EP2136654A1

EP2136654A1 - Method and device for sterilising a liquid

Info

Publication number: EP2136654A1
Application number: EP08737309A
Authority: EP
Inventors: Aleksandr Zavadtsev; Pavel Pavlovitch Koulik
Original assignee: Opus Industry SA
Current assignee: Opus Industry SA
Priority date: 2007-03-21
Filing date: 2008-03-17
Publication date: 2009-12-30
Also published as: US20100297313A1; WO2008114116A1; CN101674736B; WO2008114116A8; CN101674736A

Abstract

The invention relates to a sterilisation method that comprises heating the liquid with electric field pulses having a frequency higher that 1 MHz at a rate higher than 280° C per second to a processing temperature T between 200 and 66° C, and depending on the value of the processing temperature T, exposing the liquid to a pulsed alternating electric field immediately or shortly after heating the liquid.

Description

METHOD AND DEVICE FOR STERILIZING A

LIQUID

The present invention relates to a method for sterilizing or pasteurizing a liquid, in particular a water-based liquid or water-containing liquid, and / or solid bodies or objects in contact with this liquid, as well as a device for implementing this method. By "sterilization" is meant the destruction or neutralization of microorganisms, such as yeasts, molds, bacteria and viruses, selectively or broadly, that is, just targeting one or more types of microorganisms, or essentially all types of microorganisms contained in the liquid or on the surfaces of solid bodies or objects in contact with the liquid. In the present application, the concept of sterilization also includes what is conventionally called pasteurization.

In particular, the term sterilization is used in the present invention to qualify a method of destruction or selective or non-selective neutralization of microorganisms preferably below a threshold of 100 microorganisms / ml remaining in the liquid to be sterilized. The invention is applicable mainly, but not exclusively, to the food, pharmaceutical and medical, biophysical and biochemical fields, and sanitary water networks. Liquids to be sterilized may include, for example, contaminated water, wastewater, sewage, standing water, blood and blood components, pharmaceutical preparations, beverages or food products such as beer, mineral water, flavored water, milk and milk products, tea and others. A commonly used sterilization process is heat treatment (pasteurization) for a period of time at a temperature sufficient to destroy microorganisms. Conventional sterilization (pasteurisation) temperatures are between 90 and 120 ^° C. These processes have the disadvantage to alter the properties of sterilized liquids, for example by destroying vitamins. On the other hand, high temperatures do not permit the use of such methods for sterilizing liquids in plastic containers, such as PET bottles. Patent WO 02/34075 A1 discloses a method of sterilizing a liquid and / or a solid object in contact with this liquid by simultaneous heating with the action of an electric field and acoustic vibrations. According to this document, this process would make it possible to carry out the sterilization of a liquid, as well as the previously closed container containing it, at a critical temperature T _c lower than the thermal sterilization temperature (pasteurization) T _t .

However, in practice, this method does not substantially reduce the critical temperature T _c . because the warming of the liquid is actually not effective. The heating is done by applying an electric field, the amplitude being at the level of 1000 V / cm and the frequency of the electric field being in the frequency range of 10 ⁷ Hz or 10 ⁹ Hz. However, the structure of the microorganisms is not sensitive to such an electrical field of too low amplitude and too high frequency. By applying the conditions described in WO 02/34075 A1, it seems that it is not possible to reduce the sterilization temperature (pasteurization) below 70 ^° C. Other documents of the state of the art, namely, U.S. Patents 4,695,472, US 5,048,404, and A Continuous Treatment System for Inactivating Microorganisms with Pulsed Electric Fields, disclose pasteurization of food products at relatively low temperatures. In US 4,695,472 sterilization of liquid foods at treatment temperatures of at least 45 ° C is described. The liquid is heated and subjected to one or more electric field pulses of amplitude of between 5,000 and 12,000 V / cm for currents of at least 12 A / cm ² and duration of between 5 and 100 microseconds. Under these conditions, it is a question of a process of retarding the growth of microorganisms typically of about ten days, and not a method of destruction of microorganisms, that is to say sterilization of the product. Moreover, the creation of pulses of electric field is accompanied an electric current which causes additional heating of the product, the power density reaching, in the examples cited, values up to 6 W / cm ³ . A disadvantage of this method is that the heating efficiency is reduced due to the creation of preferential passages of the current ("pinch" effect), this accompanied by a risk of excessive local heating and even breakdown, which can lead to an alteration of the physicochemical properties of the liquid to be treated.

The method described in US Pat. No. 4,695,472 does not allow the sterilization of liquids enclosed in standard size containers in the food industry, not only because of the problems mentioned above, but also because the amplitude of the field proposed electric, applied on a bottle of about ten centimeters in diameter, would require very high voltages, difficult to generate and apply homogeneously.

The irreversible electroporation process can be considered as a method which in principle allows the sterilization of aqueous liquids at low temperature (for example at 20 ^° C.) by subjecting the liquid to repeated electric field pulses of 10-20 KV / cm. In the case of sterilization of beverage containers of 0.5-1.5 liter, this would mean that one should provide voltages exceeding 10-20-10 ⁶ V, which is not feasible under industrial conditions. In view of the above, an object of the invention is to provide a process for sterilization or pasteurization of a liquid, effective and reliable, which does not alter, or little alter, the properties of the liquid. Another aim is also to provide a device for the implementation of such a method.

It is advantageous to provide a method for sterilizing a liquid that does not heat the liquid, even locally, above 70 ^° C, but preferably not above 65 ° C.

It is advantageous to provide an economical and simple sterilization process to control and implement.

It is advantageous to provide a high performance method for the efficient and reliable sterilization of a hermetically sealed liquid in containers, especially containers of common sizes in the food industry, including plastic or other materials which do not withstand high temperatures.

Objects of the invention are realized by a sterilization method according to claim 1, and a device for carrying out a sterilization process according to claim 11.

The sterilization process according to the present invention comprises heating the liquid by electric field waves having a frequency greater than 1 MHz, at a speed greater than 28 ^° C. per second, up to a treatment temperature T lying between 20 ^° C. and 66 ° C, and depending on the value of the treatment temperature T, the exposure of the liquid to an alternating electric field in pulses immediately or shortly after heating of the liquid, the amplitude E of the electric field in V / cm being selected from so that the equation:

C (T) <log (E + 1) <B (T) is satisfied for the values: B (T) = -2,340. 10 ⁵ T ³ + 1, 290. 10 ³ T ² - ^3, 110. 10 ² T + 5.0

C (T) = -4.503. 10 ⁵ T ³ + 2.888. 10 ³ T ² - 5,900. 10- ² T + 4.0 where T is the treatment temperature in degrees Celsius.

Surprisingly, the inventors have found that by heating the liquid very rapidly, at a speed greater than 28 ° C per second, the electric field to be applied to destroy the microorganisms can be greatly reduced. Thus, at processing temperature values of 64 to 66 ° C, the magnitude of the electric field can even be zero. In other words, the effective and reliable pasteurization of the liquid requires no exposure to the electric field for a treatment temperature above 64 ° C, and for lower temperatures, exposure to a field of much lower amplitude to what is conventionally proposed.

Because of the importance of the heating rate on the pasteurization efficiency, uniform heating in volume is important to ensure that the entire volume of the liquid is subjected to rapid heating. For this purpose, the liquid is preferably agitated or turbulized and the heating in volume is performed by high frequency waves or microwaves. Heating by HF waves or microwaves makes it possible to obtain a heating by stirring of the water molecules by minimizing ohmic heating by electric current, to avoid problems of "pinch" effect inducing non-uniformities of heating. . The frequencies of these radiations are preferably more than 1000 kHz.

To treat hermetically sealed containers, it is advantageous to use alternating electric fields at a frequency greater than 10OkHz ₁ but less than 100OkHz. As the lipid membrane of the microorganism has some inertia, it does not react to electroporation beyond about 100OkHz. In practice, the application of an electric field of frequency less than 100 kHz will be accompanied by an electric current that heats the aqueous solution, creating, at the limit, local areas of breakdown, which is undesirable.

To avoid overheating and breakdown zones, the electric field is pulsed. Preferably, one adjusts the amplitude of the electric field as well as the duration of an electric field pulse to avoid the appearance of breakdown in the liquid to be sterilized. For the case of a plurality of electric field pulses, the total duration of the electric field pulses and their frequency are preferably chosen so as to avoid a heating of more than a few degrees of the liquid to be treated.

According to the invention, the total heat energy supplied to the aqueous solution by the electric field pulses is preferably less than 0.05 J / cm ³ and the frequency of repetition of the alternating electric field pulses on each portion of the liquid to The process is preferably between 10 and 100 Hz. It is useful to pause between the heating step and the step of applying the electric field pulse (s). This pause is useful to better standardize the temperature field in the liquid to be sterilized so that all areas of the liquid, including those of the boundary layers at liquid-solid interfaces of the container, acquire essentially the same temperature before application of the electric field. The parameters of the thermal pulse and of the electric field according to the present invention depend on the thermodynamics of the evolution of the molecular states of the membrane surrounding the microorganism and responsible for its vitality, when this membrane is immersed in a liquid containing the water. The qualitative understanding of the role of temperature and electric field in the evolution of molecular states in the membrane surrounding microorganisms and responsible for its vitality is based on the study of the behavior of structures of lipid molecules in contact with clusters of water when the membrane is immersed in an aqueous solution and subjected to an electric field. In general, the membrane is subjected to the formation of pores ("poration"). These pores form and fill up sporadically. When the electric field is zero, the increase in temperature causes irregularities in the structure of lipid molecules of the cell membrane of microorganisms due to the change in shape of the "tails" of lipid molecules. If a pore is formed, these changes in shape cause phase transformations that stimulate the increase in size (and possibly also the number) of pores until the loss of stability, the tearing of the membrane. Normally, these transitions can take place from and above a temperature close to 70 ⁰ C. This phase transition causes the increase of the pore diameter, the tearing of the membrane and the "death" of the microorganism . But if the temperature increases slowly, the phase transition is delayed, the membrane withstands this increase in temperature, adapts its molecular morphology in a metastable state, and only at higher temperatures (about 100 ⁰ C), the phase transition takes place, accompanied by the tearing of the membrane and thus the "death" of the micro-organism. The values of 70 ^° C. and 100 ^° C. are only average values. These values depend on the nature of the microorganism. Depending on the nature of the microorganism concerned, these values may vary between 65 and 75 ^° C. and between 95 and 135 ° C. respectively. The slow increase in temperature corresponds to the classic thermal destruction (sterilization). For speeds of increase of the temperature of the order of 1 ° C per second or less according to current practice, we will have a conventional metastable sterilization.

On the other hand, for rates of increase of the temperature of more than 28 ° C. per second, preferably greater than 30 ^° C. per second, any adaptation of the molecular morphology of the microorganisms in a metastable state is avoided.

The thermal stresses on the membranes of the micro-organisms due to the very fast increase of the temperature of the liquid are added to the stresses due to the effects of the alternating electric field, whose frequency is chosen to oscillate the effects of stress on the membranes. and therefore amplify the maximum local stresses that these membranes undergo. This combination makes it possible to better focus the energy of the electric field on the destruction of microorganisms by electroporation, minimizing the loss of electrical energy in heat and therefore the electrical power necessary for the irreversible destruction of the microorganisms. This makes it possible to treat larger volumes and more easily to avoid problems of breakdown and local heating that can alter the properties of the liquid to be sterilized.

An important advantage of the present invention is therefore to be able to perform, at temperatures below 66 ° C and with an electric field of small amplitude compared to conventional methods, irreversible collective electroporation operations on cells in large quantities. in an aqueous solution, in particular being inside a hermetically sealed container.

This makes it possible to pasteurize a liquid at a temperature at which plastic containers do not deform and the physicochemical properties of the liquid are not modified / degraded.

The sterilization process according to the invention can advantageously be done selectively, because for each kind of microorganism it is possible to choose the parameters (amplitude, oscillation frequency, pulse frequency, duration of the pulses) which are specific for the destruction of said microorganism. This makes it possible to better target the destruction of harmful micro-organisms, and, if necessary, not to destroy a certain quantity of useful micro-organisms.

The sterilization process according to the invention can advantageously be applied to continuous streams, pulsating streams, containers filled with liquid to be sterilized, or containers filled with liquid and being in an aqueous solution, which also makes it possible to sterilize the internal and external surfaces of the containers.

The present invention can be applied to any solid body of a dielectric material, in particular a polymeric material. The solid bodies may be in the form of hermetically sealed containers and containing an aqueous solution therein, in particular they may be in the form of plastic containers such as PET bottles or soft plastic bags, or even glass bottles. .

The practical conclusion of this analysis is that a first step to reduce the treatment temperature is to effect warming of the liquid containing the microorganisms rapidly, preferably more than

30 ^° C. per second and more advantageously from 30 ° to 40 ^° C. per second.

This makes it possible to obtain the tear of the microorganism membrane at temperatures lower than the conventional pasteurization temperatures and with much lower electric fields than the fields proposed in the state of the art, see zero for a temperature. treatment beyond

64 ° C.

The interaction of a low-frequency electric field, in particular between 100 kHz and 1000 kHz, with the dipoles of the "tails" of the lipid molecules concentrated on the surface of the pore, causes the shift of the threshold of the transition temperature of phase towards low temperatures. The greater the amplitude of the electric field, the lower the threshold moves. This means that the lethal temperature threshold for microorganisms can be decreased to and from room temperature. The electric field amplitude necessary to kill a microorganism (by electroporation) at ambient temperature (20 ^° C.) is of the order of 10 ⁴ to 2 × 10 ⁴ V / cm. It is important to emphasize that it is question of the amplitude of the local electric field, that is to say in the liquid to be treated or the interface liquid-membrane.

The device for carrying out the sterilization process comprises a heating station with a liquid heating system, an electric field generating station with a pulsed electric field generation system, and a liquid transport device. process comprising a conduit capable of carrying a liquid passing through the heating and electric field application stations, the heating system being configured to heat the liquid passing through the heating station at a rate greater than 28 ° C per second. The pulsed electric field generation system is configured to generate an alternating electric field with an oscillation frequency between 10OkHz and 1000kHz.

The device preferably comprises a cooling station downstream of the electric field generation station traversed by the transport device in order to rapidly cool the liquid to be treated.

According to one variant, the electric field pulse generation system comprises electrodes disposed on either side of a passage section of the conduit and capable of generating an electric field transverse to this section.

According to another variant, the electric field pulse generation system comprises an inductor with one or more primary windings toroidally arranged around a passage section of the conduit and capable of generating a substantially longitudinal electric field to this section.

The device may further include an electric field sensor in the area of application of the electric field and temperature sensors along the transport device, upstream, downstream and in the heating station.

The transport device may comprise a pump system and a transport liquid for conveying containers containing the liquid to be treated along the conduit, and a return circuit for returning the transport liquid from an outlet to an inlet of the device. transport. The conduit of the device may have portions with different passage sections for varying the flow velocity of the liquid.

It is advantageous to use the device for the decontamination of blood or a liquid component of blood contained in hermetically sealed flexible containers or for the sterilization of drinks or liquid food products contained in hermetically sealed containers such as glass bottles or in plastic.

Other objects and advantageous features of the invention will emerge from the claims and the detailed description given below, by way of illustration, with reference to the accompanying drawings, in which:

FIG. 1 shows a graph illustrating the relationship between the treatment temperature and the amplitude of the electric field according to the invention;

Figure 2 shows a graph illustrating electric field pulses according to the invention; Figure 3 shows a device for carrying out a sterilization process according to one embodiment of the present invention;

Figure 4a shows an electric field distributor device according to a first embodiment; and

4b shows an electric field distributor device according to a second embodiment.

The sterilization method according to the present invention comprises heating the liquid to be treated by an electric field having a frequency greater than 1MHz, at above 28 ° C per second speed until a treatment temperature T between 20 ⁰ C and 66 ^° C. According to the value of the treatment temperature T, the liquid is exposed to an alternating electric field in pulses immediately or shortly after heating of the liquid, the amplitude E of the electric field in V / cm being chosen so that the empirical equation:

C (T) <log (E + 1) <B (T) be satisfied for the values: B (T) = -2.340. 10 ^'5 T ³ + 1, 290. 10 ^"3 T ² - 3.1 10 ² T + 5.0 C (T) = -4.503, 10 ^" T ³ + 2.888. 10 ^"3 T ² - 5,900 10 ^{" 2} T + 4.0 where T is the treatment temperature in degrees Celsius.

This relationship is illustrated by the graph of FIG. 1. B (T) represents the upper limit of the electric field amplitude reasonably required under industrial pasteurization conditions of water-based products according to the present invention.

C (T) represents the lower limit of the magnitude of the electric field below which there is no destruction of all typical microorganisms representing a hazard to the quality and preservation of the product or to health consumer or individual (hatched area in Figure 1).

A (T) represents the lower limit of the electric field magnitude below which pasteurization of a water-based product containing the typical microorganisms representing a hazard does not take place according to the present invention. for the quality and preservation of the product or for the health of the consumer or the individual.

For example, the value of the electric field necessary for pasteurizing a liquid according to A (T) is:

E ≈ 0 V / cm, when T = 65 ⁰ CE ≈ 10 ² V / cm, when T = 60 ⁰ C

E ≈ 10 ³ V / cm, when T = 50 ° C

E ≈ 5.10 ³ V / cm, when T = 40 ⁰ C

E "10 ⁴ V / cm, when T = 30 ⁰ C

E ≈ 5.10 ⁴ V / cm, when T = 20 ⁰ C

It will be noted that this relation gives only a first estimate, which can be specified empirically according to the microorganisms (cells) to be destroyed and the properties of the liquid. The appearance of the alternating electric field pulse is illustrated in Figure 2 where are indicated the times ti, t ₂ and ta.

The oscillation of the electric field is preferably substantially sinusoidal, but may be of another form. The characteristics and shape of the alternating electric field pulses are configured to maximize the electroporation of the microorganism membranes and reduce the generation of electric current lost to heat. For this purpose, the period ti of an oscillation of the electric field preferably has a value ti> 1 μs (10; ⁶ seconds)

Below this time, microorganisms are insensitive to oscillations of the electric field.

For a constant electric field amplitude, the greater is ti, the more intense are the current losses due to ohmic heating accompanying the passage of the oscillating electric current through the heated medium, given the finite electrical resistivity of the medium. In the case of heating plastic containers filled with beverage by high frequency currents, in order to minimize these losses, it is very advantageous to limit the frequency to 100 kHz, ie 1 1 to 10 μs, preferably 5 μs. We therefore have for the limiting condition:

1μs <ti <10μs.

The duration t ₂ of an oscillating electric field pulse is greater than the period t i of an oscillation of the electric field: t ₂ > t i. The higher value of t ₂ is determined by the total warming of thermal disturbance zones due to the fact that the electrical resistance of electrolytes - beverages are a special case - decreases with increasing temperature. The electric current, in this case, will always focus in more or less cylindrical areas oriented along the electric field vector. These areas then contract rapidly, stimulated by pinch effects. The temperature in these zones increases exponentially, which leads to unacceptable local heating or even breakdowns.

These constraints lead us to the limiting relation for t ₂ :

X ₂ <c. dT. R / E where c, dT, R, E are, respectively, the specific heat, the temperature difference, the resistivity of the medium, and the amplitude of the electric field.

Taking into account the experimental fact that the electrical resistivity of an aqueous medium such as a drink does not exceed 10 Ohm. m and that c = 4 megajoules / m ³ .degree, for dT <5 degrees Celsius and E = 1000 kV / m, we have:

t ₂ <20 μs.

The duration t ₃ is the lapse of time between two pulses of electric field. It is preferably greater than the compensation time of the ohmic heating disturbances by the hydrodynamic turbulence pulsations. If v is the characteristic velocity of the hydrodynamic instabilities and L is their amplitude, the compensation condition is: t ₃ > L / v

In the case of pasteurization of filled and sealed bottles, according to the present invention, there is L> 0.003 m and v <1m / s, hence t ₃ > 0.001 s. The upper limit for t ₃ is given by the condition of having at least one pulse per treated container. In this case t ₃ <LL / vv where LL is the characteristic dimension of the container in the direction of its movement through the electric field, and w, its speed.

For the typical case of pasteurisation of bottles of 0.5 I ₁ LL = 0,3m and vv> 1 m / s, we have: t ₃ <0.3 s.

If we treat a liquid flow, t ₃ <LLL / vvv where LLL is the length of the area of application of the electric field and vvv, the speed of this flow through this area. For the typical case where LLL = 0.3m and vvv> 1m / s, we have: t ₃ <0.3 s.

In the sterilization process according to the invention, the liquid may be heated simultaneously with the pulse or the electric field pulses. In practice, it is more advantageous to first subject the liquid to the heating pulse, and then to apply the pulse or the electric field pulses. This pause is useful to better standardize the temperature field in the liquid to be sterilized so that all areas of the liquid, including those of the boundary layers at liquid-solid interfaces of the container, acquire essentially the same temperature before application of the electric field.

If x is the characteristic thickness of the boundary layer (at most 0.3 mm), the pause time t _p is preferably greater than: tp = (dcx ² ) / z where d, c and z are respectively the density , the thermal capacity and the thermal conductivity of the liquid to be sterilized. For most applications, the duration of this pause does not exceed 1 or 2 seconds.

For certain applications it is advantageous to space the zone of action of the thermal pulse from that of the electric field pulse. For example, one can insert a transit zone between the two, where the electric field is zero or negligible and where the temperature field is standardized in the volume of the liquid so that the temperature difference between the central and peripheral parts. liquid does not exceed one degree. The liquid to be treated passes through this transit zone during the pause mentioned above between the heating of the liquid and the application of the electric field.

Figure 3 illustrates a diagram of the device for implementing the method according to the present invention.

The device 1 comprises a transport system 2 of the liquid to be treated 3, a volume heating station 4 of the liquid to be treated and a station for applying a pulsed electric field 5. The transport system 2 comprises an input station 6, a transport duct 7, and an outlet station 8. The containers can be brought by a standard conveyor 33 and deposited on a bucket chain (or any other equivalent mechanism) in a column portion 7a of the conduit 7. The transport system may further comprise a pumping system 9a, 9b, for the circulation of the liquid to be treated in the case of a continuous flow treatment of liquids, or for circulation a transport liquid 10 in which sealed containers 11 containing the liquid to be treated are immersed. The transport system may advantageously comprise a hot circuit 12a and a cold circuit 12b, each provided with a pumping system 9a, 9b and recirculation of the transport liquid. The hot circuit transports the containers through the electric field heating and application stations and returns the transport liquid through a return conduit 13a to the transport conduit 7 near the inlet station. The cold circuit 13b also has a pumping system 9b and a return pipe 13b interconnecting the transport pipe 7 between a position near the outlet station 8 and an interface 14 separating the hot and cold circuits.

The interface 14 advantageously comprises seals 15 in the form of a plurality of juxtaposed flexible walls, for example of rubber, comprising openings matching the profile of the container to be treated. Thus, the container contributes to the creation of the seal between the hot and cold circuits.

The cold and hot circuits may further comprise heat exchangers 31 and 32 on the return ducts, for recovering the heat of the transport liquid and / or the liquid to be treated. The cold circuit makes it possible to rapidly reduce the temperature of the liquid to be treated in order to preserve the properties of the liquid and, if necessary, reduce the problems of deformation of plastic containers.

The heating station 4 comprises a thermal pulse generation system 35 powered by a thermal energy generator 37. The thermal generator may, for example, be in the form of a high frequency electric field generator operating at a frequency greater than 1MHz or a microwave generator. The energy is transferred from the generator 37 to the system 35 via a coaxial cable or a waveguide 16. It is possible to provide several generators disposed juxtaposed along the transport conduit 7. The An electric field application station 5 comprises a bipolar oscillating electric field pulse distributor 17 connected to a bipolar oscillating electric field pulse generator 18 via a coaxial cable 19.

The thermal pulse stations 4 and the electric field application 5 are separated by a transit section of the thermally insulated conduit 20 creating a pause between the heat treatment and the treatment of electrical pulses. This pause advantageously makes it possible to standardize the temperature field in the liquid to be treated and on the surfaces of the solid bodies in contact with it.

In the embodiment of Figure 3, the liquid to be sterilized is contained in containers 11 immersed in a transport liquid 10 flowing in the conduit 7 to transport the containers. The containers may, for example be plastic bottles, filled, for example, with a beverage or a liquid food.

Once raised in the outlet column portion of the conduit 7b, the containers can be evacuated by a pusher or other mechanism on a conveyor 33.

It is also possible to transport the containers containing the liquid to be sterilized through a heating station and an electric field application station by means other than a liquid in a conduit, for example by a flow of gas under pressure. in a duct (the pressure of the gas being chosen so as to compensate the pressure inside the container, which makes it possible to avoid any deformation of the container due to heating) or by a mechanical transport mechanism such as a conveyor system . Nevertheless, a fluid transport system has the advantage of allowing a good uniformity in the temperature distribution around the container during its heating and during the pause before the application of the electric field. Using a liquid Transporting with dielectric properties similar to those of the liquid to be sterilized advantageously allows to control the warming of the liquid to be sterilized and the application of the local electric field in the liquid to be sterilized. The containers, of dielectric material, can be in the form of rigid containers, such as glass or plastic bottles (for example PET), or in the form of flexible containers, such as plastic bags (polypropylene, PET, or other polymers).

The liquid to be sterilized can also flow directly into the conduit of the device through the heating stations and the application of the electric field.

Agitators 21 may be added to the system to agitate the liquids and, where appropriate, the bodies in a transport liquid. Alternatively, the agitation device creates turbulence in the liquid flowing in the conduit, thus unifying the temperature field in the liquid. Containers transported in the conduit may also be agitated or rotated, for example, by current control in the transport liquid, in order to uniformize the liquid to be treated within the containers.

Tubes of dielectric material (quartz, for example) 22 are mounted in the conduit so as to ensure the passage of the electric field for heating the liquid inside the conduit.

Temperature sensors 23 are arranged all along the duct for measuring the temperature of the liquid at the inlet of the thermal pulse generation station, in the heating zone, at the exit of this zone and at the exit of the transit section of the conduit.

An electric field sensor 24 is disposed in the area of application of the electric field.

In one embodiment of the device, a mechanism is provided to ensure a variable speed of the displacement of the solid bodies during their passage through the conduit, for example, by changing the section (diameter) of the conduit to vary the speed of the flow of the transport liquid.

An electric field distributor device according to a first variant is shown in FIG. 4a. In this variant, the distributor comprises electrodes 25a, 25b disposed on either side of the duct to ensure the passage of alternating electric field pulses of frequency between 10OkHz and 1000kHz transversely through the duct 7 (of FIG. ), as illustrated by the field lines 26.

In particular, the electric field passes from the upper electrode 25a to the lower electrode 25b, the two electrodes being mounted inside a tube

27 (in quartz, for example), hermetically integrated in the conduit through which the liquid 3 and 10 pass. The distance "a" between the electrodes can be optimized empirically so as to ensure the best possible uniformity of the transverse electric field in the volume If the distance a is for example of the order of 4 cm, to obtain an effective electric field amplitude of 1 - 3 kV / cm, it is necessary to have a potential difference between the electrodes of the order of 400 - 120O kV.

Figure 4b illustrates an electric field distributor device according to a second variant. In this variant, the pulses of the electric field are created by an induction system and the electric field lines 26 'are essentially longitudinal. The conduit 7, filled with water as a transport liquid 10 carrying containers 11, such as bottles containing a liquid to be sterilized, passes through a body of the induction system 25. The electric field distributor device is provided with a core 28 and one or more primary windings 29 connected to a power supply via connections 30a, 30b. The amount of primary windings can be determined empirically, for example by measuring the electric field present in the transport liquid.

In the embodiment of FIG. 3, the containers 11 are immersed at a depth H in a column portion 7a of the transport pipe 7 filled with the transport liquid 10. The transport liquid column exerts an external pressure which tends to compensate for the internal pressure during heating of the liquid to be treated according to formula (2) which makes it possible to determine the height H of the column corresponding to the temperature T> T ₁ . (2) H xdxg = (T ₂ / T ₁ ) x P ₁ - C + Vp + Vs where:

"H" is the height of the column of liquid in which the containers to be treated are immersed;

"D" is the density of the external liquid;

"G" is the local acceleration of gravity; "Po" is the initial pressure of the compressible liquid in the container as it enters the device;

"Vs" is the difference between the saturated vapor pressures of the incompressible liquid at temperatures T ₂ and T ₁ . For water, at Ti = 20 ° C for example, the saturated vapor pressure is very small and, practically, Vs is equal to the pressure of the saturated vapors of water at the temperature T ₂ . For example, if T ₂ = 65 ° C, then V _s = 0.25 bar;

"C" is equal to (kx V _v ) where k is the volume elasticity coefficient of the container material at the temperature T ₂ and Vv is the volume strain;

"Vp" is the variation of internal pressure due to the saturation variation of the incompressible liquid by the compressible liquid. Vp is measured in a non-deformable container (for example glass) of the same shape and volume as the treated container, as the pressure difference between the actual gauge pressure at temperature t ₂ and the pressure P ₂ = Po x (T ₂ / Ti). For unsaturated CU ₂ drinks, such as flavored water or milk, V _P is close to zero. Compensation is total when C = O.

The depth H can be decreased by increasing the density d of the external liquid medium used in which the containers are immersed. In particular, it is possible to add to this liquid small solid bodies p (p must be much smaller than the characteristic dimension of the container), but with a density greater than that of the liquid, for example in powder form. This measure will be effective only when the pressure exerted by the solid bodies will be equal in all directions. This will require that the solid bodies be provided with a chaotic motion whose average velocity will be greater than the square root of gp where: "g" is the local acceleration of gravity "p" is the size of the solid bodies and that their specific quantity n (amount of solid body per unit of volume) corresponds to the increase in target density.

To satisfy this condition, it is necessary that the force of gravity of the solid body of mass m, mg, is less than the force F exerted by this body on any wall following its inertia. If v is the chaotic motion velocity, we can obtain for F the order of magnitude F = mx (v / 1), where t = d / v, then F = (mv ² ) / d. It is therefore necessary that F "mg, so that v" (gd) ^(1/2) .

If bottles are processed sequentially and in the direction of their length, one behind the other, a pusher 34 sends the bottles into the horizontal duct portion 7c.

The present invention is useful in the medical and pharmaceutical fields, in particular for the selective decontamination of microorganisms in the blood or in blood components or in other pharmaceutical preparations. It can also be used for the destruction of legionella colonies in sanitary waters.

The method and the device proposed in the present invention can be advantageously used in the food industry for the decontamination (pasteurization, sterilization) of food products containing water or containing water, such as fruit juices, beers, flavored waters, natural mineral waters, milk, milk products and other liquids and liquids.

The present invention is of interest for applications in the field of hygiene, in particular for the disinfection of wastewater, sewage water, and stagnant water. Examples:

1. Decontamination of 0.5 liter PET bottles filled with freshly squeezed orange juice and contaminated with "Byssochlamys nivea" microorganisms. The treatment was carried out on a device of the type illustrated in FIG.

Initial concentration of microorganisms: from 3.6 to 4.2 × 10 ⁵ units / ml;

> Quantity of bottles processed for each diet: 10; > Initial temperature: 20 ⁰ C; > Treatment time: 3s (passage in the horizontal duct);

> Heating: microwave 1 GHz, power 180 kW (35 ° C / s) and 45 kW

(9 ° C / s);

> Application of the electric field:

"Oscillation frequency of the electric field: 180 kHz;" Duration of a packet of oscillations: approx. 0.02 ms; "Oscillation packet frequency: 15 Hz;

Ti = 6μs, t ₂ = 20μs, t ₃ = 0.05s;

• Quantity of pulses: 12 for 180 kW and respectively 35 and 48 pulses for 45 kW;

> Productivity, linear velocity of cylinders: 0.4 m / s for 180 kW and 0.1 m / s for 45 kW. Length of the application area of the field: 0.3 m; duration of application of the electric field pulses: 0.75s; Results:

2. Selective decontamination of 0.5 I PET bottles filled with apple juice and contaminated with Saccharomyces cerevisiae yeasts and Aspergillus Niger molds. The treatment was carried out on a device of the type illustrated in FIG.

> Initial concentration Saccharomyces cerevisiae: 1, 2 - 3.1. ⁵ units / ml;

> Initial concentration Aspergillus niger: 1, 5 - 4,2. ⁵ units / ml;

> Quantity of bottles processed for each diet: 10; > Initial temperature: 20 ⁰ C;

> Treatment time: 3s (passage in the horizontal duct);

> Heating: microwave 1 GHz, power 180 kW (35 ° C / s) and 45 kW (9 ° C / s);

> Application of the electric field: • Frequency of oscillation of the electric field: 180 kHz;

"Duration of a packet of oscillations: about 0.02 ms;

"Oscillation packet frequency: 15 Hz;

"ti = 6μs, t ₂ = 20μs, t ₃ = 0.05s;

> Productivity, linear velocity of cylinders: 0.4 m / s for 180 kW and 0.1 m / s for 45 kW. Length of the application area of the field: 0.3 m; duration of application of the electric field pulses: 0.75s;

Results:

Claims

A process for sterilizing or pasteurizing a liquid to be treated, comprising heating the liquid by electric field waves having a frequency greater than 1 MHz, at a speed greater than 28 ° C. per second, up to a treatment temperature T is between 20 ⁰ C and 66 ° C, and depending on the value of the treatment temperature T, the exposure of the liquid to an alternating electric field in pulses immediately or shortly after heating of the liquid, the amplitude E of the electric field in V / cm being chosen so that the equation:

C (T) ≤ log (E + 1) ≤ B (T) is satisfied for the values:

B (T) = -2.340. 10 ^'5 T ³ + 1, 290. 10 ³ T ² - ^3, 110. 10 ^"2 T + 5.0 C (T) = -4.503, W ⁵ T ³ + 2.888, 10 ^{" 3} T ² - 5.900. 10 ² T + 4.0 where T is the treatment temperature in degrees Celsius.

2. Method according to claim 1, characterized in that the electric field is alternating with an oscillation frequency between 10OkHz and 1000 kHz.

3. Method according to claim 1 or 2 characterized in that the total heat energy supplied to the liquid to be treated by said one or more electric field pulses is less than 0.05 J / cm ³ .

4. Method according to any one of the preceding claims, characterized in that the application of one or more electric field pulses is performed after the step of heating the liquid followed by a pause during which the electric field is no or negligible and the temperature of the aqueous solution becomes uniform.

5. Method according to any one of the preceding claims, characterized in that the duration of application of a pulse of the electric field is between 10 and 100 microseconds and the repetition frequency of the electric field pulses is between 10 and 100 Hz.

6. Method according to any one of the preceding claims, characterized in that the heating rate is greater than 30 ⁰ C per second.

7. Method according to any one of the preceding claims, characterized in that the liquid to be treated is contained in a hermetically sealed dielectric material container.

8. Method according to the preceding claim, characterized in that the container is transported by a transport liquid flowing in a conduit through the heating stations and electric field application.

9. Method according to the preceding claim, characterized in that the transport liquid has dielectric properties similar to those of the liquid to be treated.

10. Process according to claims 8 or 9, characterized in that the transport liquid and the containers are agitated to standardize the temperature of the transport liquids and to be treated.

Apparatus for carrying out a method of sterilizing a water-based or water-containing liquid to be treated, comprising a heating station with a liquid heating system, a water-generating station electric field with a pulsed electric field generation system, and a liquid transport device to be treated comprising a pipe capable of carrying a liquid passing through the heating and electric field application stations, characterized in that the heating system comprises a wave generator operating at a frequency greater than 1 MHz and configured to heat the liquid flowing through the heating station at a rate greater than 28 ^° C. per second, and in that the pulsed electric field generation system is configured to generate an alternating electric field with an oscillation frequency lying between

10OkHz and 1000 kHz.

12. Device according to claim 11 characterized in that the pulsed electric field generation system is configured to provide a total heat energy of less than 0.05 J / cm ³ to the liquid to be treated.

13. Device according to claim 11 or 12 characterized in that the pulsed electric field generation system is configured to generate pulses with a duration of between 10 and 100 microseconds.

14. Device according to any one of claims 11 to 13 comprising a cooling station downstream of the electric field generating station traversed by the transport device.

15. Device according to any one of claims 11 to 14, characterized in that the electric field pulse generation system comprises electrodes arranged on either side of a passage section of the conduit and capable of generating an electric field transverse to this section.

16. Device according to any one of claims 11 to 14, characterized in that the electric field pulse generation system comprises an inductor with one or more primary windings arranged toroidally around a passage section of the conduit. and capable of generating an essentially longitudinal electric field at this section.

Device according to any one of claims 11 to 16, comprising at least one electric field sensor in the zone of application of the electric field and temperature sensors along the transport device, upstream, downstream and in the heating station.

18. Device according to any one of claims 11 to 17, characterized in that the transport device comprises a pump system and a transport liquid for transporting containers containing the liquid to be treated along the conduit, and a circuit for return to return the transport liquid from an outlet to an inlet of the transport device.

19. Device according to any one of claims 11 to 17, characterized in that the transport liquid has dielectric properties similar to those of the liquid to be treated.

20. Device according to one of claims 11 to 17, characterized in that the conduit comprises portions with different passage sections for varying the flow rate of the transport liquid.

21. Use of a device according to any one of claims 17 to 20 for the decontamination of blood or a liquid component of blood contained in hermetically sealed containers.

22. Use of a device according to any one of claims 17 to 20 for the sterilization of drinks or liquid food products contained in hermetically sealed containers.