• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    Freeze dryer for laboratory. It allows to lyophilize samples (12) of reduced volume at temperatures below -50º c, dispensing with mechanical elements that consume power, such as a condenser or a vacuum pump. It comprises a lyophilization chamber (8) equipped with a first semi-chamber (9) and a second semi-chamber (10) connectable to each other in a separable manner maintaining fluid communication. It additionally comprises a first container (3) provided with a first portion (4) containing an adsorbent product (6), and which will be submerged in liquid nitrogen (50), as well as comprising a second portion (5), thermally insulated, and connected to the first semicramera (9). Additionally comprises sealing means (15) configured to provide a tight seal between the first semicrame (9) and the second half chamber (10) under pressure conditions inside the freeze-drying chamber (8) not exceeding 0.2 pa. (Machine-translation by Google Translate, not legally binding)
    公开号:ES2542107A1
    申请号:ES201331932
    申请日:2013-12-30
    公开日:2015-07-30
    发明作者:Gonzalo GONZALO ROMEO
    申请人:Universidad de Zaragoza；
    IPC主号:
    专利说明:


    DESCRIPTION
    Laboratory freeze dryer

    OBJECT OF THE INVENTION 5

    The present invention can be included in the technical field of lyophilization. In particular, the object of the invention relates to a lyophilizer that allows lyophilization of small samples without the need to use vacuum pumps or refrigerated condensers. 10

    BACKGROUND OF THE INVENTION

    There are different and varied procedures for drying a product. Of all of them, the one known as lyophilization is the least aggressive towards the product. fifteen

    A lyophilizer is a device used to carry out lyophilization of a product that contains moisture, called lyophilizable. The lyophilization follows the following steps: First, the freeze-dried is frozen, whereby a part of the moisture is separated from the rest of the freeze-dried in the form of ice. The lyophilisable with ice is then introduced (or maintained) into a freeze-drying chamber (or in suitable containers within a freeze-dryer collector, if it is a manifold-type freeze-dryer), where the freeze-dried remains in the freeze-dried state. in vacuum under conditions of low pressure and low temperature that are substantially on the solid-gas line corresponding to water. 25

    Under these conditions, the ice sublimates with water vapor, which is removed from the lyophilizer to prevent the pressure from rising to outside the solid-gas line. Finally, when there is no ice left and, therefore, the conditions defined by the solid-gas lines are no longer applicable, most of the remaining water is desorbed by heating the lyophilizable under low pressure conditions and up to a temperature compatible with the lyophilisate integrity.

    During the lyophilization, a condenser, connected to cooling means, is used to remove released condensable gaseous compounds, for example sublimed and / or desorbed water vapor. To remove non-condensable gaseous compounds released during lyophilization, a vacuum pump is used.
     5
    DESCRIPTION OF THE INVENTION

    The present invention describes a laboratory lyophilizer, especially intended to lyophilize small samples of a lyophilizable, of the order of a few milliliters, which dispenses power consuming mechanical elements, such as a vacuum pump or a condenser, which are of use. generalized in lyophilizers, and they need to be connected to an external source of energy, for example, a source of electricity.

    The laboratory lyophilizer according to the present invention incorporates a lyophilization chamber. The freeze-drying chamber comprises two half-cameras: a first half-camera, and a second half-camera, where the half-cameras are detachable separately, maintaining a fluid communication between said half-cameras when they are connected. The first half-chamber is configured to house one or more vials inside it intended to contain samples 20 of lyophilisables.

    Sealing means are arranged to close the first half chamber and the second half chamber together, providing a tight seal that is capable of maintaining pressures of the order of 2 µbar or less for days, that is, 0.2 Pa or less. 25

    The lyophilizer additionally incorporates a first container comprising a first closed portion and a second open portion, the first portion being configured to house an adsorbent product, such as activated carbon, to adsorb gases and vapors generated during lyophilization. 30

    The first half chamber is linkable with the second portion of the first container, maintaining a fluid communication between the second portion of the first container and the
    First half camera.

    The first half chamber comprises a first end connectable in use to the first container, as indicated above, as well as additionally comprising a second open end. The second half chamber comprises a first open end 5 fluidly connectable with the second end of the first half chamber.

    Preferably, the first half-chamber and the first container may be integrated in the same element.
     10
    A thermal insulation is incorporated to thermally isolate both the second portion of the first container from the outside as well as preferably also at least a part of the first half chamber and / or the second half chamber.

    Once the first container is linked to the first half chamber (integrally or separably), the first portion of the first container is intended to be inserted into a second container containing liquid nitrogen. Thus, the first container, with the adsorbent product cooled by liquid nitrogen, exerts a function of passive condenser, that is, it is achieved, by incorporating the first container, to reproduce the function of active condensers and vacuum pumps. Freeze-dryers of the prior art without the need for an external source of energy.

    The lyophilizer described above allows lyophilizing small amounts of sample with the quality and repeatability of large lyophilizers. Likewise, since it does not require the use of mechanical elements such as condensers and vacuum pumps, it is exempt from the special precautions and limitations that said mechanical elements imply with respect to the type of lyophilizable and / or the medium in which said lyophilizable are found, in particular when it comes to solvents, volatile acids, etc., which can be harmful to mechanical elements. In the aforementioned case of working with volatile or dangerous diluents, the lyophilizer can be installed in a gas hood, although adequate measures must be taken to treat the adsorbent medium used as a toxic residue.

    On the other hand, the non-incorporation of the aforementioned mechanical elements implies some additional advantageous feature, such as a lower environmental impact, in the sense that it does not require the use of contaminating products, such as condenser refrigerants, or vacuum pump oils, as well as the energy consumption associated with said elements is avoided, which in a conventional freeze dryer can be comprised, depending on the size of the freeze dryer considered, between 1 kW for freeze dryers considered small, and 8 kW, or even higher, for a freeze dryer of the lyobeta type 25, for example.
     10
    By means of the described lyophilizer, temperatures of remarkably below -50 ° C, of the order of -60 ° C and even lower are obtained for amounts of freeze-dried within the indicated range, which is only available to the most complex and sophisticated industrial freeze-dryers, in In any case, it is not known for laboratory lyophilizers of the manifold type. fifteen

    DESCRIPTION OF THE DRAWINGS

    To complement the description that is being made and in order to help a better understanding of the characteristics of the invention, according to a preferred example 20 of practical realization thereof, a set of said description is attached as an integral part of said description. Drawings where, for illustrative and non-limiting purposes, the following has been represented:

    Figure 1.- Shows a schematic view of the lyophilizer of the present invention. 25

    Figures 2a and 2b.- They show detailed views of the sealing means, according to an assembled arrangement (see figure 2a) and according to a separate arrangement (see figure 2b).

    Figure 3.- Shows a view of some of the elements of the closing device, in a disassembled position.

    Figures 4a and 4b.- Shows a detail of the operation of the closing means, in a
    first position (see figure 4a) in which the movement of the locking bar is allowed, and in a second position (see figure 4b) in which it is locked.

    Figure 5.- Shows a view of a support intended to house the vials for depositing said vials inside the first half chamber. 5

    Figure 6.- Shows a detailed view of an embodiment that allows the lyophilizer to be arranged in a freezer.

    PREFERRED EMBODIMENT OF THE INVENTION 10

    Next, a detailed description of a preferred embodiment of the invention is described with the aid of Figures 1 to 5 above.

    The laboratory lyophilizer according to the present invention, as shown in Figure 1, incorporates a freeze-drying chamber (8), comprising two half-cameras (9, 10): a first half-chamber (9), and a second half-chamber (10), where the half-cameras (9, 10) are detachably connectable from each other, maintaining a fluid communication between said half-cameras (9, 10) when connected. The first half-chamber (9) is configured to house one or 20 vials (11) inside it intended to contain samples (12) of lyophilisables. In the embodiment shown in the attached figures, the half-chambers (9, 10) have a cylindrical shape.

    Sealing means (15) are arranged, as seen in Figure 1 and, in greater detail, in Figures 2a and 2b, to close each other the first half chamber (9) and the second half chamber (10), providing a tight seal that is capable of maintaining pressures of the order of 2 µbar or less for days, that is, 0.2 Pa or less.

    According to a preferred embodiment shown in Figures 2a and 2b, the sealing means (15) comprise: at least one gasket (16) resistant to low temperature, for example manufactured in (7) polyethylene 500, and located between the two half-cameras (9, 10); a chain (17) of rollers (53) for pressing on the joints (16); and pressure means (46), to press the roller chain (17) (53) on
    the joints (16). Figure 2a shows a view of the elements that make up the sealing means (15) in a working position, where the half-chambers (9, 10) and the seal (16) have not been represented. Figure 2b shows the elements separately.
     5
    Preferably, as shown in the aforementioned figures 2a and 2b, the pressure means (46) comprise: a frame (47); a first fastener (48), for example, a first hook, located in the frame (47) to be removably attached to a first end of the roller chain (17) (53); a second fastener (49), for example, a second hook, to engage a second end of the roller chain (17) (53), the second fastener (49) being movably linked to the frame (47 ), so that a movement of the second fastener (49) allows the roller chain (17) to be pressed (53) against the joint (16).
     fifteen
    Even more preferably, the second fixing element (49) is fixed to a threaded rod (51), as well as the frame (47) incorporates an internally threaded cylindrical guide (52) to accommodate the rod (51), of such so that by rotating the rod (51) it is possible to move the rod (51) with respect to the frame (47) inside the guide (52), to press the roller chain (17) (53) against the joint (16 ). twenty

    The sealing means (15) described above provide a more uniform pressure on the joints (16), which is not easy to achieve in the case of joints (16) used for low temperatures and / or aggressive products, given that said joints (16) are less elastic. Additionally, the lyophilization chamber (8) is closed in a relatively short time, on the order of a few seconds, usually in about five seconds.

    The lyophilizer additionally incorporates a first hollow container (3) which, in the embodiment shown (see Figure 1), preferably has an elongated shape and, preferably, hollow cylindrical. The first container (3) comprises a first closed portion (4) and a second open portion (5), the first portion (4) being configured to accommodate an adsorbent product (6), such as activated carbon, for
    adsorb gases and vapors generated during lyophilization. Preferably, the first portion (4) of the first container (3) constitutes a widening of the second portion (5), having a transverse surface larger than the second portion (2).
     5
    The incorporation of a thermal insulation (7) is provided to thermally isolate both the second portion (5) of the first container (3), and preferably at least part of the first half chamber (9) and / or the second half chamber (10) from the outside. ).

    The first half chamber (9) is linkable with the second portion (5) of the first container (3), fluid communication being maintained between the second portion (5) of the first container (3) and the first half chamber (9). The first half chamber (9) comprises a first end connectable in use to the first container (3), as well as additionally comprises a second end. The second half camera (10) comprises a first end fluidly connectable with the second end of the first half camera (9). In the embodiment shown in the figures, the first half chamber (9) and the first container (3) can be integrated into the same element.

    The first portion (4) of the first container (3), is intended to be inserted into a thermally insulated second second container (1) containing liquid nitrogen (50), as illustrated in Figure 1. Thus, the first container ( 3), with the adsorbent product (6) cooled by the liquid nitrogen (50) of the second container (1), it exerts a passive condenser function, that is, it is achieved, by incorporating the first container (3), to reproduce the function of the active condensers of the lyophilizers of the prior art without the need for an external source of energy.

    The second container (1) can be of the Dewar glass type or the like; in general, it can be any container equipped with a convenient thermal insulation, and adapted to contain liquid nitrogen (50). 30

    Additionally, as seen in Figure 1, the first container (3) may incorporate longitudinally, within at least part of the second portion (5),
    a conduction body (14) of highly conductive material, such as, for example, a copper tube, communicated with the first half chamber (9). The conduction body (14) allows heat to be removed from the first half-chamber (9) towards the liquid nitrogen (50), allowing to maintain a lower temperature in the first half-chamber (9), at the cost of a higher consumption of liquid nitrogen (50 ) and of a longer duration in the lyophiization process 5. Preferably, the conduction body (14) is removable, conduction bodies (14) being able to be used with different thermal conductivities, for example, varying the length and / or thickness of the conduction body (14), to adapt the lyophilizer at different temperature needs.
     10
    The lyophilizer additionally incorporates, as can be seen in Figure 1 and, in greater detail, in Figures 3, 4a and 4b, in a way that can be coupled to the second end of the second half chamber (10), a closing device for once finished lyophilization, close the vials (11) comprising samples (12) of lyophilisables. Usually, the vials (11) incorporate standard rubber stoppers (13). The closure device incorporates a press (19), which is movable inside the lyophilization chamber (8) along a direction of travel that is the longitudinal direction of the lyophilization chamber (8).

    The press (19) comprises a pushing face (20) intended to contact the 20 caps (13) to push the caps (13) and thus cover the vials (11). The press (19) allows a fluid communication between the first half chamber (9) and a first bore (25) of a locking body (24), as will be explained later. For example, as shown in the figures, the press (19) can incorporate at least one through hole (21), which for simplicity is coaxial. 25

    The closing device further comprises locking means to retain the longitudinal displacement of the press (19). The locking means comprise a locking body (24) linked to the press (19) at one end of the press (19) opposite the thrust face (20). In the embodiment shown, the locking body 30 (24) and the press (19) are integrated in the same element. The locking body (24) is hollow, since it incorporates a first longitudinal bore (25), preferably cylindrical, as well as a first spring (26) housed in the first bore (25). The body of
    lock (24) additionally incorporates at least a second through hole (27), preferably at least two second holes (27), which communicate the outer surface of the lock body (24) with the first hole (25).

    The blocking means further comprise a longitudinally movable locking bar (28), 5, provided with a first end and a second end, and comprising a first portion (29), preferably cylindrical, located at the first end, and housed in the first hole (25), in contact with the first spring (26). The first portion (29) maintains a play (not shown) with the wall of the first bore (25) to allow fluid communication between the lyophilization chamber (8) 10 and a pressure sensor (37), as will be explained below. . The first portion (29) of the locking bar (28) comprises a spring section (30) and a stop section (31). The spring section (30) is located in correspondence with the first spring (26) and preferably incorporates an axial housing (32) to accommodate part of the first spring (26). The stop section (31) is farther to the first end of the locking bar (28) 15 than the spring section (30), as well as having a section, preferably cylindrical, of smaller value than the spring section (30).

    The blocking bar (28) also comprises a second portion (33), following the stop section (31), which has a decreasing section from the junction with the 20 stop section (31). Preferably, the second portion (33) has a frustoconical shape. Additionally, the locking bar comprises a third portion (34), which occupies the second end of the locking bar (28), and protruding from the second end of the second half-chamber (10), preferably allowing fluid communication between the freeze drying chamber (8) and outside. 25

    The blocking means additionally comprise fasteners (35) represented in the figures in the form of rigid spheres. The latches (35) occupy the second holes (27), and are provided with a transverse movement through said second holes (27), limited by the locking body (24) and the locking bar (28), between the 30 which are the fasteners (35) retained.

    The locking bar (28) is forcedly movable against the first spring
    (26) with respect to the press (19) and the locking body (24) to a position of maximum contraction of the first spring (26) shown in Figure 4a. In this position, the first spring (26) exerts a force that tends to move the locking bar (28) until the stop section (31) comes into contact with the latches (35) and the displacement in favor of the first spring (26) is blocked by the pressure of the 5 second holes (27) on the fasteners (35), as shown in Figure 4b.

    Preferably, the second half-camera (10) can incorporate grooves (56) to partially accommodate the fasteners (35).
     10
    The closing device additionally incorporates a second spring (36) linked inside the second half chamber (10), see figures, 1, 4a and 4b, to press the assembly formed by the press (19) towards the vials (11), the locking body (24) and the locking bar (28).
     fifteen
    The closing device may additionally comprise:
    - a threaded portion (56), at the second end of the locking bar (28); Y
    - a retaining nut (55) connectable in the threaded portion (56) to keep the second end of the locking bar (28) outside the second half chamber (10) when the second spring (36) is in a position of maximum elongation. twenty

    Preferably, the lyophilizer can incorporate a pressure sensor (37), shown in Figure 1, to estimate the pressure of the lyophilization chamber (8). As shown in Figure 1, the lyophilizer incorporates a sheath (38), for example rubber, where a first end of the sheath (38) surrounds the second end of the second half chamber (10), including, where appropriate , the second end of the locking bar (28). The first end of the sheath (38) is in communication with a second free end of the sheath (38), in which the pressure sensor (37) is located.

    The sheath (38) may incorporate inside a pusher (39) integral with the sheath (38), 30 which is sandwiched between the second end of the sheath (38) and the position intended to be occupied by the second end of the lock bar (28). The pusher (39) is configured to allow fluid communication between the first end and the second
    sheath end (38), to facilitate measurement by the pressure sensor (37). Also, between the first end of the sheath (38) and the second end of the second half-chamber (10) a removable separator (40) is located, which can be removed to allow the sheath (38) to move towards the second end of the second half camera (10). 5

    Additionally, the sheath (38) can incorporate an inlet (41), fluidly connectable with the lyophilization chamber (8), to subject the samples (12) to an atmosphere under the required conditions.
     10
    To break the gap, the following steps are performed:
    A: separating the freeze-drying chamber (8) and the first container (3) from the second container (1), which can be arranged in a support element (not shown) and then the separator (40) is removed, as well as the sheath (38) is pushed towards the second half chamber (10), so that the pusher pushes the locking bar (28) in 15 against the first spring (26), so that the latches (35) are unlocked, allowing the second spring (36) push the press (19) against the caps (13), to close the vials (11) with the caps (13).

    B: Next, the sheath (38) is pulled away from the second half chamber (10) 20 until the entrance (41) exceeds a second end, opposite the first end, of the second half chamber (10).

    To introduce an atmosphere under the required conditions, step B is performed first and then, once the pressures are balanced, step A is carried out.

    To carry out the lyophilization procedure using the described lyophilizer, proceed in the following order:

    0.-The assembly of the first half-chamber (9) and the second container (3) is placed in a preparation support (42), comprising a threaded bore (43) to insert a threaded rod (44), verifying that The press (19) is prepared for the closure of vials (11), as shown in Figure 4b.

    1.-The first portion (4) of the first container (3) is filled with the appropriate amount of the adsorbent material (6).

    2.-Once prepared the vials (11) with the samples (12) and the corresponding caps (13) 5 in the support (42), the assembly is introduced in liquid nitrogen with the help of a threaded rod (44) that It allows simple handling.

    3.-With the frozen samples in its support (42), the support (42) is moved with the help of the threaded bar (44) to the first half chamber (9). 10

    4.-The second half-chamber (10) is placed on the first half-chamber (9) with the interposition of the seal (16) and the lyophilization chamber (8) is closed with the sealing means (15).
     fifteen
    5.-The separator (40), the sheath (38) and the sensor (37) are placed so that the lyophilizer is closed tightly.

    6.-We introduce the first portion (4) of the first container (3) in the second container (1) previously filled with liquid nitrogen. twenty

    It is desired that, before the adsorbent material (6) reaches the temperature of liquid nitrogen, the freeze dryer assembly is hermetically sealed so that the adsorbent material (6) is not saturated with the gases of the atmosphere and is rendered useless.
     25
    The sublimation of the humidity of the samples (12) takes place, which is transformed into steam and condenses in the form of ice in some area of the first container (3) next to the adsorbent material (6) and with the appropriate temperature for it. It is desired to emphasize that, between the temperature of the liquid nitrogen of the adsorbent material (6) of the first portion (4) of the first container (3), and the temperature of the freeze-drying chamber (8), a temperature gradient is established in which there will always be an area with a temperature low enough to condense the sublimed water vapor from the samples in ice form. Next, a chamber heater is operated
    (45) to heat the lyophilization chamber (8), in particular the first half chamber (9), so that the moisture and, where appropriate, other substances remaining in the samples (12), evaporate and condense on the walls of the second portion (5) of the first participant (3) or adsorbed by the adsorbent material (6) in the first portion.
     5
    Next, the void is broken, as explained in a previous paragraph.

    Finally, the sealing means (15) can be removed, that is to say, release the roller chain (17) (53), and remove the closed vials (11). 10

    A container heater (54) is surrounding the second portion (5) of the first container (3), to defrost the condensed ice during lyophilization, thus preparing the lyophilizer for the next lyophilization operation.
     fifteen
    For very low freeze-drying temperatures, the sublimation rate is extremely small (thicknesses less than 1 mm per day for temperatures below -65 ° C), whereby the supply of energy from the environment is decisive and limiting. Therefore, the lyophilizer of the present invention can be introduced into a freezer adapted to extreme process temperatures, for example up to -70 ° C. 20 For this purpose, as shown in Figure 6, the lyophilizer can additionally incorporate an insulating body (57) that thermally surrounds and insulates the sheath (38) and the pressure sensor (37), as well as can also incorporate a heater sheath (58), for example electrical resistors, to keep the sheath (38) and the pressure sensor (37) away from extremely low temperatures that can affect its correct operation and even its integrity.

    权利要求:
    Claims (20)
    [1]

    1.- Laboratory freeze dryer, characterized in that it comprises:
    - a first container (3), comprising a first closed portion (4) and a second open portion (5), where the first portion (4) is configured to, in use, 5 contain a gas adsorbent material (6) and vapors, as well as to remain submerged in liquid nitrogen (50);
    - a thermal insulation (7) to provide thermal insulation to at least the second portion (5) of the first container (3);
    - a freeze drying chamber (8) comprising: 10
    - a first half chamber (9), configured to accommodate one or more vials (11) with freeze-dried samples (12), and comprising: a first end fluidly connectable, in use, with the second portion (5) of the first container (3) ); Y
    - a second half-camera (10), linkable to the first half-camera (9) in a separable manner maintaining fluid communication; and 15
    - sealing means (15) configured to provide a tight seal between the first half chamber (9) and the second half chamber (10) under pressure conditions inside the freeze drying chamber (8) not exceeding 0.2 Pa.

    [2]
    2. Laboratory freeze dryer, according to claim 1, characterized in that it additionally comprises a second vessel (1), thermally insulated, configured to contain liquid nitrogen (50), and detachably connectable to the first portion (4) of the first container (3), to accommodate said first portion (4) of the first container (3) submerged in the liquid nitrogen.
     25
    [3]
    3. Laboratory freeze dryer according to claim 1, characterized in that it additionally comprises a closing device for, after lyophilization, closing the vials (11), wherein the closing device incorporates:
    - a movable press (19) along the lyophilization chamber (8);
    - a pushing face (20), located at one end of the press (19) and intended to contact with stoppers (13) for the vials (11);
    - blocking means for retaining the movement of the press (19), comprising:
    - a locking body (24) connected to the press (19) at an opposite end
    that of the thrust face (20), comprising the locking means:
    - a first longitudinal bore (25);
    - a first spring (26) housed in the first bore (25); Y
    - at least a second through hole (27) through the first hole (25); 5
    - a locking bar (28), comprising:
    - a first portion (29) located at a first end, and housed in the first bore (25), in contact with the first spring (26), which comprises a spring section (30) in correspondence with the first spring (26 ), and a stop section (31), farther from the first end of the 10 stop bar (28) than the spring section (30), and provided with a smaller section than that of the spring section (30);
    - a second portion (33), following the stop section (31), with decreasing section from the junction with the stop section (31); Y
    - a third portion (34), which occupies a second end of the locking bar (28), and which protrudes through the second end of the second half chamber (10);
    - one or more fasteners (35), housed in the corresponding second holes (27), and provided with a transverse movement through the second holes (27), limited by the locking body (24) and the locking bar ( 28), among the 20 which are the guarantors (35) retained; Y
    - a second spring (36) connected to the interior of the second half chamber (10), to press together the vials (11) the press (19), the locking body (24) and the locking bar (28), where the locking bar (28) is longitudinally movable by the action of the first spring (26) from a first position in which the first spring (26) is compressed to a second position in which the stop section (31) is in contact with the fasteners (35) and the fasteners (35) are retained in the second holes (27), preventing the movement of the locking bar (28); as well as the locking bar (28) is movable, by means of the third portion (34) of said locking bar (28), against the first spring (26), to return to the first position and allow the second spring (36) move the locking body (24) and the press (19) against the caps (13) to close the vials (11).

    [4]
    4. Laboratory freeze dryer according to claim 3, characterized in that the second half chamber (10) incorporates grooves (59) to partially accommodate the fasteners (35).

    [5]
    5. Laboratory freeze dryer according to claim 3, characterized in that the locking body (24) and the press (19) are integrated in the same element.

    [6]
    6. Laboratory freeze dryer according to claim 3, characterized in that the spring section (30) additionally incorporates an axial housing (32) to accommodate part of the first spring (26). 10

    [7]
    7. Laboratory freeze dryer, according to claim 3, characterized in that it additionally incorporates:
    - a sheath (38) provided with a first end that surrounds the second end of the second half-chamber (10), housing the second end of the locking bar (28), 15 being the sheath (38) movable with respect to the second half-chamber (10);
    - a pusher (39), integral with the sheath (38) inside the sheath (38), and which is sandwiched between the second end of the sheath (38) and the position intended to be occupied by the second end of the locking bar (28);
    - a removable separator (40), located between the first end of the sheath (38) and the second second end of the second half chamber (10), to separate the sheath from the second half chamber (10); Y
    - a pressure sensor (37) located inside the sheath (38), at a second end of the sheath (38);
    where the pressure sensor (37) is in fluid communication with the lyophilization chamber (8) through the press (19), the locking body (24), the second half chamber (10), the third portion (34 ) of the locking bar (28), the sheath (38) and the pusher (40).

    [8]
    8. Laboratory freeze dryer, according to claim 7, characterized in that, the sheath (38) additionally incorporates an inlet (41), fluidly connectable with the lyophilization chamber (8), to submit the samples (12) to an atmosphere under the required conditions.

    [9]
    9. Laboratory freeze dryer according to claim 3, characterized in that the closing device further comprises:
    - a threaded portion (56), at the second end of the locking bar (28); Y
    - a retaining nut (55) connectable in the threaded portion (56) to keep the second end of the locking bar (28) outside the second half chamber (10) when the second spring (36) is in a maximum elongation position.

    [10]
    10. Laboratory freeze dryer according to claim 1, characterized in that the sealing means (15) comprise:
    - at least one gasket (16) resistant to low temperature, and located between the two half-chambers (9, 10);
    - a chain (17) of rollers (53) for pressing on the at least one gasket (16); Y
    - pressure means (46), to press the roller chain (17) (53) over the seals (16). fifteen

    [11]
    11. Laboratory freeze dryer according to claim 10, characterized in that the pressure means (46) comprise:
    - a frame (47);
    - a first fastener (48), located in the frame (47), to be removably attached to a first end of the roller chain (17) (53);
    - a second fastener (49), to engage a second end of the roller chain (17) (53), the second fastener (49) being movably linked to the frame (47), so that a displacement of the Second fastener (49) allows the roller chain (17) to be pressed (53) against the seal (16). 25

    [12]
    12. Laboratory freeze dryer, according to claim 11, characterized in that it additionally incorporates:
    - a threaded rod (51) fixed to the second fixing element (49); Y
    - an internally threaded cylindrical guide (52), and fixed to the frame (47) to accommodate the rod (51), such that a rotation of the rod (51) provides a displacement of the rod (51) relative to the frame (47) ) inside the guide (52), to press the roller chain (17) (53) against the seal (16).

    [13]
    13. Laboratory freeze dryer according to claim 1, characterized in that the first container (3) has an elongated shape.

    [14]
    14. Laboratory freeze dryer according to any one of claims 1, 5 and 13, characterized in that the first portion (4) of the first container (3) has a larger cross-section than the second portion (5).

    [15]
    15. Laboratory freeze dryer according to claim 1, characterized in that the semi-chambers (9, 10) have a cylindrical shape. 10

    [16]
    16. Laboratory freeze dryer according to claim 1, characterized in that the first container (3) longitudinally incorporates, inside at least part of the second portion (5), a conductive body (14) of conductive material , communicated with the first half-chamber (9), to remove heat from the first half-chamber 15 (9) towards the liquid nitrogen (50).

    [17]
    17. Laboratory freeze dryer according to claim 16, characterized in that the conduction body (14) is removable.
     twenty
    [18]
    18. Laboratory freeze dryer according to claim 1, characterized in that at least part of the first half chamber (9) and / or the second half chamber (10) additionally incorporates the thermal insulation (7).

    [19]
    19. Laboratory freeze dryer according to claim 1, characterized in that it additionally comprises a support (42) for housing the vials, wherein the support comprises a threaded bore (43) to accommodate a threaded rod (44) to displace the support (42).

    [20]
    20. Laboratory freeze dryer according to claim 7, characterized in that it additionally comprises:
    - an insulating body (57) that thermally surrounds and insulates the sheath (38) and the pressure sensor (37), and
    - a third heater (58), to heat the sheath (38) and the pressure sensor (37). 5
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    同族专利:
    公开号 | 公开日
    ES2542107B1|2016-05-12|
    WO2015101681A1|2015-07-09|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    US4232453A|1978-09-25|1980-11-11|C. Reichert Optische Werke, Ag|Device for freeze drying and synthetic resin impregnation when necessary of small biological objects for electron microscopic examination|
    AT398849B|1992-09-08|1995-02-27|Sitte Hellmuth|CHAMBER FOR FREEZING DRYING BY CRYOSORPTION|
    US8196416B2|2004-02-02|2012-06-12|Core Dynamics Limited|Device for directional cooling of biological matter|CN112146363B|2020-09-10|2021-09-21|天津华龛生物科技有限公司|Pre-freezing drying system and method for microcarrier|
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    ES201331932A|ES2542107B1|2013-12-30|2013-12-30|LABORATORY LIOFILIZER|ES201331932A| ES2542107B1|2013-12-30|2013-12-30|LABORATORY LIOFILIZER|
    PCT/ES2014/000218| WO2015101681A1|2013-12-30|2014-12-17|Freeze-dryer for a laboratory|
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