MX2010005882A - Multiautoclave with set of vessels for combinatorial synthesis of zeolites and other materials. - Google Patents

Abstract

A vessel arrangement having a base (22) and multiple vessels (28) suited for simultaneously conducting a plurality of isolated experimental reactions or treatments at atmospheric process conditions or elevated temperatures and pressure condition has been developed. A component of a first material is introduced into one independent vessel (28) through an opening in its top of the first vessel and another component of a second material is introduced into a different independent vessel through its top. Both vessels (28) are removably located about a base (22) at different first locations. Transformation of the components in the vessels occurs to produce different materials therein. After completion of the experiments a displacement medium (44) simultaneously urges the vessels (28) from their respective locations about the base (22). Typically at least one property of the materials from the vessels is determined either within the vessel or after recovery of the materials.

Description

MULTIAUTOCLAVE WITH A SERIES OF TANKS FOR THE COMBINATORY SYNTHESIS OF ZEOLITES AND OTHER MATERIALS FIELD OF THE INVENTION The present invention relates to a tank arrangement having a base and multiple tanks adapted to simultaneously perform a plurality of experimental reactions or treatments isolated under conditions of atmospheric processing, or under conditions of high temperatures and pressures.

BACKGROUND OF THE INVENTION In recent years, new automated methods have been developed for the systematic preparation of new compounds, known as "combinatorial techniques". A wide variety of methodologies, tools and techniques are labeled as combinatorial methods. Generally, these methods seek to accelerate the discovery of new materials and the application of new or known materials to new uses, by increasing the number and speed of material testing through reductions in the size of material samples. A particular type of combinatorial methods is focused on the creation or analysis of dispositions of materials at discrete locations on a substrate of some kind. The substrates often comprise a base that has regions defined by depressions, cells, walls and other structural devices, for Separate the regions and keep the different materials in the isolated arrangements for their synthesis and analysis.

The sizes of the samples of material in the regions are necessarily small, to achieve the objective of such provisions in the combinatorial methodology. Consequently, the diameter of the regions rarely exceeds 15 mm, and generally presents regions of much smaller size. The small size of these regions may imply pollution problems. Pollution, whether detected or not, can interfere with the usefulness of such provisions by corrupting the data obtained from samples of materials, thus producing false conclusions that consume time and resources. Therefore, the reuse of a substrate as a base that receives material directly on its surface requires careful treatment or cleaning, to avoid the presence of any contaminants from previous experiments. Since regions are by definition small, intensive and careful cleaning of small areas can present a challenge. In addition, the composition of the substrate or base can exacerbate the problems. The use of easily convertible or formable materials facilitates the manufacture of small structures on the surface of the base that define the vast number of small regions necessary for such arrangements. However, the materials easily Transformable or formable materials are typically less susceptible to the severe conditions necessary to remove contaminants from small regions.

The synthesis of a multitude of samples of materials in small tank arrangements is already known in the art. For example, it is known to produce various metal oxides in small tanks that are in the form of individual crucibles supported by a base. The use of individual tanks allows their disposal or intensive cleaning once all the experimental steps with the materials contained in them have been completed. However, many of the synthesis operations, processing steps and analysis of a material may require moving the provisions. Thus, on the one hand, the tanks must remain fixed in the base during such procedures which, in addition to moving pieces of equipment, may require agitation within the equipment. But, at the same time, the tank should not be so fixed in the base or substrate that it can not be easily removed for disposal. Placing tanks on a base with little tolerance could prevent them from being removed after concluding the experiment. In addition, certain steps of the treatment may produce minor distortions in the tanks or the base that holds them together at the conclusion of the experiment.

Such conditions occur in the synthesis of various materials. An example of such materials, zeolites, are prepared by what is known as hydrothermal synthesis at temperatures between 100 and 200 ° C, and require crystallization times of one hour or more. For synthesis carried out at temperatures higher than the boiling point of the solvent, it is necessary to use pressure tanks, and these must be suitable for the temperature and pressure used during the operation. This in turn requires sealing the tanks in a way that prevents contamination of the materials that are synthesized.

The synthesis of the zeolites is generally carried out in strongly alkaline media, often at a pH > 14, and the reaction mixture often contains toxic compounds such as, for example, fluorides. Conventionally, syntheses that can be produced at temperatures below 110 ° C are made in polymer bottles, often Teflon ™ (tetrafluoroethylene), whereas reactions at higher temperatures require steel autoclaves, sometimes coated with TefIon ™. A cost-effective combinatorial method for such synthesis is very useful, since the price of an autoclave of this type, with the required safety details, is typically of the order of US $ 1,000. or more. Likewise, such an autoclave weighs 1 kilogram or more, and all these elements represent limitations in regard to the synthesis number that • can be carried out in most laboratories within a year.

The synthesis of zeolites is often carried out by keeping the synthesis mixture at about 100 ° C for at least 6 h. At these moderate temperatures, sealed chambers are necessary in order to prevent the synthesis mixture from drying out. U.S. Pat. No. 3,130,007 A exemplifies the conventional synthesis of zeolites. What all the synthetic processes mentioned, and all the other known synthesis procedures for the preparation of zeolites on a laboratory scale, have in common for the purpose of discovering new zeolites, or to optimize the existing zeolites, is that they are carried out in a cumbersome and expensive way, as it is necessary to prepare each reaction mixture separately, which typically consists of 4 to 7 reagents, and as it is necessary to add the reagents one by one. In many other examples, the synthesis of zeolites and other molecular filters requires temperatures well above 100 ° C, making necessary steel pressure tanks or the like.

Patent application WO 02/07873 discloses new combinatorial techniques that can be used for synthesis in liquid phase, at temperatures of more than 100 ° C, in the sense that it describes the synthesis to be carried out in a hermetically sealed tank at high pressures . Exists, for example, a known design called "multiblock", see Krchnak, V .; Vagner, J. Peptide Res. 1990, 3.182, consisting of i) a Teflon ™ block holding 42 reactors, polypropylene syringes equipped with polymer filters, ii) a vacuum adapter connecting each reactor with a vacuum line (not described in detail), and allowing rapid washing in a device for continuous flow, iii) two Teflon ™ plates with 42 plugs in which the Teflon ™ block is fixed during use, and iv) a cover glass that is used during homogenization. The problem with this design is that the reactors, which are made of glass and lack protective side walls, can only be used at low pressures, and not with strongly alkaline solutions.

Until recently, there was no literature describing methods or equipment to use provisions that could be used in practical work to sufficiently retain the tanks in the arrangement to carry out combinatorial experimentation, but also allow the tanks to be easily removed for replacement in the substrate or base. The synthesis of zeolites can be particularly problematic, since such synthesis requires, almost without exception, hydrothermally treating a solution or gel with a relatively high water content, and often high contents of organic compounds in a closed chamber at high temperatures and pressures.

The patent application WO 98/36826 discloses a system for screening synthetic conditions for the preparation of zeolites and other non-carbonic materials that require hydrothermal conditions in the temperature range of between 100 and 250 ° C. Some of the parameters that have been made more profitable with the multi-autoclave of the patent application WO 98/36826 include: a smaller size of the separated reaction chambers and a greater number of reaction chambers; a reduced use of reagents; the automated addition of reagents, for example through a pipetting machine that quickly and accurately adds all possible liquid reagents; and devices that allow automated analysis with X-ray diffraction and the automatic identification of known crystalline phases. The patent application WO 98/36826 also relieves automated equipment for larger series of synthesis, as well as preparation formulations based on mixtures of different liquids / solutions with variable proportions of reagents.

The invention of the patent application WO 98/36826 is a reactor tank by means of pressure and temperature comprising a central block that has a multitude of perforations. The perforations are holes, cavities or other form of permanently sealed openings at one of their ends. A cover is connected to the central block to seal the open ends of the perforations and thus form a multitude of cameras. A sealing device, operatively associated with the cover, forms a pressure seal when a fastening device holds the cover attached to the sealing device, so that the reaction chambers are hermetically sealed. The applications for the invention of patent application WO 98/36826 can be directed, in addition to the synthesis of zeolites, to any field of research and development activities related to products in which at least one production step comprises mixing different liquids, for example, in the fields of organic and inorganic synthesis, paint production, fuel formulation, food industries, etc., and, in addition, applications in clinical tests, dissolution and digestion of acid samples, etc., in that a liquid reagent is added to a liquid or solid, or when a solid is added to a liquid. The invention of the patent application WO / 9836826 is extremely useful in cases where open tanks can not be used, and when it is necessary to operate at temperatures that cause high pressures in the liquid part of the mixture.

The present invention is a breakthrough in the art compared to the patent application WO / 9836826, in the sense that a series of tanks is insured detachably within associated perforations defined by a base. The tanks are constructed with a material that is inert in the reactions or treatments carried out within a synthesis zone, including the conditions of pressure and temperature that can occur when using a substrate or base of any type, from a simple plate to a multi-autoclave. . The tanks, which are each a unit, cover the inside of the perforations, both their interior walls and one of their ends. The tanks allow the use of a simple device to extract material from the multi-autoclave, to be replaced with new tanks to minimize contamination from one process to another using the tanks. Optionally, the tanks can be used to weigh reagents such as powders or liquids, to have a greater accuracy. Others have used a coating on specific units of tanks, as in U.S. Pat. No. 4, 554, 136 A, in which a fluoropolymer coating is used to inhibit acid corrosion of the pressure tank walls, US Pat. No. 3,048,481 A, which discloses a refractory liner used within a synthesis gas generator, and U.S. Pat. No. 3, 396, 865 A, which discloses a pressure synthesis tank having a thermally conductive pressure curtain and a chemically resistant and thermally insulating coating within the breastplate, made of a dense and refractory concrete. However, the present invention is unique in its type because it uses a series of tanks to facilitate the extraction of solid products and minimize contamination between processes that use tank disposal.

SUMMARY OF THE INVENTION The present invention makes it possible to form dispositions of materials in amounts suitable for research and development using tanks that are easily maintained at their disposal during the experimentation steps, and the arrangement can be discarded once the experimentation is complete. The present invention solves the problems of using a plurality of small tanks in a method or device, and solves the problems of adequately securing the tanks for handling during experimentation and also removing from the disposal tanks that have become stuck. In one of its forms, the present invention introduces a component of a first material in an independent tank through an opening in the upper part of the first tank, and introduces another component of a second material in another separate independent tank through its upper part. Both tanks are loosely placed on a base at different first places. Then the transformation of the components in the tanks occurs, to produce in these different materials. After completing the experiments, a displacing device simultaneously drives the tanks of their respective placements in the base, to be discarded or reused after any necessary cleaning. Typically, at least one property of the materials in the tanks is still being determined there, or after the materials are recovered.

It is also possible to practice the present invention without using a base per se, by re-entering the component of independent tanks of first and second materials. In this case, one of the independent tanks is detachably located in one opening of a frame in one location, and the other independent tank is detachably placed in another opening of the frame, in a different place. The placements of the tanks and the frame allow the contact of the frame with a portion of each tank. In this form, the present invention also provides a unique gripper surface for contacting a different portion of each of the tanks when they are in place in the frame. By forcing the clamping surfaces in unison to come in contact with the tanks, a clamping contact is created between the tanks and the frame, whereby the positioning of the tanks with respect to the frame is fixed for the manipulation of the provisions during the steps of the experimentation. The components in the tanks are transformed to produce materials for experimentation in the desired arrangement, using one or more steps. After the steps, forcing the first and second fastening surfaces to separate from the first and second tanks allows the first and second tanks to be easily removed from the frame. In most cases, the frame comprises a base with perforations for receiving the tanks, although the frame may simply comprise a grid of openings through which the tanks pass in part.

In another form, the present invention provides a method for forming a material arrangement, when at least one component of a first material is introduced into a first tank; introducing at least one component of a second material in a second tank; and releasably securing the first tank at the first location within a first bore defined by a base, and releasably securing the second tank at the second location within a second bore defined by the base by interaction between a surface of each tank and a wall of its respective perforation. The components in the first tank are transformed into the first material, and the components in the second tank are transformed into the second material. At least a portion of the first material is recovered in isolation from the second material. In a modality of the present invention, at least the first tank is beveled to interact between only a portion of an outer side wall of the first tank and the inner wall of the first bore. In a more limited embodiment of this form, at least a plurality of perforations extends completely through the base, where each perforation retains a tank and the perforations of the plurality are closed at their distal ends to create at least temporarily a bag, by fixing a lower closure to the base covering the distal ends of the perforations, and optionally removing the lower closure allows the at least partial displacement of the tanks by either side of the perforation that fixes them detachably. Optionally, this embodiment of the present invention can provide a displacement means in the form of a series of displacement pins fixed in a pattern that aligns a bolt with each distal end of the plurality of perforations. After removing the lower closure, the bolts move the perforation tanks by contacting an individual bolt with a bottom of each displaced tank, forcing the bolts into the perforations.

The present invention may also comprise a unit containing a multitude of pressure tanks, also referred to as a "multi-autoclave". The multi-autoclave typically it has from 10 to 10,000 or more separate small chambers that hold a tank, each with a typical volume between 0.001 to 10 mi. The multi-autoclave can be composed of a base that has perforations that define the chambers, and optionally extend completely through the base. If the perforations extend partially through the base, a single plate covers the top to maintain the pressure inside the tanks. If the perforations extend completely through the base, a series of plates cover opposite faces of the base. Each tank is detachably secured within a bore of the base, and optionally a thin sheet can be walled between the base and the two plates, to improve the pressure seal.

BRIEF DESCRIPTION OF THE FIGURES Figure 1 is a perspective view of a base with perforations.

Figure 2 is a plan view of the base of Figures 1 and 2.

Figure 3 is a section of the base of the Figure 2 taken throughout section 3-3.

Figure 4 is a perspective view of the bottom side of the base of Figures 1-3.

Figure 5 is a perspective view of a tank for use in the present invention.

Figure 6 is a front view of the tank of the Figure 5 Figure 7 is an optional plug for sealing the tank of Figures 5 and 6.

Figure 8 is a front view of a section of the plug of Figure 8.

Figure 9 is a perspective view showing the base of Figures 1-4, retaining a plurality of the tanks of Figures 5-8.

Figure 10 is a perspective view of an optional cover for sealing the tank and base assembly of Figure 9.

Figure 11 is a perspective view of the assembled base and lid of Figures 9 and 10.

Figure 12 is a sectional view of a base, showing different configurations of the tank and the optional lid for use with the present invention.

Figure 13 is a perspective view of a displacement means comprising a guide and aligned bolts.

Figure 14 is a perspective view of an alternative base configuration with shallow perforations.

Figure 15 is a section representative of the base of Figure 14, which has tanks placed therein and an optional lid configuration.

Figure 16 is a section showing an alternative arrangement for the base section of Figure 15.

Figure 17 is a section of an alternative configuration of base, tank and lid.

Figure 18 is a perspective view showing an assembly of a frame with clamping surfaces, to retain the tanks and perform their simultaneous removal.

Figure 18a is a perspective view of the frame of Figure 18, isolated from the assembly of Figure 18.

Figure 18b is a perspective view of the clamping surfaces of Figure 18, isolated from the assembly of Figure 18.

Figure 18c is a perspective view of the frame of Figure 18, isolated from the assembly of Figure 18 and retaining tanks.

Figure 19 is a representative section of Figure 18, with the clamping surfaces placed in a first position with respect to the frame.

Figure 20 shows the fastening surfaces of Figure 19, placed in a second position with respect to the frame.

DETAILED DESCRIPTION OF THE INVENTION As summarized above, the present invention is a method for forming a material arrangement. The method uses at least a first and second tanks. The tanks will be described later in greater detail. It is preferred to use a larger number of tanks in order to increase the efficiency of the method. You can use eight, sixteen, forty-eight, ninety-six or a larger number of tanks. You can extend the number of tanks to hundreds, thousands, or tens of thousands. The tanks are detached on a base or frame.

Figure 1 shows a perspective view of a modality of a base. The base 22 defines a multitude of perforations with openings 24 in the upper part of the base for receiving tanks. If the base is used at temperatures within a range of 150 to 250 ° C, the base can be made of stainless steel, aluminum, titanium or other rigid material such as polyethylethyl ketone (PEEK) or the like. For use at temperatures greater than 150 ° C, the base 22 can be made entirely of Teflon ™, for use at less than 130 ° C it can be made of polypropylene, and for use at less than 105 ° C it can be made of polyethylene. It is preferred that the perforations be complete or, in other words, that the perforations extend from one surface of the base to a second parallel surface of the base. base. However, and as can be seen in Figure 2, the apertures 24 in the perforation define a passage through the thickness of the base 22, but only one port 26 of smaller diameter to the bottom of the base 22. The port 26 provides a form of release opening for use with a displacement means that will be described later. The difference in the diameters of the openings of the perforations 24 and the ports 26 is shown in Figure 3, as well as the depth of the opening 24 through the thickness of the base 22. Figure 4 shows the opening of port 26 in the bottom of the base 22. Alternatively, the perforations can define cavities that do not have an opening that extends completely through the base. In general, the present invention will be described as the preferred embodiment of a base having perforations with perforation openings in one surface of the base, and ports connecting perforation openings to the other side of the base.

Figure 5 is a perspective view of a typical tank 28 that occupies at least a portion of the perforations in the base. The tanks may conform to the shape of the perforations in the base, and are arranged so that each tank extends to at least one of the perforation openings 24. Figures 5 and 6 show a cylindrical tank 28. The Figure 6 shows the contour of the interior of the tank 28 and an optional depression 32 in the bottom of the tank to assist in the withdrawal of the tank. Each tank has at least a portion of the walls of the drilling opening 24 and covers the bottom of the drilling opening near port 26. Alternative tanks are possible, and will be discussed in detail later. The tank is preferably made of an inert polymeric material such as Teflon ™, polyethylene, polypropylene, ethylene propylene fluorinated with perfluoroalkoxy, and polyethylethyl ketone, which is capable of withstanding the temperatures and pressures necessary for synthetic reactions. The tanks may be constructed of a material transparent to radiation to facilitate further analysis, for example, transparent to infrared radiation, or transparent to X-rays. However, tanks may themselves provide a convenient way to provide a catalytic function to the reaction that occurs inside the tank. For example, the catalyst may be present on the inner surface of the tanks, it may be released from the cavities that are inside the walls of the tanks, it may be released from an adsorbent that lines the walls of the tanks, and the like.

In one embodiment of the present invention, materials are produced in amounts suitable for research and development experiments. For example, the materials They can produce in quantities that vary from milligrams to grams. The tanks in this application can have a maximum internal diameter of 10 mm. In an application of multiple tanks, and typically there are 8, 48, 96, 188 or more tanks disposed loosely on a base.

Tanks provide several advantages over previous equipment, where the most important is the simple device to remove a tank from the base. This allows a greater degree of flexibility, in the sense that different tanks can be grouped for different types of experiments. Another benefit is the ease of extracting solid products from the separate reaction tanks, as opposed to extracting several solid products from a unitary device. Another advantage is the significantly reduced probability of contamination between one process and another using multiple pressure tanks. Small tanks can improve operations by eliminating the need to clean small confined regions on plates, and thereby eliminate the risk of undetected contamination that compromises future experiments. The individual tank can also be used to weigh the reagents or products with a high degree of precision. The tanks also provide an alternative approach to product recovery through the use of ports 26 on the base 22. Tanks containing products of synthesis can be oppressed to remove them from the perforations of the base using an extraction device that is discussed in greater detail later.

At least one component of a first material is introduced into a first independent tank, and at least one component of a second material is introduced into a second tank. The components can be introduced in series to each of the tanks, or simultaneously to the respective tanks. Also, additional components can be added to one or more of the tanks. Several components can be mixed and added to a tank, or they can be introduced into the tank separately. When several components are separately introduced into a tank, the various components can be introduced in sequence or simultaneously. Different or equal amounts can be added to the tanks. The materials can be organic or inorganic. Preferred materials include zeolites, ceramics, composite materials and the like. The term "different materials" includes materials produced from the same components. For example, varying the quantities of the components or the order in which the components are added, even if the identity of the reagents remains the same, could result in different product materials.

Various different techniques can be used to introduce the components to the tanks, such as methods manual or automatic. Preferably, the components are introduced to the tanks in measured quantities, the measurement can be contemporaneous with the introduction, before the introduction, or after the introduction. One mode can use a dispenser such as a pipette, micropipette or powder dispenser. It is preferred that the spout be automatic, although this is not necessary.

The components are transformed, being inside the tanks, into materials that have at least one property that is different from that of the initial component. It is expected that materials transformed between at least two of the tanks have at least one property that is different.

Figures 7 and 8 show an optional cover that can cover the upper part of the tank. Figure 7 shows the outline of a hollow portion 36 inside a lid 34. The lid 34 can be inserted into the opening of the inner portion 30 of the tank 28. The lid 34 can be formed with a conical end 33 to facilitate inserting the lid 34 into the interior portion 30 of the tank 28. The lid 34 may also have an upper portion 35 to prevent the lid 34 from being fully inserted into the interior portion 30 of the tank 28. A purpose of the lid 34 It is to keep the components and materials inside the tank during its handling, processing and transformation. Other purpose from lid 34 is to close the tank for purposes of maintaining an internal pressure as required for hydothermal synthesis. The lid 34 can be constructed with materials as described above for the tank and the base.

Figure 9 shows a plurality of tanks 28 and lids 34 assembled in a base 22. Figure 10 shows a retaining plate 38 that joins the lids to force the bottoms of the tanks 28 into contact with the bottom of the tank. the respective perforations in the base 22 when assembled with the base of Figure 9 in the assembly shown in Figure 11. The retainer plate 38 may also be operated to force a portion of the lid 34 into the interior portion of the container. Tank 28. Lids can be an integral part of the retainer plate, or the retainer plate can retain a separate lid for each tank that has a lid. The tanks 28 are disposed detachably within the opening of the perforations 24 defined by the base 22. The tanks may be detachably disposed in the base before, during or after the components have been introduced. The tanks can be detached from the base in sequence, at the same time, or in groups. In one embodiment, a perforation does not contain more than one tank. The term "at the base" includes within, above or against the base.

Optionally, the retaining plate 38 can be fixed to the base 22 using tweezers or bolts. The bolts with rope can operate through the perforations in the retaining plate 38 and corresponding perforations in the base 22 to maintain the assembly during handling and processing.

The holding plate has several functions. The retaining plate, in combination with the lids, provides a mechanism for independently sealing each of the tanks in order to keep the materials inside the tanks during mixing operations such as stirring, vibrating, stirring, tumbling, and the like. Also, since each tank is sealed independently, the components can be mixed inside a tank without causing contamination between the different tanks. A possible feature of the present invention that uses one or more retainer plates is that a large number of assemblies can be placed one on top of the other, forming layers of reaction chambers according to the desired capacity. As an example, one can be placed on top of ten other assemblies like those shown in Figure 11. The retaining plate, or lid, or the combination of the retaining plate and the lid can also operate to produce a pressure that prevents that the tanks move rotationally relative to the base, or the retainer plate can operate to prevent any movement of the tanks with respect to the base.

Figure 17 more fully illustrates the use of fasteners in the form of screws 48 that extend through a bore 52 in an upper retainer plate 38 ', a bore 54 in a base 58 defining transverse perforations 60 and a perforation. 56 on a lower retainer plate 46. The screws 48 are joined with the nuts 50 to secure the assembly as soon as the tanks 62 are ready to be sealed. To facilitate working with the tanks before closing the retaining plate 38 ', optional screws 64 can be passed through the perforations 66 and joined with a threaded bore 68 in the base 58 to secure the plate to the base while moving the screws. open ends of tanks 62 at base 58 to the various places required for the experimentation steps.

The present invention is suitable for use with a wide variety of base, retainer plate and tank configurations. Figure 17 also demonstrates the use of tanks 62 with edges 70 extending radially outwardly over the top of the base 58. These edges have a thickness much less than the depth of the tanks 62. By securing the retaining plate 38 With the base 58 the flanges 70 are pressed between the two surfaces in contact, to produce the seal necessary to maintain the pressure in the tanks 62. Preferably, the screws 48 and nuts 50 are positioned in such a manner, and adjust their amount, to obtain a sufficiently and uniformly distributed load to ensure that all the chambers are tightly closed when in use. Additionally, snap-on mechanisms may include springs or the like, which ensures that adequate pressure is maintained. All the assembly can be inside a frame made of a rigid material that ensures a good fit in the outer chambers, besides counteracting the deformation of the plates made of pure Teflon ™ or other ductile material.

Figure 12 also shows the variety of tanks that can occupy the perforations and use the retainer plate as shown in Figures 3 and 17. In place of each tank 28, the base 22 'further defines the ports 26. The plate retainer 38 'retains the caps 34 in the various forms that have been described. The tanks 28a have conical geometries, where a closed end has a diameter smaller than that of the open end, and the tanks 28a are completely contained within the bores of the base 22 ', where the outer surface of the open end of the tank is in contact with the surface of the perforation. Various closure arrangements can seal the tops of the tanks 28a to preserve the Pressure. In its simplest form, the underside of the retainer plate 38"can provide sufficient containment by contacting the proximal face of the base 22 'with sufficient force to seal the perforation retaining the tank 28a. Thinning of sealing material between the two contact surfaces of the base 22 'and the retaining plate 38"can increase the effectiveness of the seal in the perforations retaining the tanks 28a. The holding plate 38"can also produce a direct seal with the upper part of the tank 28a using a cover 34 'integrated in the retaining plate 38' and extending below its lower surface, so that the bottom of the lid 34 ' has direct contact with the edge of tank 28a.

The tanks 28b also have conical geometries in cases where a closed end has a diameter smaller than that of the open end. The tanks 28b, being positioned within the bore, extend beyond the opening of the bore in the base. The portion of the tanks 28b extending beyond the bore 28b produces a protruding region of the tank having a larger outer diameter with respect to the diameter of the bore. The outer surfaces of the tanks 28b are in contact with the opening of the borehole, and the adaptation of such contact to an adequate pressure setting inside the perforations allows friction forces to operate against rotation or any other movement, such as translatory movement of the tanks during the experimentation steps. However, the retainer plate or covers can also be used to prevent contamination, or to contain materials inside the tank during mixing. The tanks 28c, 28d, 28e and 28f have a cylindrical geometry. The tanks 28c, 28d and 28F, being positioned within the perforations, extend beyond the opening of the bore in the base. The retaining plate 38"can contact the tops of some or all of these tanks to prevent them from moving within the borehole and, if desired, produce a pressure seal between the edge of the tanks and the bottom of the bore. retaining plate 38". Although not required, any of the cylindrical tanks can be adjusted under pressure within the boreholes, as described above for the conical tanks, to restrict rotation or any other movement. For example, tank 28c may undergo a slight press fit on base 22 'when inserted into a bore to maintain its position. The tank 28d can be adjusted relatively loosely in its respective bore, and contact with the surface of the retainer plate 38"used to keep it placed inside the base 22 ', the tank 28f is a two-piece tank, comprised by a lower disc 72 in combination with a detachable side wall in the form of a sleeve 74. The sleeve 74 rests on a bottom at least partially closed 76 from the perforation. The pressure of the holding plate 38"against the upper part of the sleeve 74 forces the contact with the disc 72, so that the side wall section and the bottom section operate as a unitary tank, optionally having a seal in the upper part of the sleeve 74 with the lower side of the retaining plate 38".

As with the unit tanks, the tank 28f may be contained within the perforation, or may extend beyond the perforation, as shown. As shown, the perforation of the base 22 'completely contains the tank 28e, so that the adjacent cover 14' is partially inserted into the bore to contact the edge of the tank 28e.

Using any tank, adjusting the pressure tanks, adding components to the tanks, deforming the tanks when sealing them, exposing them to pressure and temperature conditions during experimentation, and other procedures, will create the need to extract the tanks from the base. The tanks housed inside a perforation can be extracted from the base using a means of displacement. One form of such a medium is an extraction tool like the one shown in Figure 13.

Extraction tool 40 has a guide 44 for positioning the bolts 42 in alignment with the ports 26 of the perforations or transverse perforations 60 in order to separate the tanks from the perforations. The extraction tool 40 produces a simultaneous separation of the perforation tanks. In one embodiment of the present invention, the extraction occurs by placing a base of the type shown in Figures 1-4 or 17, which contains tanks 28 or 62 inside the perforations, on the extraction tool, and forcing it downwards to that the bolts 22 enter the open hole or ports 26 and contact the tanks 62 and 28. The continuous force causes the tanks to separate from the holes in the base.

Many alternative ways of moving means to extract more than one tank from the perforations at a time are within the scope of the present invention. For example, another form of mechanical means of movement could manually and mechanically trap at least a portion of several tanks around the surface of each tank, to extract the tanks held from their respective perforations. If a tank is formed of a relatively soft material, such an extractor could use an arrangement of hooks or perforating devices to penetrate an inner or outer surface of each tank as it moves towards the block, and then extract simultaneously the attached tanks. Other forms of mechanical means of displacement can hold an edge, flange or other member of the tank to extract it from the base. For example, a series of thin members can be slid under the edge 70 of the tanks, as shown in Figure 17. In one of its forms, this extraction device can simply comprise a flat plate-shaped extractor with enlarged openings which can be adjusted around the outer edges of the edges 70, of adequate thickness to slide under the edges 70 when pushed against them to lift the tanks of the base with the plate. Such surface or electromechanical fluidic displacement means may also have utility in the present invention. For example, if ferrous tanks are used, a magnetic field can produce the displacement means to attract or repel the tanks of a block. More simply, the displacement means may comprise a compressed gas, such as air, which is supplied to one side of the perforations 60 or ports 26. An open chamber sealed around the lower perimeter of a block 22 can supply the air. Alternatively, an additional block 22 with the shape shown in Figure 4 can function as a collector, which upon contacting the underside of a block with the underside of a similar block 22 supplies compressed gas from its ports 26 to ports corresponding 26 of the similar block to remove the tanks from the perforations that hold them. Similarly, block 22 can function as a vacuum manifold by placing its bottom over the top of a similar block 22 that holds the tanks, and forms a vacuum between the tanks and ports 26 by keeping the two blocks in contact at least partially sealed. Forming the vacuum can simply dislodge the tanks, and extraction with an additional displacement means or maintaining the vacuum between the tanks and ports 26 can allow the complete removal of the tanks when removing the block 22. In this way, the displacement means it can comprise any effective force supplied to the tanks to carry out the extraction displacement of more than one tank at a time.

The arrangement of the tanks does not need to be significantly extended within a perforation, or even to enter it, to utilize the present invention. Figures 14 to 16 illustrate shallow depressions 80 with optional perforations 82, or simply perforations 84 in different regions of the base 78. The depressions 80 and perforations 84 can retain tanks 86 or 86 '(shown in outline) placed in the regions. The size of the perforations 80 can allow a snap fit with the outer wall of the tanks 86 to retain them on the plate. Pass compressed gas through the perforations optional 82 may also function as a displacement means for ejecting tanks 86 from depressions 80. Alternatively, placing tanks 86 with a relatively loose fit within depressions 80, and then forming and maintaining a vacuum through optional perforations 82 , can produce the holding force for the tanks. In such an arrangement, releasing the vacuum through the perforations 82 also releases the tanks, so that the absence of the vacuum functions as a means of displacement. The use of the vacuum travel means can eliminate the need to have depressions 80, when it is possible to produce sufficient retention by simply forming the vacuum through the perforations 84 to create sufficient force to retain the tank 86 'directly on the surface of the vessel. base 78.

To use another form of displacement means, the tanks 86 or 86 * may comprise a ferrous material, and the space of the perforations 82 or 84 may function as contact points in an electromagnet array that may contain the tanks 86 or 86 ' on the base until the tanks are released by turning off the power supply of the magnets. In another embodiment, the base 78 may comprise an electromagnet to retain the ferrous tanks, which eliminates the need for perforations or depressions.

Figure 15 shows a section that further illustrates the above description of the interaction of the tanks and the base, together with additional forms of means of displacement. On the right, Figure 15 shows a tank 86 'retained on top of the base 78 when connecting it to the vacuum source through the bore 84. Then, to the left in Figure 15, a tank 86 resides in a depression 80. Again, the tank 86 may have a snap fit with the depression 80, in which case the perforation 82 may accommodate a mechanical or pneumatic displacement means for forcing the tank 86 and several tanks similarly located outside the depression 80. when so desired. Alternatively, the tank 86 can be adjusted relatively loosely in the depressions 80 ', and not having the optional bore 82 retains the tanks 80 in a press fit as previously described, and the bore 86 can retain the tank 86 selectively in its place with emptiness or another means. An inclined holding plate 90 contacts the top of the tanks 86, and holds them in the depressions 92. Securing the inclined holding plate 90 by the threaded bolt 94 in the threaded bore 96 of the base 78 provides additional stability to the assembly of base and tanks to transport or shake the materials contained in these, and can also produce a sealing of the tanks for operations Pressure. The retaining plate 90, in combination with the depressions 92, can supply another form of mechanical displacement means, by unscrewing from the base 78 using the plate 90 to simultaneously tilt two or more tanks out of the depressions 80 ', thereby that the need for any other means of displacement is eliminated.

In a manner similar to that described above, it is also possible to use the same displacement means to extract relatively rigid tanks from a relatively flexible, and preferably elastic base, where the base allows almost all the deformation necessary to retain the tanks in a press fit. . In such an instance, releasing the tanks, while possibly using many of the different means of displacement described above, may simply require joining and tilting the tanks of the base using a grid to produce simultaneous contact with the tanks. Examples of such grids, which will be described later, are a frame 120 or retaining plate 108, which can be joined with the upper portions of the tanks to tilt them from the base.

The holding plate 90 may also include ports 98 for communicating fluids with the tanks 86. A plenum chamber 100, screwed or welded onto the part The upper part of the retaining plate 90 can produce a sealed chamber 102 for communicating or evacuating fluids from the tanks 86. By producing vacuum in the chamber 102, the retaining plate can function as a displacement means by vacuum allowing the simultaneous raising of the tanks 86 of the depressions 80 '. The chamber 102 can also supply fluids to treat or test the materials in the tanks 86. The plenum can be divided with individual pipes for each divided zone, to supply any number of fluids other than groups of tanks 86, or even to tanks 86 individual Figure 16 provides another alternative arrangement for placing tanks 86"directly on top of base 78. Tank 86" has posts 88 at its bottom to be inserted into bore 84 that extends completely through base 78, or the perforation 84 'extending partially to the base. The post 88 may be joined with the perforations 84 or 84 'in a snap fit or loose fit to eject the post with a means of mechanical, pneumatic or other displacement, in case of snap-fit and retention with retention methods. vacuum, magnetic or otherwise susceptible to selective deactivation. Again, a retaining plate 90 'can secure the tanks more firmly to the base using a bolt 94 and a threaded bore 96. addition of the guide plate 104 to join with the sides of the base 78 can further improve the function of increasing stability of the retaining plate 90. The retaining plate 90 ', in combination with the projections 106 coming out of its bottom to tanks 86", can provide another form of mechanical displacement means when unscrewed from base 78 using plate 90 'to simultaneously tilt the poles of two or more tanks to remove them from bores 84 or 84'. retainer 90 'may also include ports 98' for communicating fluids or solids with tanks 86, and may again use a plenum chamber in communication with ports 98 '.

Figures 18, 18a, 18b and 18c illustrate another embodiment of the present invention that utilizes the release of a mechanical retention device to produce the displacement means. Figure 18 shows an assembly 126 of a clamping plate 108 having fastening surfaces in the form of perforations 112 placed on a frame 110 for moving the clamping surfaces to the unison. As shown in Figure 18a, the frame 110 comprises a perforation arrangement 116 in a flat plate 118 supported by side walls 120. Figure 18c shows the tank 114 'occupying all the perforations in the frame 110. The perforations 116 fit comfortably when contacted with a portion of the side walls of the Tanks The size of the perforations allows for easy insertion into, and removal from, the frame 110. The frame 110 may have a hollow interior, as shown in Figure 18a, or may comprise a solid block with perforations extending partially or completely through the base. Generally, the frame 110 will have a bottom plate to prevent the tank from completely falling through the perforations 116. To complete the assembly, the plate 108 rests on top of the frame 110, and the tanks 114 'extend through the frame 110. of the perforations 112, which have sizes that allow them to easily fit over the tanks to contact a portion of their side walls.

Figures 19 and 20 show the relative positioning of the frame 110 and the holding plate 108 to retain and release the tanks 114 '. Figure 19 shows the release position, where the perforations 122 of the holding plate 108 are aligned relatively concentrically with respect to the perforations 116 of the frame 110, to allow easy insertion and removal of the tanks 114 '. Placing the frame 110 and plate 108 in this manner allows the tanks 114 'to be inserted individually or collectively into the assembly 126 through the perforations 122 and 116. As the tanks 114' are put into the assembly, they rest on a holding plate optional. The simultaneous extraction of several tanks 114 'of the assembly 126 is performed by removing the lower plate 124 or lifting the assembly 126 to leave the tanks 114' on the lower plate 124. The effectiveness of the pinching action of the plate 108 and the frame 110 to retain the tanks 114 'allows the perforations 122 and 116 to be dimensioned in such a way that the tanks 114' no longer adhere or stick inside the assembly 126 when it is placed to release the tanks, as shown in Figure 19.

After inserting the tanks 114 'in the assembly as shown in Figure 19, placing the plate 108 and the frame 110 in the relative positions shown in Figure 20 retain the tanks in the assembly 120 to move the tanks during the different steps of experimentation. With the tank 114 * in place, sliding the plate 108 to align the perforations 122 in an eccentric arrangement with respect to the perforations 116 causes the clamping surfaces produced by the edges of the perforations 116 to simultaneously contact portions of the tank 114 'in one side, while at opposite edges of the tanks, opposite clamping surfaces produced by the edges of the perforations 122 are simultaneously contacted with portions of the tanks at an opposite point and slightly higher in the tanks. The assembly can use any suitable press for hold the relative positions of the plate 108 and the frame 110 in the holding position, until it is desired to release or remove the tanks 114 'of the arrangement.

The steps used in the transformation of the component or components contained in the tanks can be any of those known in the art. Heat, mixing, stirring, hydrothermal conditions, and the like can be applied. You can use several steps, or just one. For example, it is often desirable to calcine inorganic samples after their synthesis. Additional optional steps are washing, grinding and sieving. Different components can be added between transformation steps. The materials formed can be further processed or analyzed using different techniques, and it is not necessary to treat them as a single arrangement. The materials are retained in the defined matrix which, in a simple way, can be transferred to an automatic unit for changing samples for analysis, for example by X-ray diffraction or IR thermography.

An additional advantage of using independent tanks is that the base is ready to be used again, with little or no cleaning. The residues of the above reactions are removed in the tanks, and the base is virtually free of residues for subsequent synthesis reactions. The general benefits of Advances in the present invention are mainly related to the increase in efficiency to eliminate the synthesized materials, the reduction of contamination, and the increase in efficiency to prepare the devices for a subsequent use. Advances in automated disposal make it possible to simultaneously perform large numbers of synthesis and formulations simultaneously and with greater efficiency, and therefore it will be very useful for all research laboratories in the industry, as well as in research institutions and universities.

Claims (10)

1. A method for forming an arrangement of materials in amounts suitable for research and development experiments comprising: a) introducing at least one component of a first material into a first independent tank through an upper opening of the first tank; b) introducing at least one component of a second material in a second independent tank through an upper opening of the second tank; c) removably placing the first independent tank on a base at a first location, and releasably placing the second independent tank on the base at a second location, where the base provides a plurality of perforations adapted to receive a plurality of tanks at least partially within of the perforation, wherein each perforation has a release end at an end opposite the end of the perforation receiving the tank, and the application of a displacement means at one end of each perforation ejects at least partially a plurality of the tanks of the perforation. opposite end of the perforation to remove at least a portion of the tanks from the base; d) transform the components in the first tank to the first material, and transform the components in the second tank to the second material; e) determine at least one property of at least one portion of the first material in isolation from the second material; and f) contacting the first and second tanks with the displacement means simultaneously ejecting the first and second tanks from their respective first and second locations, where the displacement means is selected from the group consisting of: i) a release guide comprising a plurality of displacement bolts fixed in a pattern aligning at least one bolt with one end of each bore, and contacting each tank with at least one bolt at least partially ejecting each borehole tank; ii) an extractor comprising a plurality of vacuum ports aligned with one or more of the perforations, wherein a surface of the extractor is contacted with at least a portion of the surface of the tank in communication at least partially sealed to effect a pressure reduction inside the tanks when the extractor communicates a pressure reduction to a plurality of vacuum ports, in such a way that the extractor is placed with respect to the base to hold a plurality of the tanks when creating a vacuum at least partial, and the extractor removes the plurality of tanks as the extractor moves from the base; iii) compressed gas, where the application of the compressed gas to one side of the base communicates the compressed gas to one end and ejects at least partially a plurality of the base tanks; and iv) partially raise an interaction of the base with the tanks, to allow the displacement of the tanks with respect to the base, where the tanks are fixed with respect to the base against any movement with respect to the base, at least in part the interaction with when less a portion of an exterior surface of each tank and a surface of the base.

2. The method of claim 1, wherein each tank receives at least two components of material before transforming the components into a material, and after the transformation of the components, the first and second material have at least one difference in their properties.

3. The method of claim 1, wherein at least a portion of the tanks is joined against displacement in any direction and rotation with respect to any axis until contacting with the moving means.

4. The method of claim 1, wherein at least one of the tanks has a protruding edge that encircles its outer diameter, and has a thickness less than the depth of the tank.

5. The method of claim 1, wherein at least the first tank receives at least one component of its respective material before being placed in the base, and preferably a plurality of tanks receive two or more material components before being placed in their places in the base.

6. The method of claim 1, wherein one or more materials are deposited in a tank, and tanks containing one or more materials are inserted in series in perforations of the base.

7. The method of claim 1, wherein the first tank on at least the portion received by the piercing possesses at least one region with dimensions to interfere with a wall of the piercing, and press fit the region of the tank in the pierce joins the tank. with the base.

8. The method of claim 1, wherein the base defines perforations having closed bottoms at least partially, where the first tank comprises a bottom section and a removable side wall section, where the bottom section is contacted with the bottom of the hole, the side wall section is contacted with the side wall section, and the side wall section and the bottom section are forced to contact each other, so that the side wall section and the bottom section function as a unit tank.

9. The method of claim 1, wherein at least a plurality of the perforations extends completely through the base, each perforation retains a tank, and the plurality of perforations are closed at their distal ends to create at least temporarily a space by fixing the lower lock in the base, which covers the distal end of the perforations, and optionally removing the lower lock allows the at least partial displacement of the tanks through one of the sides of the perforation by means of the displacement means.

10. A reactor tank with pressure and temperature comprising: a) a plate; b) a base in which material was removed to define a multitude of cavities, where the plurality of cavities have walls, a series of open ends, and a series of ends closed at least partially; c) a series of tanks associated with the base, positioned in such a way that each tank extends towards a corresponding cavity and covers the walls and the closed end at least partially of the cavity; d) a seal operatively associated with the plate for joining with the base and optionally the tanks, for sealing the series of open ends of the cavities; e) a clamping device acting in concert with the plate and base to join the seal and defining a multitude of pressure-tight reaction chambers; and f) a displacement means operating with activation to at least partially eject at least one tank from the base.