CZ2017789A3 - Devices for cooling gases, liquids and / or volatile substances - Google Patents

Abstract

The device is intended for cooling gases, liquids and / or volatile substances that pass through a straight tube (1.6, 2.6., 3.6, 4.6), the device comprising a container (1.1, 2.1, 3.1, 4.1) for the refrigerant. The vessel (1.1, 2.1., 3.1, 4.1) has at least one wall (1.3, 2.3, 3.3, 4.3) selected from the side walls and the bottom made of a thermally conductive material, with a contact element (1.5, 2.5 , 3.5, 4.5) U-shaped. The advantage of the designed cooler is the simplicity of the apparatus, its easy removability and the ease of moving / moving the cooled spot along the apparatus tube.

Description

Technical field

The present invention provides apparatus for cooling gases, liquids and / or volatiles, particularly suitable for laboratory use.

BACKGROUND OF THE INVENTION

In many chemical, physical and technological processes, it is necessary to cool or freeze gases, liquids and / or volatiles from the mixture passing through the apparatus. In particular, on a laboratory scale, it would be highly advantageous to freeze gases or volatiles at substantially any point in the apparatus tube as needed.

At present, there is no commercially available laboratory aid that would allow gas freeze to temperatures near the boiling point of liquid nitrogen in a horizontally oriented tube. Typically, therefore, it is necessary to provide an apparatus in which gases, liquids and / or volatile substances are to be freeze-dried with elements which allow the conducting of gases, liquids, resp. volatile substances below the level of liquid nitrogen or other coolant (eg U-tube or freeze-thumb). This increases the complexity, failure rate and cost of the constructed apparatus, and gases, liquids and volatiles can only be frozen at a predetermined location of the apparatus. There are also gas coolers for apparatus where the gas passes through a set of two coaxial tubes between which a liquid is placed and which optionally may have elements increasing the contact area for heat transfer (WO 2013/150318). At least the inner tube must be of a material which is inert to the flowing gases and which consists of a solid, so that after assembly of the apparatus it is not possible to change the cooling or freezing of the gases and cannot easily remove the cooler from the apparatus.

SUMMARY OF THE INVENTION

The present invention provides a device for cooling gases and / or liquids and / or volatiles, particularly suitable for laboratory use (laboratory cooler), which allows to cool gases, liquids and / or volatiles in a straight tube without the need to replenish the tube with other elements necessary for freeze-drying and without the need for specific modifications to the cooled section of the tube.

By cooling gases, liquids and / or volatiles is meant reducing the temperature of gases, liquids and / or volatiles by transferring heat therefrom to the apparatus of the invention. One type of cooling is freezing. By freezing gases, liquids and / or volatiles, it is meant to lower the temperature of the gases, liquids and / or volatiles so as to change their state from gaseous to solid or liquid, or from liquid to solid. Freezing of gases, liquids and / or volatiles is often used to isolate one component from a mixture, for example from a mixture of gaseous or liquid components. Preferably, gases and / or volatiles are isolated from the gas mixtures by freeze-drying. Volatiles may include sublimers, where cooling (preferably freeze) results in a change of state from gaseous to solid. Cooling, preferably freezing, can be carried out with a cooling medium having a temperature such that the desired gas, liquid and / or volatile species are latched at a given pressure. The cooling medium can be, for example, liquid nitrogen (-196 ° C, particularly suitable for gas freezing), ethanol-solid CO 2 (-78 ° C), water with ice, optionally with salt, water. A person skilled in the art is aware of the transition temperatures at a given pressure as well as suitable coolants, or can be found in the general literature and tables, and optionally calculated according to relevant equations.

- 1 Mar 2017 - 789 A3

The apparatus for cooling gases, liquids and / or volatiles passing through a straight tube comprises a coolant vessel having at least one wall made of a thermally conductive material, wherein a U-shaped open element is provided along the entire length of the wall. The U-shape allows insertion of the tube into the contact element and its eventual encirclement by the fastening element, so its width should correspond to the diameter of the tube for which it is intended.

The term wall herein may include a side wall of the container or the bottom of the container. When the wall is a side wall, the device is particularly suitable for cooling gases, liquids and / or volatiles passing through a vertically or substantially vertically oriented straight tube. When the wall is a bottom, the device is particularly suitable for cooling gases, liquids and / or volatiles passing through a horizontally or substantially horizontally oriented straight tube.

In one case, the contact element is a U-shaped recess made in the container wall (side wall or bottom). In such a case, the container wall is then usually thickened so that its thickness is greater than the depth of the recess. It is particularly preferred that the height of the legs of the U-shaped recess is greater than the diameter of the tube for which the device is intended. The U-shaped recess should match the diameter of the tube for which the device is designed to achieve the best possible heat transfer. In one preferred embodiment, at least two recesses are provided in the thickened wall inside the container, which reduce the material thickness between the cooled tube and the cooling material and further increase the cooling efficiency.

In another case, the contact element may be a U-shaped profile on the wall of the container, for example if the container is made of sheet metal, the arms of the profile being longer than the diameter of the tube and its width corresponding to the diameter of the tube. This profile can be made by molding a portion of the wall towards the inside of the container.

It is also particularly advantageous if the container including the wall provided with the contact element, but excluding the contact surface of the U-shaped contact element for the tube, is provided with thermal insulation on the outer walls. This is particularly useful when the cooling medium is a very low temperature medium such as liquid nitrogen. In general, thermal insulation reduces the warming of the coolant from the environment and increases the cooling efficiency of the tube in which gases, liquids and / or volatiles are to be cooled. Preferably, the wall of the container with the contact element, including the cooled section of the tube in the contact element, is also insulated from the environment by thermal insulation. However, the insulation in this section must be easily removable to ensure that the entire device can be easily removed from the tube if necessary.

The container may have any suitable wall shape provided with a contact element. If the wall is a bottom, a suitable bottom shape may be, for example, round, square, rectangular. The bottom may advantageously be provided with a U-shaped recess as a contact element. In the round bottom shape, the U-shaped recess is preferably guided along the diameter of the circle, through the center of the circle.

In a square wall shape, the U-shaped recess may be guided parallel to the side of the wall or, especially if the wall is a bottom, to increase the diagonal heat transfer area. In a rectangular wall shape, the U-shaped recess can be guided parallel to the side of the wall, preferably the longer side of the wall, or - especially if the wall is a bottom - to increase the diagonal heat transfer area.

The material of the thermally conductive wall or the entire container may preferably be a metal, in particular aluminum or copper. It is preferable that the entire inner wall of the container is made of one piece of metal, integral with the bottom, since this reduces the risk of coolant leakage and at the same time increases the useful life of the container used. Such a container can be formed, for example, by turning from the metal, or by molding from metal sheet.

The vessel is provided with an opening for the coolant inlet. In one embodiment, the coolant inlet may be non-closable, i.e., for example, the container may have an open top end,

-2GB 2017 - 789 A3 to remove any gases released when captured by some coolants (eg using liquid nitrogen).

The container can be applied and held by the user over the insulating layer when used for freezing (for safety reasons and to minimize unnecessary losses / heating of the coolant), can be fixed in the desired position against the tube using laboratory clamps and holders, or provided in the region of the wall provided with the contact element with fastening means for fastening to the tube, for example fastening clamps or strips, or may be provided with telescopic legs for resting on a support in the desired position with respect to the tube.

In addition to the simplicity of the apparatus, another advantage of the proposed cooler is its easy removability and easy movement / displacement of the cooled location along the apparatus tube. Simplifying the cooling or freezing apparatus also reduces its internal surface and thus suppresses the memory effect during sample processing. The device according to the invention is relatively easy to manufacture with relatively low material and labor costs.

When using the proposed type of cooler, the apparatus itself can be quite simple, in some cases only the horizontal or vertical tube is sufficient. Such a relatively inexpensive apparatus can be easily and quickly created and, if necessary, can also be easily and quickly replaced with a new one.

The advantage of the simplified apparatus is its low price and also easy and quick feasibility. In some of the cases tested, the apparatus itself consisted only of a tube which was sealed at one end. A new tube could therefore be used to process each sample.

The present invention includes a set of tube and device according to the invention.

The present invention further encompasses the use of the apparatus of the invention to freeze gases and / or volatiles passing through a straight tube, particularly in laboratory apparatus.

Further, the present invention includes a method of cooling / freezing gases and / or volatiles passing through a straight tube, particularly in laboratory apparatuses, which comprises contacting or fastening the device of the invention so that the U-shaped recess encircles the tube.

Clarification of drawings

Giant. 1 shows the device described in Example 1 (in a cross-section through the U-shaped recess, in a cross-section through the U-shaped recess, and in a top view).

Giant. 2 illustrates the apparatus described in Example 4 (in cross section through the U-shaped contact element, in cross section perpendicular to the U-shaped contact element, and in a top view).

Giant. 3 shows the device described in Example 5 (in a cross-section through the U-shaped recess, in a cross-section through the U-shaped recess, and in a top view).

Giant. 4 illustrates the device described in Example 6 (in cross section through the U-shaped contact element, in cross section perpendicular to the U-shaped contact element, and in a top view).

-3GB 2017 - 789 A3

DETAILED DESCRIPTION OF THE INVENTION

Example 1

An example of a device for freezing gases and / or volatiles passing through a horizontal tube is shown in Figure 1 (in cross section through U-shaped recess, in cross section perpendicular to U-shaped recess, and in top view). The apparatus comprises a vessel 1.1 with a coolant space 1.2 having a wall (here bottom) 1.3 made of a thermally conductive material, wherein a U-shaped recess 1.5 is provided over the entire length of the bottom. As seen in Fig. 1 the bottom 1.3 has a thickness greater than the diameter of the tube 1.6 for which the device is intended. The U-shaped recess 1.5 corresponds in shape to the tube L6 for which the device is intended.

The vessel 1.1, including the bottom 1.3, but excluding the U-shaped recesses 1.5, is provided with 1.4 thermal insulation on the outer walls. This is particularly useful when the cooling medium is a very low temperature medium such as liquid nitrogen.

The container may have any suitable bottom shape, for example, round, square, rectangular. In the embodiment shown in Fig. 1, the container 1.1 has a round bottom shape and the U-shaped recess extends along the diameter of the circle, through the center of the circle, and through this recess the tube 1,6 passes through.

The material of the bottom or the entire container is thermally conductive, for example a metal, in particular aluminum or copper. In the embodiment shown in FIG. 1, the entire inner wall of the container is made of metal, integral with the bottom, since this reduces the risk of coolant leaking. For example, the container may be turned.

On bottom 1.3, two auxiliary recesses 1/7 are provided for better heat transfer for cooling the tube. When the container is filled, the coolant flows into these auxiliary recesses 1.7.

The vessel is provided with an opening for the coolant inlet. In the embodiment of this example, the container has an open top end and is therefore suitable for use with a horizontally positioned tube 1.6.

The container can be applied and held by the user's hand when used for freezing, it can be fixed in the desired position with respect to the tube by means of laboratory clamps and brackets, or can be provided in the bottom area with fixing means (not shown) for tube mounting, for example optionally, it may be provided with telescopic uprights for resting on a support in a desired position relative to the tube (not shown).

Example 2

Preparation and cleaning of tar combustion products released by thermal decomposition of wood

The apparatus of Example 1 was used to isolate CO 2 and water resulting from the burning of tars released by heating a wood sample. A quartz glass tube with an outer diameter of 12 mm, a wall thickness of 1 mm, and a total length of 1000 mm was used. One end was sealed. A 1 g sample of wood was placed in the sealed tube end. At a distance of about 50 mm from the sample, a CuO (oxidizing agent) layer having a total weight of approx. The mounted tube was fixed in a horizontal position using laboratory holders. The open end of the mounted tube was connected to a vacuum pump via a vacuum coupling and its internal volume was then evacuated for 30 minutes to a final pressure of less than 15 Pa. After the pump was disconnected by the tap behind the vacuum coupling, CuO was tempered to approximately 700 ° C. Thereafter, the cooling apparatus of Example 1 was cooled with liquid nitrogen, the temperature stabilizing after approximately five minutes of cooling the vessel. The liquid nitrogen tempered device was placed on a stepped tube between the sections

-4GB 2017 - 789 A3 with CuO and unsealed end. The wood sample was then heated with a gas burner, the released tars were burned in a tempered CuO layer, and the tar combustion products (CO2 and H2O) were collected in a portion of the tube cooled by the proposed apparatus. After the thermal decomposition of the wood sample was completed, a similar cooling device was placed on the closed side of the tube and the device was removed from the originally cooled part. The prepared CO 2 and H 2 O were again passed through a layer of tempered CuO in order to be free of residual tar content. After quantitative conversion, the purified combustion products were recycled back through the CuO layer and condensed at the original site. Then the CuO heating was stopped, the tube was connected via a vacuum coupling to an evacuated liquid nitrogen cooled vial. The purified combustion products were then (after removal of the device from the tube) sublimated into a chilled ampoule for further processing (analysis of hydrogen and carbon isotopes in the combustion products).

Example 3

Remove tar from the water sample

A quartz glass tube having an outer diameter of 12 mm, a wall thickness of 1 mm and a length of 1000 mm was sealed at one end. Approximately in the middle of the tube, a CuO layer (approx. 10 g) was placed and its position was fixed with S1O2 cotton wool (2x approx. 4 mL). The mounted tube was fixed in a horizontal position by means of laboratory holders and clamps, connected to a vacuum pump via a vacuum coupling, evacuated and disconnected from the pump by a tap. The apparatus of Example 1 was tempered with liquid nitrogen and placed near the closed end of the tube. The CuO layer was tempered to 700 ° C. Then the tar-containing water (prepared by burning the wood sample) was transferred by sublimation to a tube. After the quantitative transfer of water to the freeze section of the tube, another liquid nitrogen tempered apparatus of Example 1 was placed between CuO and the vacuum coupling. Thereafter, the device was removed at the closed end of the tube and the water vapor was passed again through tempered CuO. An evacuated liquid nitrogen-cooled vial was then connected to the tube via a vacuum coupling. The cooling device (in the position between the CuO and the vacuum coupling) was removed from the tube and the purified water was sublimated into an evacuated vial for further processing.

Example 4

The apparatus of Example 4 is shown in Fig. 2. Analogously to the apparatus described in Example 1, the apparatus has a vessel 2.1 with a cooling space 2.2, wherein a contact element 2 is formed in one wall (here bottom) 2.3. The container with the contact element is molded from sheet metal and provided with an external thermal insulation of 2.4. It is suitable for horizontally oriented cooled tubes 2.6 whose diameter corresponds to the dimensions of the contact element 2.5.

Example 5

The apparatus according to Example 5 is shown in FIG. 3. This apparatus has a vessel 3.1 with a coolant compartment 3.2 provided with external thermal insulation 3.4. In the side wall 3.3 (cylindrical shell wall), the contact element 3.5 is milled, which is a U-shaped recess. The device is turned integrally of metal. The U-shaped recess 3.5 corresponds dimensionally to the cooled tube, and is suitable for a substantially vertically oriented tube.

-5GB 2017 - 789 A3

Example 6

The apparatus of Example 6 is shown in FIG. 4. The apparatus has a vessel 4.1 with a cooling chamber 4.2. The container is molded from sheet metal such that a recess U in the shape of a recess U is formed in the side wall 4,3 (cylindrical casing wall). The vessel is provided with an external thermal insulation of 4.4.

PATENT CLAIMS

Claims (10)

Apparatus for cooling gases, liquids and / or volatiles passing through a straight tube (1.6, 2.6, 3.6, 4.6), the apparatus comprising a vessel (1.1, 2.1, 3.1, 4.1) for a coolant, characterized in that the vessel (1.1 , 2.1, 3.1, 4.1) has at least one wall (1.3, 2.3, 3.3, 4.3) selected from side walls and a bottom made of a thermally conductive material, wherein a contact element (1.5, 2.5, 3.5, 4.5) is provided along the entire length of said wall ) in the U shape. Device according to claim 1, characterized in that the contact element is a U-shaped recess (1.5, 3.5) made in the container wall, the depth of the U-shaped recess (1.5, 3.5) being greater than the diameter of the tube (1.6, 3.6) and its the width corresponds to the diameter of the tube (1.6, 3.6), preferably the wall (1.3, 3.3) of the container is thickened and at least two recesses (1.7) are provided therein from the interior of the container. Device according to claim 1, characterized in that the contact element is a U-shaped profile (2.5, 4.5) on the container wall (2.3, 4.3), the arms of this profile (2.5, 4.5) being longer than the diameter of the tube (2.6) , 4.6) and its width corresponds to the diameter of the tube (2.6, 4.6). Device according to any one of the preceding claims, characterized in that it is a vessel (1.1, 2.1, 3.1, 4.1) excluding the contact surface of the contact element (1.5, 2.5, 3.5, 4.5) for the tube (1.6, 2.6, 3.6, 4.6), provided with thermal insulation on the outer walls (1.4, 2.4, 3.4, 4.4). Device according to any one of the preceding claims, characterized in that the material of the wall (1.3, 2.3, 3.3, 4.3) provided with the contact element (1.5, 2.5, 3.5, 4.5) or the entire container (1.1, 2.1, 3.1, 4.1), is a metal, preferably aluminum or copper. Device according to claim 5, characterized in that the entire container (1.1, 2.1, 3.1, 4.1) is integrally made of metal in one piece. Device according to any one of the preceding claims, characterized in that, in the region of the wall (1.3, 2.3, 3.3, 4.3) provided with the contact element (1.5, 2.5, 3.5, 4.5), there are fastening means for fastening to the tube (1.6, 2.6). 3.6, 4.6) or that it is provided with telescopic legs for resting on a support in the desired position relative to the tube (1.6, 2.6, 3.6, 4.6). Cooling kit for gases, liquids and / or volatiles, characterized in that it comprises a tube (1.6, 2.6, 3.6, 4.6) and a device according to any one of the preceding claims. Use of a device according to any one of claims 1 to 7 for cooling, preferably for freezing, of gases, liquids and / or volatiles passing through a straight tube, in particular in laboratory apparatus. Method of cooling, preferably freezing, of gases, liquids and / or volatile substances passing through a straight tube (1.6, 2.6, 3.6, 4.6), in particular in laboratory apparatus, characterized in that it is connected to this straight tube (1.6, 2.6, 3.6) 4.6) attach or fasten the device according to any one of claims 1 to 7 such that the U-shaped contact element (1.5, 2.5, 3.5, 4.5) surrounds the tube (1.6, 2.6, 3.6, 4.6).