JP2002159836A - Continuous processing method and device for liquid substance - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a method and a device capable of correctly evaluating the effect of a continuous processing such as oxygen deactivation/disinfection of a liquid-like substance using a fluid operating to a microorganism or the like (operating fluid). SOLUTION: Carbon dioxide is dissolved in a carrier liquid by fine-bubbling and introducing a high pressure carbon dioxide gas (operating fluid) to the carrier liquid while the carrier liquid (physiological salt solution or the like) is continuously flowed to a dissolution tank 16 disposed on a line at a predetermined flow rate. After the carrier liquid in which carbon dioxide is dissolved is made to a desired processing temperature by a first heating device 18, a sample liquid including a microorganism or the like to be processed is introduced to the carrier liquid. Thereafter, the carrier liquid flows in a line while it maintains the processing temperature by a second heating device 20 and a pressure thereof is reduced when it passes through a pressure regulating valve 48. By this pressure reduction, carbon dioxide dissolved in the carrier liquid is gasified and is separated from the carrier liquid.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for continuously treating liquid substances (liquid foods, liquid chemicals, etc.) using a fluid having an inactivating effect on enzymes and spores and / or a killing effect on bacteria. In particular, the present invention relates to a method and an apparatus suitable for evaluating the effect of the continuous processing as described above. In addition,
In the present specification, bacteria, fungi, enzymes, spores, and the like are collectively referred to as “microorganisms,” and a fluid having the above-described action is referred to as “fluid acting on microorganisms or the like” or “working fluid.”

[0002]

2. Description of the Related Art FIG. 2 shows an example of a procedure for a continuous treatment of a liquid substance using a fluid acting on microorganisms or the like. In this process, first, a working substance is introduced into the raw material liquid at a predetermined flow rate in the middle of the line while a liquid substance (hereinafter, referred to as a raw material liquid) containing a microorganism or the like to be treated is continuously flown at a predetermined flow rate. Thus, the working fluid is mixed and dissolved in the raw material liquid (dissolution step). Next, the raw material liquid in which the working fluid is dissolved is heated to a predetermined processing temperature (heating step), and the temperature and pressure of the raw material liquid are maintained for a predetermined processing time. During this treatment time, the working fluid dissolved in the raw material liquid acts on microorganisms and the like in the liquid, the enzymes and spores are inactivated, and the bacteria are killed (inactivation / sterilization step). Thereafter, the working fluid is separated from the raw material liquid (separation step), and the processed raw material liquid is recovered as a product.

As the working fluid, a liquid in which a chemical acting on microorganisms or the like is dissolved can be used.
In recent years, attention has been paid to a technique using a supercritical fluid, a subcritical fluid, or a high-pressure gas as a working fluid. In particular,
Carbon dioxide in supercritical, subcritical or high-pressure gas state is the most important because of its high safety, low cost, easy separation from raw material liquid, and remarkable effect. Many are used. In addition, there is an example in which a substance (for example, nitrogen) other than carbon dioxide is used.

In the above treatment, the main factors affecting the treatment effect include the concentration of the working fluid in the raw material liquid, the temperature at which the working fluid is brought into contact with microorganisms (hereinafter referred to as the treatment temperature), and the time (hereinafter referred to as the treatment temperature). , Processing time). Conventionally, when evaluating the influence of these factors on the treatment effect, a raw material liquid containing a known amount of microorganisms is treated as described above while controlling predetermined conditions (concentration of working fluid, treatment temperature, treatment time). After that, the raw material liquid is collected, the number of microorganisms and the like remaining in the raw material liquid is measured, and the number is compared with the number of microorganisms and the like contained in the raw material liquid before the treatment. Was out.

[0005]

In the above process, the time from the introduction of the working fluid to the raw material liquid to the separation of the working fluid from the raw material liquid is a substantial working time of the working fluid. The action time is not constant when viewed at the individual level of microorganisms and the like, and if the line becomes long or the line configuration becomes complicated, it is unavoidable that the action time greatly varies. Therefore, in order to sufficiently increase the accuracy of evaluating the effect obtained by the above-described processing, it is necessary to eliminate the influence of the variation in the operation time by lengthening the processing time.

In the above treatment, there is a heating step between the dissolving step and the deactivation / sterilization step. In this heating step, the working fluid acts somewhat on microorganisms and the like. Therefore, for example, in an experiment aimed at evaluating the effect of the working fluid in the inactivation / sterilization process, factors such as the concentration of the working fluid in the raw material liquid and the processing temperature and time in the inactivation / sterilization process are controlled. Even if the processing is performed, a correct evaluation result cannot be obtained.

SUMMARY OF THE INVENTION The present invention has been made to solve the above-described problems, and an object of the present invention is to correctly evaluate the effects of treatments such as enzyme deactivation / sterilization of a liquid substance using a working fluid. It is an object of the present invention to provide a method for continuously processing a liquid substance that can be evaluated and a continuous processing apparatus for a liquid substance suitable for the evaluation.

[0008]

SUMMARY OF THE INVENTION In order to solve the above-mentioned problems, a method for continuously treating a liquid material according to the present invention is directed to a method for processing a liquid material using a supercritical fluid, a subcritical fluid, or a high-pressure gas as a working fluid. In the continuous processing method, a step of continuously flowing a carrier liquid at a predetermined flow rate into a line, and dissolving the working fluid in the carrier liquid by continuously introducing the working fluid at a predetermined flow rate into the carrier liquid flowing through the line. Dissolving step, a temperature adjusting step of adjusting the temperature of the carrier liquid in which the working fluid is dissolved to a predetermined processing temperature, a pressure adjusting step of adjusting the pressure of the carrier liquid in which the working fluid is dissolved to a predetermined processing pressure, the processing A sample introduction step of introducing a sample containing a microorganism or the like to be processed into the carrier liquid at the temperature and the processing pressure, wherein the carrier liquid into which the sample has been introduced is placed in the carrier liquid for a predetermined processing time; Characterized in that the temperature and pressure hold step to maintain the process temperature and process pressure, and a carrier liquid having passed through the temperature and pressure hold step comprises the step of separating the working fluid.

Further, the continuous processing apparatus for a liquid substance according to the present invention is a continuous processing apparatus for a liquid substance using a supercritical fluid, a subcritical fluid or a high-pressure gas as a working fluid. Means for supplying the working fluid to the carrier liquid at a predetermined flow rate in the middle of the line, a carrier liquid supply means for continuously flowing the working fluid at a predetermined flow rate, Temperature adjusting means for adjusting the pressure of the carrier liquid into which the working fluid has been introduced, a pressure adjusting means for adjusting the pressure of the carrier liquid to a predetermined processing pressure, and a sample containing a microorganism to be processed in the carrier liquid having the processing temperature and the processing pressure. A sample introduction unit to be introduced, a carrier liquid into which the sample has been introduced for a predetermined time, a temperature / pressure maintaining unit for maintaining the processing temperature and the processing pressure,
And separating means for separating the working fluid from the carrier liquid having passed through the temperature / pressure maintaining means.

[0010]

DESCRIPTION OF THE PREFERRED EMBODIMENTS In the method and apparatus according to the present invention,
First, a carrier liquid containing no microorganisms to be treated is continuously supplied to the line. As the carrier liquid, for example, physiological saline or a buffer can be used. When evaluation data on enzyme deactivation / sterilization treatment of microorganisms or the like contained in a specific liquid substance is required, the liquid substance obtained by sterilizing the liquid substance may flow as a carrier liquid into a line. Next, as described above, the working fluid (supercritical fluid, subcritical fluid, or high-pressure gas) is introduced into the carrier fluid flowing through the line, thereby dissolving the working fluid in the carrier fluid. In the dissolving step, for example, a dissolving tank having a liquid inlet and a liquid outlet is provided in the middle of the line, and while the carrier liquid is caused to flow through the dissolving tank, the working fluid is finely bubbled into the carrier liquid flowing in the tank. And then introduce it.

In the temperature adjusting step, the temperature of the carrier liquid in which the working fluid is dissolved is adjusted to a predetermined processing temperature by a temperature adjusting means comprising a heater, a temperature sensor and the like. Also,
In the pressure adjusting step, the pressure of the carrier liquid is adjusted to a predetermined processing pressure by pressure adjusting means constituted by a pump, a pressure adjusting valve, and the like. The order of the temperature adjustment step and the pressure adjustment step is not essential to the present invention, and both steps may be performed simultaneously.

In the sample introducing step, a sample containing a microorganism to be treated is introduced into the carrier liquid whose temperature and pressure have been adjusted as described above. The sample introducing means includes, for example, a first pipe through which the carrier liquid whose temperature and pressure are adjusted as described above, a sample inlet provided in the pipe, a sample outlet of a container containing a sample, and the sample inlet. It is configured to include a second pipe connecting the port and a pump disposed on the way of the second pipe.

In the temperature / pressure maintaining step, the carrier liquid into which the sample has been introduced as described above is maintained at the processing temperature and the processing pressure for a predetermined processing time. The temperature / pressure maintaining means is, for example, for heating a processing unit (including a carrier liquid flow path therein) disposed on the way of the first pipe downstream of the sample introduction port, and a processing tank thereof. , A temperature sensor for monitoring the temperature of the carrier liquid flowing through the flow path of the processing tank, a pump and a pressure control valve for adjusting the pressure in the flow path of the processing tank, and the like. If a step that affects the pressure of the carrier liquid is not included between the pressure adjusting step and the present step, the pressure adjusting unit described above is operated to operate the carrier liquid in the present step. Is automatically maintained at the processing pressure. In this case, it is not necessary to provide a pressure adjusting mechanism for the temperature / pressure maintaining step.

In the separation step, the working fluid is separated from the carrier liquid that has undergone the temperature / pressure maintaining step. For example, when the working fluid is carbon dioxide in a supercritical state, a subcritical state, or a high-pressure gas state, when the carrier liquid in which the carbon dioxide is dissolved is decompressed, the carbon dioxide is vaporized, while the carrier liquid maintains a liquid state. Therefore, carbon dioxide can be easily separated from the carrier liquid.

[0015]

FIG. 1 shows a schematic configuration of a continuous processing apparatus according to an embodiment of the present invention. The apparatus 1 includes a cylinder 10 in which liquid carbon dioxide is sealed, a carrier liquid tank 12 in which a carrier liquid is stored, a sample tank 14 in which a sample liquid containing microorganisms to be treated is stored, and dissolving carbon dioxide in the carrier liquid. Dissolving tank 16, a first heater 18 for adjusting the temperature of the carrier liquid in which carbon dioxide is dissolved to a predetermined processing temperature, and maintaining the temperature of the carrier liquid at the processing temperature for a predetermined time. And a second heater 20 for heating.

The liquid outlet of the cylinder 10 is connected to a carbon dioxide inlet 1 provided at the bottom of the dissolving tank 16 by a carbon dioxide supply pipe 21 provided with a pump 22 and a vaporizer 24.
61 is connected. The carbon dioxide inlet 161 penetrates the bottom wall of the dissolving tank 16 from outside to inside, and a micro filter 26 is attached to an upper end thereof. The liquid outlet of the carrier liquid tank 12 is provided with a pump 28 and an electromagnetic valve 30.
The dissolution tank 16 is provided by a carrier liquid supply pipe 32 provided with
Is connected to a carrier liquid inlet 162 provided at a lower portion of the side wall of the liquid crystal display. A liquid outlet 16 is provided above the side wall of the dissolving tank 16.
3 are provided. The liquid outlet 163 is connected to a liquid inlet 181 of the first heater 18 by a pipe 34. The tube 34 is provided with a temperature sensor 36 for measuring the temperature of the liquid flowing therein.

The first heater 18 has a liquid inlet 1 therein.
A spiral flow path 183 from 81 to the liquid outlet 182 is formed. The liquid outlet 182 is connected to the liquid inlet 201 of the second warmer 20 by a pipe 38 provided with the sample inlet 37.
Is connected to The tube 38 is provided with a temperature sensor 42 for measuring the temperature of the liquid flowing therein. The sample inlet 37 is connected to a liquid outlet of the sample tank 14 by a sample supply pipe 46 provided with a pump 44. The second heater 20 has a spiral flow path 203 extending from the liquid inlet 201 to the liquid outlet 202, and a pipe 203.
A temperature sensor 40 for measuring the temperature of the liquid flowing in the vicinity of the liquid outlet 202 is incorporated. The liquid outlet 202 of the second heater 20 is connected to the separation tank 51 by a pipe 50 provided with the pressure control valve 48.

In the dissolving tank 16, a gas outlet 164 is provided at the top of the dissolving tank 16. One end of a carbon dioxide recovery pipe 58 in which two pressure regulating valves 52 and 54 and a carbon dioxide recovery tank 56 are disposed is connected to the gas outlet 164. Further, a liquid outlet 165 is provided at a lower portion of the side wall of the dissolving tank 16, and a drain pipe 62 having an electromagnetic valve 60 is connected to the liquid outlet 165.

The apparatus 1 includes a control device 6 for controlling the operation of a pump, a solenoid valve, a pressure control valve, a heater, and the like in accordance with an operation signal from the operation section 64 and an output signal of each temperature sensor.
6 are provided.

An evaluation experiment using the apparatus 1 configured as described above is performed as follows.

First, after a user puts a sample liquid containing a microorganism to be processed into the sample tank 14, a processing temperature and a processing pressure are set through the operation unit 64 according to the purpose of the experiment. Instructs the start of processing. Upon receiving this instruction, the control device 66 closes the electromagnetic valve 60 of the drain pipe 62, opens the electromagnetic valve 30 in the middle of the carrier liquid supply pipe 32, and starts the pump 28. When the pump 28 is started,
The carrier liquid stored in the carrier liquid tank 12 flows into the dissolution tank 16 through the carrier liquid supply pipe 32. The carrier liquid flowing into the dissolution tank 16 flows upward in the tank 16 and flows into the pipe 34 from the liquid outlet 163.
The carrier liquid that has flowed into the pipe 34 is heated to the processing temperature in the first warmer 18, and is heated by the pipe 38 and the second warmer 2.
0 and flows into the separation tank 51 through the pipe 50.

In response to the instruction from the user, the control device 66 starts the pump 22 of the carbon dioxide supply pipe 21. Then, the liquid carbon dioxide sealed in the cylinder 10 flows into the carbon dioxide supply pipe 21. The liquid carbon dioxide is vaporized when passing through the vaporizer 24 and becomes a high-pressure gas, and the high-pressure gas becomes fine bubbles when passing through the microfilter 26. The fine bubbles rise in the dissolving tank 16 together with the carrier liquid, during which time the carbon dioxide in the fine bubbles dissolves in the carrier liquid. Depending on the conditions, some carbon dioxide remains in the form of fine bubbles.
4 and collected in a carbon dioxide recovery tank 56 for reuse.

When a sufficient time has elapsed in the above state, the carrier liquid in which the carbon dioxide is dissolved is supplied at a stable flow rate through the pipe 34, the first heater 18, the pipe 38, and the second heater 20.
And flow through the tube 50. Here, the pressure of the carrier liquid flowing through the pipe 50 rapidly decreases when passing through the pressure control valve 48. As a result of this reduced pressure, carbon dioxide dissolved in the carrier liquid evaporates. The gasified carbon dioxide is naturally separated from the carrier liquid in the separation tank 51.

After the above-mentioned stable state is established, the controller 66 starts the pump 44 of the sample supply pipe 46. Then, the sample liquid stored in the sample tank 14 is
6 through the sample inlet 37 and into the tube 38. At this time, the control device 66 controls the temperature sensor 40
And two heaters 18 so that the temperature of the carrier liquid determined from the output signals of and is maintained at the processing temperature.
20 is controlled.

In the above treatment, the time during which carbon dioxide dissolved in the carrier liquid acts on microorganisms and the like is from the time when the sample liquid is introduced into the carrier liquid to the time when the carrier liquid is depressurized. This time depends on the flow rate of the carrier liquid, the flow rate of the carbon dioxide, the flow rate of the sample liquid, and the sample inlet 37.
From the pressure control valve 48 to the pressure control valve 48. Then, by sequentially using a plurality of heaters 20 having different internal spiral flow paths as the second heater 20, an evaluation experiment using the operation time as a control parameter can be performed. As for the processing pressure, the pressure in the line can be set to a desired pressure by appropriately setting the output of the pump and the opening of the pressure control valve. Regarding the processing temperature, two heaters 18,
By using 20, the temperature of the carrier liquid during the working time can be maintained at a desired temperature.

[0026]

According to the present invention, the time required for carbon dioxide dissolved in the carrier liquid to act on microorganisms and the like is much longer than the time required when a raw material liquid containing microorganisms and the like is used from the beginning as in the prior art. Short. Further, according to the present invention, the carrier liquid flows without stagnation in a section where carbon dioxide acts on microorganisms and the like. From the above, according to the method of the present invention, the variation in the action time at the individual level such as microorganisms is much smaller than in the conventional method, and the experiment can be performed with high accuracy even in a short time. .

According to the present invention, the sample containing the microorganisms to be treated is introduced into the carrier liquid after the heating step. Therefore, for example, in an experiment aimed at evaluating the effect of the working fluid in the inactivation / sterilization process, factors such as the concentration of the working fluid in the raw material liquid and the processing temperature and time in the inactivation / sterilization process are controlled. By performing the treatment while doing so, it is possible to correctly evaluate the influence of these factors on the effect.

[Brief description of the drawings]

FIG. 1 is a schematic configuration diagram of a continuous processing apparatus according to an embodiment of the present invention.

FIG. 2 shows an example of continuous treatment of a liquid substance using a fluid acting on microorganisms and the like.

[Explanation of symbols]

 DESCRIPTION OF SYMBOLS 1 ... Continuous processing apparatus 10 ... Cylinder 12 ... Carrier liquid tank 14 ... Sample tank 16 ... Dissolution tank 18, 20 ... Heater 24 ... Vaporizer 26 ... Microfilter 51 ... Separation tank 66 ... Control device

Continued on the front page (51) Int.Cl. ⁷ Identification symbol FI Theme coat II (reference) A61L 2/24 A61L 2/24 // A23L 3/015 A23L 3/015 F term (reference) 4B021 LA42 LP07 LW06 LW10 4C058 AA12 AA30 BB07 JJ06 JJ12 JJ28 JJ29

Claims (2)

[Claims] 1. A method for continuously treating a liquid material using a supercritical fluid, a subcritical fluid, or a high-pressure gas as a working fluid, wherein a carrier liquid is continuously supplied to a line at a predetermined flow rate. A dissolving step of dissolving the working fluid in the carrier liquid by continuously introducing the working fluid at a predetermined flow rate; a temperature adjusting step of adjusting the temperature of the carrier liquid in which the working fluid is dissolved to a predetermined processing temperature; A pressure adjusting step of adjusting the pressure of the carrier liquid in which the working fluid is dissolved to a predetermined processing pressure; a sample introducing step of introducing a sample containing a microorganism to be processed into the carrier liquid having the processing temperature and the processing pressure; The carrier liquid into which the sample has been introduced is subjected to a predetermined processing time,
A method for continuously processing a liquid material, comprising: a temperature / pressure maintaining step of maintaining the processing temperature and the processing pressure; and a step of separating the working fluid from the carrier liquid having passed through the temperature / pressure maintaining step. 2. A continuous processing apparatus for a liquid substance using a supercritical fluid, a subcritical fluid or a high pressure gas as a working fluid. Fluid introduction means for continuously introducing the working fluid into the carrier liquid at a predetermined flow rate, temperature adjusting means for adjusting the temperature of the carrier liquid into which the working fluid has been introduced to a predetermined processing temperature, and introducing the working fluid. Pressure adjusting means for adjusting the pressure of the obtained carrier liquid to a predetermined processing pressure; sample introducing means for introducing a sample containing a microorganism to be processed into the carrier liquid having the processing temperature and the processing pressure; A temperature / pressure maintaining means for maintaining the liquid at the processing temperature and the processing pressure for a predetermined time, and the operation from the carrier liquid passing through the temperature / pressure maintaining means. An apparatus for continuously treating a liquid substance, comprising a separation means for separating a fluid.