DE20101303U1 - Vessel for the synthesis of solvent-based mixtures - Google Patents

Description

-,*" NEYMEYER & PARTNER GbR, patent attorneys · I*··* ! J* * JSOSj Vül^igen-Schwenningen (DE)

¹ A MN/mn *..**.,* *,.* " ** * * January 25, 2001

Applicant ref.: S 073

Applicant: Siegel Helmut, St.-Trudpert-Str. 1,

79189 Bad Krozingen
Applicant No.:

Description: Vessel for the synthesis of solvent-based

Mixtures of substances

Description

The invention relates to a vessel, in particular for the synthesis of solvent-containing substance mixtures by vacuum evaporation, in which evaporation energy is supplied to the substance mixture via the vessel wall and/or the vessel bottom.

In synthesis laboratories in the chemical, biochemical or pharmaceutical industries, solvent-containing mixtures are often synthesized, for example to identify new compounds or to determine process parameters. Synthesis processes are known in which the synthesis includes vacuum distillation, in which evaporation energy is supplied to the mixture via the vessel wall and/or the vessel bottom and the vessels can be placed under a controlled vacuum. This accelerates the synthesis.

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These are achieved at the lowest possible solvent temperature. However, it has been shown that with this acceleration of the distillation rate, a larger amount of heat of vaporization is removed from the solvent-containing mixture during the evaporation process, so that the mixture cools down considerably after a short time.

Since a certain maximum temperature must not be exceeded in such synthesis processes due to the heat sensitivity of the mixture of substances, the highest possible energy supply via a corresponding heating device is also extremely limited in order to safely rule out overheating of the mixture of substances. This in turn means that the heating device is set to the maximum possible temperature via a corresponding control and thus there is always only a relatively small temperature gradient between the heating device and the mixture of substances in the vessel during the evaporation process. Due to this extremely small temperature difference, a correspondingly rapid energy supply to the mixture of substances during the evaporation process is not possible. A reduction in the temperature level to lower process temperatures and a corresponding further reduction in the

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NEYMEYER & PARTNER GbR, Patent Attorneys I i * . . * t &Idigr;* ! JSOSJ V9$ngen-Schwenningen (DE)

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However, reducing the vacuum is also not desirable, as in these cases the evaporating solvent may no longer condense and thus can no longer be recovered. This is because condensation and recovery of the solvent requires a temperature difference of at least 30 Kelvin between the vapor temperature of the solvent and the condensation temperature in order to ensure reliable condensation of the evaporated solvent. This in turn means that with a maximum possible "boiling temperature" of the mixture of substances of, for example, 40 ^° C, a condensation temperature of at most -15 °C must be selected in order to ensure reliable condensation of the solvent even when the mixture of substances cools down during the evaporation process and the solvent vapor cools down as well. On the other hand, the condensation temperature cannot be chosen arbitrarily low, since some solvents also change from the liquid to the solid state at temperatures around the freezing point of 0 ⁰ C and thus condensation and recovery of the solvent is also excluded by this so-called "icing".

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This in turn means that in order to accelerate the synthesis process, the vessel in which the solvent-containing mixture is located should have the best possible thermal conductivity coefficient in order to achieve the best possible energy supply for evaporating the solvent from the mixture.

A number of suggestions for improvement have been made in the state of the art, for example DE 44 19 971 Al, which are concerned with improving heat transfer in the cases mentioned above. The subject of the publication DE 44 19 971 Al is to achieve better heat transfer by designing a bottom with displacement elements. However, these vessels are made of plastic and therefore cannot be used in the conventional sense for all tasks in a synthesis laboratory.

Furthermore, an article has become known from the publication DE 44 13 423 A1, in which the production of laboratory vessels made of sapphire, aluminum or silicon nitride with diamond coating is described. These materials also have a very low thermal conductivity coefficient and are also suitable for the production

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NEYMEYER & PARTNER GbR, Patent Attorneys I ·*··* ! &iacgr; * I {»OS} Viilfcigen-Schwenningen(DE)

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of such a vessel is not without problems, especially with regard to the shape of the vessel.

Vessels made of metallic materials are also used, but due to their non-transparent nature they do not allow observation of the synthesis process and are therefore only used in synthesis laboratories in exceptional cases. However, these metallic materials are known to have a high thermal conductivity coefficient, so that when such vessels are used, relatively good heat transfer occurs even when the temperature difference between the heating device and the vessel is small.

The invention is therefore based on the object of designing a vessel of the generic type, in particular for the synthesis of solvent-containing mixtures of substances by vacuum evaporation, in such a way that the mixture of substances can be synthesized as quickly as possible, in particular the energy supply to the mixture of substances in the vessel can take place quickly even at lower temperature levels.

The object is achieved according to the invention in that at least a portion of the vessel bottom and/or the

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The vessel wall is made of a highly thermally conductive material and forms a separate component that is tightly connected to the rest of the vessel body, which is made of a glass material.

The design according to the invention provides a vessel which is particularly suitable for the synthesis of solvent-containing mixtures of substances by vacuum evaporation. On the one hand, the vessel body made of glass material ensures that the synthesis process is always visually monitored. On the other hand, the vessel base and/or vessel wall, which are made of a highly thermally conductive material at least in some areas, can supply the mixture with a maximum of evaporation energy, so that cooling is reliably excluded, which also speeds up the entire synthesis process. This means that according to the invention, the vessel consists of two materials, namely a glass material as the base material, as is also known from the prior art, and a material with high thermal conductivity. Borosilicate glass, for example, can be used as the glass material, as can be seen, for example, in the company catalog of IKA-Werke GmbH and Co. KG, 79219 Staufen, on page

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61 , where such a vessel of the conventional
The vessel body of the vessel according to the invention can also consist of such a borosilicate glass, while parts of the vessel bottom or the entire vessel bottom or parts of the vessel wall
made of a highly thermally conductive material.
These sub-areas are designed as separate components
which are sealed with appropriate sealing agents
are tightly inserted into the rest of the vessel body.

According to claim 2, this highly thermally
conductive material can be a metallic material. This design enables easy production
guaranteed, whereby metallic materials are also extremely cost-effective.

According to claim 3, the vessel bottom can be flat on the outside
be designed and have a low clearance in the
through the glass body formed by the vessel wall. In the area of this holding section, a corresponding elastic seal is provided according to claim 3, which seals the holding section of the vessel bottom to the vessel wall all around. The elastic seal is designed in such a way that the vessel bottom with its holding section is clamped in the glass body

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Preferably, no further connection, such as a threaded connection or the like, is provided between the vessel bottom and the vessel wall. It is understood that, for example, such a threaded connection or also, for example, an adhesive connection or the like can be provided for vessels subject to high stress.

According to claim 4, the vessel can be essentially cylindrical and a circumferential ring body or a circumferential wall section of the housing base made of highly thermally conductive material can be tightly inserted into its vessel wall. This means that the glass body formed from the vessel wall is divided into two parts by this circumferential ring body.

According to claim 5, the circumferential ring also has a holding section for both vessel wall sections of the vessel wall that protrudes into the glass body formed by the vessel wall, in the peripheral area of which an elastic seal is also provided. Due to the design according to claim 5, the vessel according to the invention is extremely cost-effective and extremely simple to manufacture. Here too, preferably no further connection is provided between the ring body and the glass body.

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so that the ring body with its holding sections is held in the vessel wall sections by a corresponding clamping of the seal. It should also be mentioned here that for extreme operating conditions the ring body can be additionally held to the glass body by threaded connections or adhesive connections.

In order to be able to use the vessel according to the invention as an alternative to existing vessels, the ring body according to claim 6 has the same outer diameter as the vessel wall.

According to claim 7, the seal between the separate components and the rest of the glass body can consist of an O-ring seal or a lamellar seal. This design makes production extremely simple.

According to claim 8, the lamellar seal can be part of a chemically inert coating of the respective separate component. Such a coating made of chemically inert material of the separate component, i.e. the vessel bottom or the ring body, can be necessary, for example, if the material selected for the vessel bottom or the ring body is not chemically inert.

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Due to the chemically inert coating of these components
This reliably prevents a chemical reaction between the mixture of substances in the vessel and the vessel base or the ring body. To simplify production, this chemically inert coating can simultaneously form the actual lamellar seal between the glass body and the ring body or the glass base.

According to claim 9, the components of the vessel made of the highly thermally conductive material can optionally be equipped with technical devices such as sensors,
Heating, cooling elements or ultrasonic probes or
but also any other measuring electronics. This considerably expands the field of application of the vessel according to the invention. For example, the

Provision of a heating element, for example in the form of a Peltier element, in the bottom of the vessel and, on the other hand, cooling elements in the ring body in the simplest way by
Heating and cooling of the mixture of substances in these liquid flows can be achieved in certain areas. Furthermore, mixing or homogenization of the mixture of substances can be achieved by providing ultrasonic probes. No further
Additional equipment or devices are necessary to

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to achieve such mixing in the vessel according to the invention.

The area of application of the vessel according to the invention is also expanded by the design according to claim 10. One or more calibrated

Blind holes can be provided in which, for example, after vacuum distillation, certain amounts of solids are deposited and used for further tests
can be used. Furthermore, the inside of the vessel bottom can also have a concave, conical, spherical or curved inner surface. The corresponding design allows for a targeted deposition of the residual materials on the vessel bottom.

The inventive design of the "glass vessel" with its glass bottom or ring body in the glass wall made of a highly thermally conductive material
A much higher heat transfer rate is achieved, particularly during synthesis, during vacuum distillation compared to conventional glass flasks, so that the end of the process can be reached much sooner.

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NEYMEYER & PARTNER GbR, Patent Attorneys · * **« « &idigr;&idigr; ,*» J8052 VilKngen-Schwenningen (DE) MN/mn *..*'. »**·».*.:!. *..' .!. January 25, 2001

A preferred embodiment of the invention is explained in more detail below with reference to the drawing. It shows:

Fig. 1 shows a first embodiment of a vessel according to the invention with a separate vessel bottom

made of highly thermally conductive material;

Fig. 2 shows a section through a vessel according to the invention in the connection area of the vessel bottom and the vessel wall with an O-ring seal;

Fig. 3 is a further sectional view corresponding to Fig. 2 but with a lamellar seal;

Fig. 4 shows a second embodiment of a vessel according to the invention, in which both the vessel bottom and a portion of the vessel wall are made of a highly thermally conductive material.

stands;

Fig. 5 shows a further embodiment of a vessel according to the invention with a separate vessel bottom and an annular body inserted into the vessel wall, each made of highly thermally conductive

Material.

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Fig. 1 shows a first embodiment of a vessel 1 according to the invention, the basic shape of which corresponds, for example, to the shape of the basic vessel from the company catalog of IKA-Werke GmbH & Co. KG on page 67. It is understood that the shape of the vessel 1 is not limited to the embodiment shown, but can also have any other shape.

The vessel 1 shown as an example has a threaded section 2 at its upper end, onto which a screw cap can be screwed, for example, to close the vessel 1. Radially expanded, a vessel body 4 consisting of a circumferential, cylindrical housing wall 3 adjoins this threaded section towards the bottom. The vessel body 4 is formed in one piece together with the threaded section 2 and is made of a glass material such as borosilicate glass.

A vessel base 5, which is designed as a separate component, is inserted into the underside of this vessel body 4. This vessel base 5 has a substantially flat outer surface 6, with which the entire vessel 1 can be placed on a flat surface. This flat outer surface 6, in its outer contour, is the same as the housing wall 3.

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of the vessel body 4 and has the same diameter as the cylindrical vessel body 4. This means that the vessel body 4 sits with its housing wall 3 on the radial outer ring surface 7 of the vessel bottom 5. Within this radial ring surface 7, the radial width of which corresponds approximately to the wall thickness of the housing wall 3 of the vessel body 4, a holding section 8 is provided which extends cylindrically into the housing wall 3 of the vessel body 4. In its peripheral area, the holding section 8 has a seal 9 which in the embodiment of Fig. 1 is designed as an O-ring seal 10, as can be seen from the enlarged sectional view of Fig. 2.

From Fig. 2 it can also be seen that the holding section of the vessel bottom 5 has a circumferential receiving groove 11 in which the O-ring seal 10 is inserted. A gap 12 is provided between the holding section 8 of the vessel bottom 5 and the circumferential housing wall 3 of the vessel body 4. The diameter of the holding section 8 is thus somewhat smaller than the inner diameter of the vessel wall 3, so that there is a clearance of approximately 0.2 mm between the holding section 8 and the vessel wall 3. This clearance of 0.2 mm

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the vessel base, which is made of a metallic material such as aluminum, is given enough space to be able to expand when heated without any tensions occurring in the vessel wall 3. This in turn means that the vessel base 5 with its holding section 8 is held firmly and replaceably in the vessel body 4 via the O-ring seal 10. The O-ring seal 10 is clamped against the inner wall of the vessel body 4.

Furthermore, it can also be seen from Fig. 2 that the vessel wall 3 of the vessel body 4 rests flat on the annular surface of the housing base 5.

Fig. 3 shows an embodiment of another type of seal in section. In this embodiment, the vessel bottom 5/1 with its holding section 8/1 has a cylindrical outer contour 13 which is designed without any receiving groove. In the embodiment of the housing bottom 5/1, this consists of a non-inert material which could chemically react with mixtures of substances filled into the vessel 1/1 without further precautions. In order to prevent such a chemical reaction, the housing bottom 5/1 has a chemically inert coating 14 towards the interior of the vessel 1/1, for example made of

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PTFE, through which the housing base 5/1 is completely covered to the interior of the vessel 1/1. Thus, the coating 14, which extends to the radial annular surface 7/1 of the vessel base 5/1, reliably prevents a chemical reaction between the mixture of substances in the vessel 1/1 and the housing base 5/1.

To simplify the manufacture of the housing base 5/1 with its coating 14, the seal required between the housing base 5/1 and the vessel wall 3/1 can be formed by a lamellar seal 15. This lamellar seal 15 consists, as shown by way of example in Fig. 3, of several circumferential lamellae extending radially outward from the holding section 8/1. According to the present exemplary embodiment, this lamellar seal 15 can be an integral part of the coating 14, which simplifies manufacture.

Due to the choice of a metallic material with highly thermally conductive properties, an extremely high amount of energy per unit of time can be conveyed into the mixture by means of a suitable heating device, for example during the vacuum distillation of a solvent-containing mixture. This facilitates the vacuum evaporation and thus the overall synthesis of a

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such a mixture of substances is significantly accelerated. Due to the simple removal and the firm hold of the vessel base 5 or 5/1 via its seal 10 or 15 in the vessel wall 3 or 3/1, the cleaning of the vessel 1 or 1/1 is also possible in an extremely simple manner.

Fig. 4 shows a further embodiment 1/2 of a vessel, the basic shape of which also corresponds to the shape of the vessel 1 from Fig. 1. The vessel 1/2 from Fig. 4 also has an upper threaded section 2/2 and a vessel wall 3/2, which also forms a vessel body 4/2. In contrast to the embodiment of Fig. 1, in the vessel 1/2 from Fig. 4 the vessel base 5/2 is provided with a circumferential wall section 16, so that the vessel base 5/2 forms approximately the lower half of the entire vessel body 4/2.

In the upper end area of the wall section 16, this has a holding section 17 with a tapered diameter, which in its design corresponds approximately to the holding section 8 of the vessel bottom 5 from Fig. 1. Accordingly, a seal in the form of an O-ring seal 10/2 is also provided in the area of this holding section 16. The vessel bottom 5/2 is connected to

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its surrounding wall section 16 is firmly and replaceably arranged on the vessel wall 3/2.

Fig. 5 shows a further embodiment of a vessel 1/3, at the upper end of which a threaded section 2/3 is also provided. In the vessel 1/3, the vessel wall 3/3 is divided and separated by a circumferential ring body 18. This ring body 18 is also made of a highly thermally conductive material, as is the housing base 5, which in the embodiment of the vessel 1/3 is identical to the housing base 5 of the embodiment of the vessel from Fig. 1.

The ring body 18 has a holding section 21 or 22 with a tapered diameter for each of the two vessel wall sections 19 and 20 of the vessel wall 3/3, with which the ring body 18 is inserted into the corresponding wall sections 19 and 20. An O-ring seal 10/3 or 10/4 is also provided for the firm and sealing holding of the holding sections 21 and 22 in the respectively associated wall sections 19 and 20, by means of which the wall sections 19 and 20 are held firmly and tightly on the ring body 18 or its holding sections 21 and 22.

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NEYMEYER & PARTNER GbR, Patent Attorneys J ··**··· * «** J78O$Z Vttjingen-Schwenningen (DE) MN/mn ".." "..' "·»"··«· ·· »?· January 25, 2001

Furthermore, the invention provides that different technical devices are integrated into these separate components 5, 5/1, 5/2 and 18, which are made of a highly thermally conductive, preferably metallic material. For example (not shown in the drawing) sensors of all kinds, heating or cooling devices, for example in the form of Peltier elements or ultrasound probes, are provided. By designing these highly thermally conductive components 5, 5/1, 5/2 or 18 with one or more of these technical devices, the vessel 1, 1/2 or 1/3 according to the invention can be used extremely variably for a wide variety of purposes. In particular, when using this vessel 1, 1/1, 1/2 or even 1/3 according to the invention in connection with the synthesis of solvent-containing mixtures of substances by vacuum evaporation, on the one hand the synthesis process can be easily observed through the transparent components of the vessel and on the other hand the mixture of substances in the vessel can be supplied with sufficient evaporation energy via the vessel bottom 5, 5/1 or 5/2 or also via the ring body 18, so that the entire synthesis of the mixture of substances is considerably shortened.

NEYMEYER & PARTNER GbR, Patent Attorneys J &iacgr;.**.»&idigr; ! .** J78052 Viflingen-Schwenningen (DE) MN/mn *·«'"·»* *»·*···· ".. ··* January 25, 2001

Furthermore, in the case of the embodiment 1/3 according to Fig. 5, it can also be provided that heat is supplied to the mixture of substances in the vessel 1/3 via the vessel bottom 5, while heat is removed from the mixture of substances via the ring body 18, i.e. the mixture of substances is cooled via this ring body 18. By controlling the temperature in this way, a so-called convection mixture can be achieved in the mixture of substances via the vessel 1/3, without an agitator or the like, for example in the form of a magnetic stirrer, having to be introduced into the vessel 1/3.

Furthermore, the vessel bottom 5, 5/1 or 5/2 can be made of a magnetic material or have ferromagnetic properties, so that the stability of the vessel is improved overall.

Claims (10)

1. Vessel ( 1 , 1/1 , 1/2 , 1/3 ) , in particular for the synthesis of solvent-containing substance mixtures by vacuum evaporation, in which evaporation energy can be supplied to the substance mixture via the vessel wall (3, 3/1, 3/2 , 3/3 ) and / or the vessel bottom ( 3 , 5/1 , 5/2 , 5/3 ) , characterized in that at least a partial region of the vessel bottom ( 5 , 5/1 , 5/2 ) and/or the vessel wall ( 3 , 3/1 , 3/2 , 3/3 , 16 , 18 ) consists of a highly thermally conductive material and forms a separate component which is tightly connected to the rest of the vessel body ( 4 ) consisting of a glass material. 2. Vessel ( 1 , 1/1 , 1/2 , 1/3 ) according to claim 1, characterized in that the highly thermally conductive material is a metallic material. 3. Vessel ( 1 , 1/1 , 1/2 , 1/3 ) according to claim 1 or 2, characterized in that the vessel bottom (5, 5/1, 5/2 ) is flat on the outside and forms a holding section ( 8 , 8/1 ) which projects with little play into the vessel body (4) formed by the vessel wall, and that an elastic seal (9, 10, 15) is provided in the region of the holding section (8, 8/1 ) between the vessel wall ( 3 , 3/1 , 3/3 ) and the vessel bottom ( 5 , 5/1 ). 4. Vessel ( 1/2 , 1/3 ) according to claim 1, 2 or 3, characterized in that the vessel ( 1/2 , 1/3 ) is essentially cylindrical and that a circumferential wall section (16 ) of the vessel bottom (5/2) and/or an annular body (18 ) made of the highly thermally conductive material is tightly inserted into the vessel wall ( 3/2 , 3/3 ) . 5. Vessel ( 1/2 , 1/3 ) according to claim 4, characterized in that the circumferential annular body ( 18 ) has a holding section ( 21 , 22 ) projecting into the vessel wall sections ( 19 , 20 ) towards both vessel wall sections ( 19 , 20 ) of the vessel wall ( 3/3 ), in the peripheral region of which a seal (10/3, 10/4 ) is provided . 6. Vessel ( 1/3 ) according to claim 4 or 5, characterized in that the annular body (18 ) introduced into the vessel wall ( 3/3 ) has the same outer diameter as the vessel wall ( 3/3 ). 7. Vessel ( 1 , 1/1 , 1/2 , 1/3 ) according to one of claims 1 to 6, characterized in that the seal ( 9 , 10 , 10/2 , 10/3 , 10/4 , 15 ) between the separate component ( 5 , 5/1 , 5/2 , 5/3 , 18 ) and the remaining vessel walls ( 3 , 3/1 , 3/2 , 3/3 ) is formed from an O - ring seal ( 10 , 10/2 , 10/3 , 10/4 ) or a lamellar seal ( 15 ) . 8. Vessel ( 1/1 ) according to claim 7, characterized in that the lamellar seal ( 15 ) is part of a chemically inert coating ( 14 ) of the separate component ( 5/1 ). 9. Vessel ( 1 , 1/1 , 1/2 , 1/3 ) according to one of claims 1 to 8, characterized in that the components ( 5 , 5/1 , 5/2, 5/3, 18) of the vessel (1, 1/1, 1/2 , 1/3 ) consisting of the highly thermally conductive material are optionally provided with technical devices such as sensors, heating or cooling elements or ultrasonic probes . 10. Vessel ( 1 , 1/1 , 1/2 , 1/3 ) according to one of claims 1 to 9 , characterized in that the vessel bottom consisting of the highly thermally conductive material is provided with one or more calibrated blind holes and/or has a concave conical, spherical or curved inner surface.