 2023-06-16 | 广东省农业科学院蚕业与农产品加工研究所 | Based on CO 2 Concentrated solution manufacturing device and method for phase change balance regulation and control |
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