Device for storage gas storage gas, agent for adsorption and retention of methane, complex dicarboxylic acid with copper

 

(57) Abstract:

Usage: the invention relates to techniques for storing gas containing methane as a main component, and also applies to its use as a fuel tank in the vehicle gaseous fuel. The inventive device for storing gas containing methane as a main component, contains a pressure vessel, which can constantly maintain at normal temperature, the input/output hole to provide entrance or exit of gas to be stored, a gas-tight mechanism to maintain the gas in a compressed state inside the vessel and the pressure vessel, which can constantly maintain at normal temperature. In the pressure vessel is placed ORGANOMETALLIC complex having a one-dimensional channel structure. The invention offers improved technology, which at low cost provides greater volumetric capacity of adsorption and gas storage, as well as the best repeatability getaccountinfo characteristics. 4 C. and 20 C.p. f-crystals, 1 tab., 21 Il.

The present invention relates to techniques for storing gas containing methane as a main LASS="ptx2">

To store gas containing methane as a main component, usually as adsorbent propose to use mainly activated charcoal.

However, activated carbon has only limited getaccountinfo ability in relation to its volume. To improve this getaccountinfo capacity per unit volume has also been proposed to produce activated carbon in solid adsorbent, but even in this case, achieved a small degree of improvement. On the other hand, currently available activated carbon /activated carbon with a large specific surface having a relatively large surface area and therefore higher getaccountinfo capacity per unit volume. However, such an improved activated carbons are expensive.

Moreover, in relation to adsorption and desorption of gas activated carbon due to significant changes in the diameter of its pores has increasingly unstable adsorption-desorption characteristics by repeating adsorption and desorption of gas. This means that the activated charcoal creates a problem for re-use.

Summary of the invention

The above objective is achieved by the invention set out in paragraph 1 of the formula. Namely, according to the invention, a device for use when storing gas containing methane as a main component, which includes an opening for entrance and exit of gas to be stored, a gas-tight mechanism capable of maintaining the gas in a compressed state inside the container, pressure vessel, in which it is possible to continuously maintain a normal temperature; the pressure vessel with the contained ORGANOMETALLIC complex having a one-dimensional channel structure.

With the above construction in the pressure vessel of this device is placed ORGANOMETALLIC complex having a one-dimensional channel structure. This is on ORGANOMETALLIC complex, placed in this vessel. This storage is in the form of adsorption and retention of gas in one-dimensional channel structure of the complex and it is possible at normal temperature. In addition, for the release of gas from the device /i.e. desorption of gas from the ORGANOMETALLIC complex/ open, for example, a valve on the output hole to reduce the pressure inside the pressure vessel, through which the gas is desorbed from ORGANOMETALLIC complex and is released from the device for use with a specific purpose. In the above case, the ORGANOMETALLIC complex is compacted to a high density in order to provide a high adsorption capacity. This complex has a higher getaccountinfo holding capacity per unit volume compared to, for example, with the above-mentioned activated carbon.

ORGANOMETALLIC complex preferably contains at least one complex selected from the group consisting of terephthalic acid copper, fumaric acid copper, 1,4-TRANS-cyclohexanecarbonyl acid - copper, biphenyldicarboxylic acid copper, fumaric acid - molybdenum, 1,4-TRANS-cyclohexanecarbonyl acid - molybdenum is expendituresa acid chrome, biphenyldicarboxylic acid - chromium, terephthalic acid, rhodium, fumaric acid, rhodium, 1,4-TRANS-cyclohexanecarbonyl acid - rhodium, biphenyldicarboxylic acid - rhodium, terephthalic acid - palladium, fumaric acid - palladium, 1,4-transtikhookeanskikh acid - palladium, biphenyldicarboxylic acid - palladium, terephthalic acid - tungsten, fumaric acid - tungsten, 1,4-TRANS-cyclohexanecarbonyl acid - tungsten and biphenyldicarboxylic acid - tungsten.

By using the ORGANOMETALLIC complex of the above-mentioned type with its excellent ability to adsorb methane in conditions of high pressure and normal temperature, the gas can be stored efficiently in a relatively limited extent.

Device for gas storage according to the invention can be used in the car on gaseous fuel with the combustion engine running on gas coming from the device for gas storage.

In the car on gaseous fuel is less than the volume of the tank for the fuel gas, the better. In this case, the device for gas storage according to the invention satisfies this requirement, and the car is lsoe space to accommodate other parts of the car, than tank for storing gaseous fuel.

Specifically in this vehicle gaseous fuel in a relatively small volume at a relatively low pressure to store large amounts of fuel gas so that the car could at one time to run a greater distance despite the presence of a compact fuel tank. This improvement will contribute to the popularity of cars on gaseous fuel, which in the end will contribute to the limitation of environmental pollution due to automobile use clean energy.

ORGANOMETALLIC complex used in the vehicle, preferably represents at least one dicarboxylic acid with copper selected from the group consisting of terephthalic acid copper, fumaric acid copper, 1,4-TRANS-cyclohexanecarbonyl acid - copper, biphenyldicarboxylic acid copper, fumaric acid - molybdenum, 1,4-TRANS-cyclohexanecarbonyl acid - molybdenum, biphenyldicarboxylic acid - molybdenum, terephthalic acid - chromium, fumaric acid - chromium, 1,4-TRANS-cyclohexanecarbonyl acid - chromium, biphenyldicarboxylic acid - chromium, teretana acid rhodium, terephthalic acid - palladium, fumaric acid - palladium, 1,4-transtikhookeanskikh acid-palladium, biphenyldicarboxylic acid - palladium, terephthalic acid - tungsten, fumaric acid - tungsten, 1,4-TRANS-cyclohexanecarbonyl acid - tungsten and biphenyldicarboxylic acid - tungsten.

When this feature is possible in the car to use effectively the outstanding ability of the gas storage provided by the above-mentioned ORGANOMETALLIC complex, and to achieve the aforementioned advantages.

With the way gas storage according to the present invention the necessary gas adsorb and retain in conditions of high pressure and normal temperature on adsorption-holding substance that contains as a main component ORGANOMETALLIC complex with a one-dimensional channel structure.

When the above method of storing gas for adsorption and storage use of adsorption-holding substance as a main component includes an ORGANOMETALLIC complex with a one-dimensional channel structure and contains at least one complex selected from the group consisting of tereta the new acid - copper, fumaric acid - molybdenum, 1,4-TRANS-cyclohexanecarbonyl acid - molybdenum, biphenyldicarboxylic acid - molybdenum, terephthalic acid - chromium, fumaric acid - chromium, 1,4-TRANS-cyclohexanecarbonyl acid - chromium, biphenyldicarboxylic acid - chromium, terephthalic acid, rhodium, fumaric acid, rhodium, 1,4-TRANS-cyclohexanecarbonyl acid-rhodium, biphenyldicarboxylic acid - rhodium, terephthalic acid - palladium, fumaric acid - palladium, 1,4-TRANS-cyclohexanecarbonyl acid - palladium, biphenyldicarboxylic acid - palladium, terephthalic acid - tungsten, fumaric acid - tungsten, 1,4-TRANS-cyclohexanecarbonyl acid - tungsten and biphenyldicarboxylic acid - tungsten. Such ORGANOMETALLIC complex, as specified above, adsorbs and holds the necessary gas containing methane as a main component, and this adsorption may occur in conditions of high pressure and normal temperature. This fact re-opened by this inventor. In this way it is possible to effectively use such a remarkable property of this complex.

In addition, this ORGANOMETALLIC complex can be relatively easily obtained from lelee, as can be complex with a relatively high density thanks to its respective molding, the volumetric adsorption capacity can be considerably increased, so that this method also provides an additional advantage in terms of the ability to store gas. In addition, the diameter of pores of the complex is quite stable throughout the structure of the complex. Therefore, this complex can be rid of this problem, the persistence of complex unintentionally other adsorbed gas component than necessary gas component that would result in the deterioration of the frequency of occurrence.

As for the materials for adsorption and retention of methane, also related to the present invention, this substance is produced by mixing a dicarboxylic acid, dissolved in an organic solvent, with a solution containing at least one salt selected from the group of salts of copper, molybdenum, chromium, rhodium, tungsten and palladium. Substance as its main component contains an ORGANOMETALLIC complex having a one-dimensional channel structure.

ORGANOMETALLIC complex used in the material for adsorption and retention of methane produces the at least one salt selected from the group of salts of copper, molybdenum, chromium, rhodium, tungsten and palladium.

ORGANOMETALLIC complex used in the material for adsorption and retention of methane, preferably obtained by mixing a dicarboxylic acid, dissolved in an organic solvent, an additive containing at least one organic acid selected from the group consisting of formate, acetate and trifenatate and propionic acid, and then mixing this mixture with a solution containing at least one salt selected from the group consisting of salts of copper, molybdenum, chromium, rhodium, tungsten and palladium.

In the above, by introducing the additive into the solution of the dicarboxylic acid, it is possible to stabilize the crystal structure, making it possible to control the adsorption capacity. In addition, since the above-described synthesis process is relatively simple, you can get an inexpensive set.

Moreover, by choosing the proper form of dicarboxylic acid to adjust the diameter of the pores, making it possible to obtain the adsorption-holding substance that best corresponds to the properties of this gas.

Racy, consisting of copper formate, copper acetate, copper sulfate, copper nitrate and carbonate of copper. As a solution containing a chromium salt, a salt of molybdenum, rhodium salt, the preferred solution of chromium acetate, acetate molybdenum or rhodium acetate. As a solution containing a salt of tungsten or palladium salt, is preferred to the solution of their acetate or chloride.

The above solutions are inexpensive and easy to handle, which is useful for large-scale synthesis.

Moreover, the ORGANOMETALLIC complex used according to the invention may contain complex biphenylcarbonic acid with copper, obtained by mixing solution biphenyldicarboxylic acid with a solution containing a salt of divalent copper.

The above complex dicarboxylic acid with copper itself is a new substance.

This new complex biphenyldicarboxylic acid with copper hereinafter will be described using as an example of a complex of 4,4'-biphenyldicarboxylic acid with copper

More specifically, based on the measurement of its magnetic susceptibility, believe that this new complex of 4,4'-biphenyldicarboxylic acid with copper has a flat or two-chamber lattice and around the copper ion, connected to each other by their adjacent copper ion through dicarboxylic acid. Copper ions are present in the intersection points a, a, a. . . the lattice. In addition, according to various known structures of complexes of copper /Fig. 15/, obtained by structural analysis modeling on the computer in accordance with the method of molecular dynamics /MD/, many of the above-described two-dimensional structures, as believed to be crystallized so that the corresponding points of intersection of the vertically stacked arrays were vertically flush with the intervals b, b, b, ... between adjacent points of intersection, forming together a one-dimensional channel structure.

In addition, investigated the properties of a new complex of 4,4'-biphenyldicarboxylic acid with copper. As shown by this study, the complex has an adsorption capacity compared to the fuel gases, such as methane, ethane, propane and butane and oxygen, nitrogen, etc. moreover, according to the chest x-ray obtained from it, the distance between neighboring copper ions is approximately /Fig. 16/.

It is assumed that due to the above channel structure of a complex of 4,4'-biphenyldiol is of isomerization, polymerization, oxidation and reduction of various compounds introduced in the channel structure.

A solution of 4,4'-biphenyldicarboxylic acid may contain an additive of an organic acid.

This complex of 4,4'-biphenyldicarboxylic acid with copper can be easily obtained by mixing the solution biphenyldicarboxylic acid with a solution containing a salt of divalent copper. When carrying out this reaction with the introduction of pre-supplementation of organic acids in a solution of 4,4'-biphenyldicarboxylic acid the pH value can be adjusted to bring the specific reaction conditions in accordance with the selected salt of copper, so that it was possible under such mild reaction conditions effective to obtain a complex of 4,4'-biphenyldicarboxylic acid with copper and, in the end get a cheap product.

The organic acid may be at least one kind of acid selected from the group consisting of formate, acetate, triptoreline and propionic acid, and the solvent in the solution containing the copper salt, an alcohol, such as methanol, ethanol, propanol or an organic solvent, such as benzene, toluene, acetonitrile, tetrahydrofuran, dimethylsulfoxide, dimethylformamide, di the mind, selected from the group consisting of formate, acetate, triptoreline and propionic acid, it is hardly possible adverse effects on the above reaction.

For example, even if the copper salt is at least one type of salt selected from the group consisting of fumarata copper and copper acetate, is unlikely to be any inconvenience, which would have led to the destruction of the complex formed biphenyldicarboxylic acid with copper. Incidentally, if the copper salt is an inorganic salt of copper, such as copper sulfate, copper nitrate and carbonate of copper, it is unlikely to have an adverse impact on the above reaction. In addition, the fusion reaction can be carried out without supplementation.

For the above reaction as a solvent in the solution containing a salt of copper, a suitable alcohol, such as methanol, ethanol, propanol or an organic solvent, such as benzene, toluene, acetonitrile, tetrahydrofuran, dimethylsulfoxide, dimethylformamide, hexane, acetone, etc., so that the complex biphenyldicarboxylic acid with copper can be effectively obtained under mild reaction conditions. Therefore, the complex biphenyldicarboxylic acid with copper can be p what isatou also preferred is 4,4'-biphenyldicarboxylic acid.

When using the 4,4'-biphenyldicarboxylic acid becomes possible successful receipt complex biphenyldicarboxylic acid with copper, with a maximum adsorption capacity.

Other features of the invention set forth in the dependent claims. When these additional characteristics can be achieved even more favorable features and results.

According to the above-described various features of the present invention has made possible the creation of a device for storing gas which has a larger volumetric capacity of the gas and the car on gaseous fuel with constructive benefits.

Moreover, it is also possible to create materials for adsorption and retention of methane, which has a higher volumetric adsorption capacity and the best repeatability and which is also cheap and easy to synthesize, and storage of gas, with such features.

In addition, in this method, a gas storage due to the appropriate choice of the form of the dicarboxylic acid component of the complex, possibly high-efficiency gas storage corresponding to the particular type of gas being used.

more detailed descriptions of embodiments of the invention with reference to the accompanying drawings

Brief description of drawings

Fig. 1 is a schematic representation of the vehicle gaseous fuel.

Fig. 2 is a schematic illustrating the proposed structure of the complex of terephthalic acid with copper.

Fig. 3 is a graph illustrating getaccountinfo ability /isotherm adsorption complex/ terephthalic acid with copper.

Fig. 4 is a graph illustrating getaccountinfo ability /isotherm adsorption complex/ fumaric acid with copper.

Fig. 5 is a graph illustrating getaccountinfo ability /isotherm adsorption complex/ 1,4-cyclohexanedicarboxylic acid with copper.

Fig. 6 is a graph illustrating getaccountinfo ability /isotherm adsorption complex/ naphthaleneboronic acid with copper.

Fig. 7 is a graph illustrating getaccountinfo ability /isotherm adsorption complex/ phenylenecarbonyl acid with copper.

Fig. 8 is a graph comparatively illustrating gazoadsorbtsionnoi ability /adsorption isotherms complex/ terephthalic acid with copper, various molded products, and activated charcoal.

Fig. 9 is a graph comparatively illustriert and activated carbon, depending on the temperature.

Fig. 10 is a graph comparatively illustrating gazoadsorbtsionnoi ability /Isobar adsorption/ per unit volume of complex terephthalic acid with copper and activated carbon, depending on the temperature.

Fig. 11 is a graph illustrating the adsorption capacity of fuel gas /isotherm adsorption complex/ terephthalic acid with copper.

Fig. 12 is a graph illustrating the adsorption capacity of fuel gas /isotherm adsorption complex/ fumaric acid with copper.

Fig. 13 is a graph illustrating getaccountinfo ability /isotherm adsorption complex/ fumaric acid with copper for other gas.

Fig. 14 is a graph illustrating the distribution of the diameter of pores in the complex of terephthalic acid with copper

Fig. 15 is a schematic three-dimensional structure of a complex of 4,4'-biphenyldicarboxylic acid with copper.

Fig. 16 is a graph illustrating a powder x-ray complex of 4,4'-biphenyldicarboxylic acid with copper.

Fig. 17 is a graph illustrating the distribution of the diameter of pores in the complex of 4,4'-biphenyldicarboxylic acid with copper.

Fig. 18 - adsorption capacity for methane /isotherm adsorption/ion capacity of fuel gas /adsorption isotherms complex/ 4,4'-biphenyldicarboxylic acid with copper.

Fig. 20 is a graph illustrating gazoadsorbtsionnoi ability of oxygen and nitrogen /adsorption isotherms complex/ 4,4'-biphenyldicarboxylic acid with copper, and

Fig. 21 is a graph illustrating the adsorption capacity for methane complexes, respectively, fumaric acid with molybdenum, terephthalic acid with molybdenum and cyclohexanedicarboxylic acid with molybdenum.

Description of the preferred embodiments of the invention

Next will be described the preferred embodiments of the invention with reference to the accompanying drawings.

In Fig. 1 schematically shows a vehicle gaseous fuel 2, equipped with a device for the storage of gas according to the present invention. This car gaseous fuels 2 contains the fuel tank 1 in the form of a device for the storage of gas according to the invention and the engine 2 in the form of an internal combustion engine that receives natural gas from the fuel tank 1 storing the gas, mixing the gas with the necessary combustion oxygen-containing gas such as air/ and creates the driving force for movement of the vehicle as a result of combustion of this gas mixture.

Fuel tank 1 contains the tank, can enter and exit from it, Near each output and input holes are arranged valves 6, forming a gas-tight mechanism for maintaining gas under high pressure inside the pressure vessel 4. On the respective filling station 7 of the fuel tank 1 under the pressure of the fill gas, used as fuel. Needless to say that this fuel tank 1 with the gas is usually under normal temperature conditions without special cooling. This means that when the temperature in the summer time tank 1 is subjected to relatively high temperatures. Under such conditions, the ORGANOMETALLIC complex relevant to the present invention and described hereinafter, can act effectively, while maintaining a high adsorption capacity in this range of relatively high temperatures /ie 25 - 60oC/.

In the fuel tank 1 is an ORGANOMETALLIC complex of 8 prepared according to the present invention. This ORGANOMETALLIC complex 8 adsorb natural gas /for example, a gas comprising methane as a main component at high pressure and normal temperature. When udaetsya in the engine 3, in which the gas is burned to create the driving force for the car.

Specifically, the ORGANOMETALLIC complex is a complex of terephthalic acid with copper, having a one-dimensional channel structure and density in the pressed equal 1,53 g/cm3/ extruded under pressure of 650 kg/cm2/.

Hereinafter will be described some specific ways of synthesis of the ORGANOMETALLIC complex.

/1/ the Synthesis of ORGANOMETALLIC complexes

ORGANOMETALLIC complex used in the present invention has a one-dimensional channel structure. A typical example of such a complex is the complex of dicarboxylic acid with copper.

/1/-1. Conditions for the synthesis of complex dicarboxylic acid with copper

Dicarboxylic acid is dissolved in an organic solvent, in which for pH control as an additive is injected organic acid /this Supplement is obligatory in the case of copper formate, copper carbonate or copper acetate/. In this solution dropwise submit a solution of copper formate or acetate of copper. This mixture of solutions leave from several hours to several days, and solid, drop it in the desired chemical compound.

As the dicarboxylic acid, you can use any of the following acid: terephthalic acid, fumaric acid, 1,4-TRANS-cyclohexanecarbonyl acid, 2,6-naphthaleneboronic acid, 1.4-naphthalenedione acid, Mukanova acid, 1,4-phenylenediacrylate acid, 1,4-phenyleneoxy acid, adipic acid, subernova acid, biphenyloxy ether dicarboxylic acid, decarboxylations acid, 4,4'-biphenyldicarboxylic acid, etc. Due to the choice of these dicarboxylic acids can adjust the size of the channel.

Of the above acids are preferably terephthalic acid, fumaric acid, 1,4-TRANS-cyclohexanecarbonyl acid and 2,6-natalijagolosova acid. When using these acids can be obtained complex dicarboxylic acid with a large specific surface area and a large adsorption capacity.

As the organic solvent can be used an alcohol such as methanol, ethanol, propanol or an organic solvent, such as benzene, toluene, acetonitrile, tetrahydrofuran, dimethylsulfoxide, dimethylformamide, hexane, acetone, etc. or a mixture of these solvents, which may RA methanol, ethanol, dimethylformamide and the mixture of ethanol and dimethylformamide. These alcohols can easily dissolve substances, but does not dissolve the reaction product. In addition, they are not coordinated in the complex, so that you can easily prevent the formation readsorbing and neuderjimogo complex.

As the organic acid can be used formate, acetate, triptorelin and propionic acid. Of them preferred formate and acetate.

When the synthesis reaction, the reaction temperature may vary from about -20 to 80oC, the reaction is possible at normal temperature.

In addition, with regard to the concentration of substances in the synthesis reaction, the concentration of the dicarboxylic acid must be of 0.005 mol/l 0.1 mol/l, preferably 0.02 mol/l to 0.08 mol/L. At concentrations within the last interval can be obtained particularly satisfactory results. Further, as the above-mentioned substances, the number fumarata and copper acetate copper added as copper salts of organic acids, should be 0.5 - 2 molar equivalents relative to the dicarboxylic acid. If this number is less than the specified interval, it will decrease the output. On the contrary, eslida its relationship with the coordination number of copper /coordinated 2 copper atom/. Moreover, the formation of the complex may facilitate the introduction of an additive of an organic acid in a quantity of about 0.1 to 2.0%, preferably 0.5 to 1.0%. In this case, if the amount of additive is less videopreteen interval, the adsorption capacity will not increase sufficiently. Conversely, if this amount is greater than the specified interval, it is difficult to obtain the desired substance.

Incidentally, the complex biphenyldicarboxylic acid with copper, used according to the invention, is a new complex of dicarboxylic acid with copper, outdoor these inventors. Next will be described the synthesis conditions of the complex.

To obtain this complex biphenyldicarboxylic acid copper solution biphenyldicarboxylic acid with the introduction of a Supplement consisting of at least one kind of organic acid selected from the group consisting of formate, acetate, triptoreline and propionic acid, is mixed with another solution in which at least one kind of copper salt selected from the group consisting of copper formate, copper acetate, copper sulfate, copper nitrate and copper carbonate, dissolved in organic ristola, propanol, benzene, toluene, acetonitrile, tetrahydrofuran, dimethyl sulfoxide, dimethylformamide, dimethylacetamide, hexane, acetone, etc., Then the mixture of the solutions left alone to get complex.

Alternatively, the solution biphenyldicarboxylic acid is mixed with a solution in which at least one kind of copper salt selected from the group consisting of copper formate, copper acetate, copper sulfate, copper nitrate and copper carbonate, dissolved in organic solvents containing at least one kind of solvent selected from the group consisting of methanol, ethanol, propanol, benzene, toluene, acetonitrile, tetrahydrofuran, dimethyl sulfoxide, dimethylformamide, hexane, acetone, etc., Then the mixture of solutions it is possible to obtain the desired complex as a product of its deposition.

This new complex biphenyldicarboxylic acid with copper is used as material for adsorption and retention of gaseous methane. For example, at a pressure of about 30 g/cm2/abs./ complex in powder form could adsorb and hold about 150 NCM3/,

/1/-2. Examples of the synthesis of complexes of dicarboxylic acid and copper

Were made pachislot - copper, 1,4-transtikhookeanskikh acid - copper, 2,6-natalijagolosova acid - copper, p-phenylendiamine acid - copper and biphenyldicarboxylic acid - copper.

[a] Terephthalic acid - copper

/1/ 1.2 g of terephthalic acid when heated, dissolved in a solvent which is a mixture of 800 cm3methanol and 30 cm3formic acid. After this solution was cooled to normal temperature, and then this solution was introduced dropwise to another solution in which 3.0 g of copper formate was dissolved in 150 cm3methanol, and then was left alone for two days. Then the product precipitate was filtered under vacuum and dried 4 hours at 120oC, which was obtained 2.1 g of the complex of terephthalic acid with copper. This substance had a specific surface area of 220 m2/year Measurement NDT method using argon showed that this material had a pore diameter of 6.0 /Fig. 14/. Incidentally, in another dimension by Mr method using nitrogen its pore size was equal to 9.3 in Addition, it was found that for measuring the diameter of the pores in the complex dicarboxylic acid with copper this type is suitable NDT method, as usually considered suitable for a mixture of 400 methanol and 20 cm3acetate. After cooling the solution to normal temperature it dropwise introduced another solution, which is 0.95 g of copper formate was dissolved in 50 cm3methanol, and then was left alone for two days. After that, the product precipitate was filtered under vacuum for 4 h, dried at 110oC, resulting in a received 0,41 g of the complex of terephthalic acid with copper.

/III/ 0,41 g of terephthalic acid when heated, dissolved in a solvent mixture of 250 cm3methanol and 15 cm3formic acid. After this solution was cooled to normal temperature, this solution was dropwise introduced another solution in which 0.50 g of copper acetate was dissolved in 40 cm3methanol, and then was left alone for a few days. After that, the product precipitate was filtered under vacuum for 4 h, dried at 110oC, resulting in a received complex terephthalic acid with copper.

[b] Fumaric acid - copper

/1/ 1.2 g of fumaric acid when heated, dissolved in a solvent mixture of 100 cm3methanol and 12 cm3formic acid. After this solution was cooled to normal temperature, this solution was introduced dropwise other RA is Yan. After that, the product precipitate was filtered under vacuum for 4 h, dried at 120oC, resulting in received of 1.37 g of the complex of fumaric acid with copper.

This substance had a specific surface area equal to 450 m3/,

/II/ 1,74 g of fumaric acid and 40 cm3acetate when heated was dissolved in 100 cm3of methanol, and this solution was dropwise introduced 100 cm3solution of methanol containing 2,98 g dissolved in the copper acetate. Then the solution was left at rest for two days at room temperature. The product precipitate was filtered under vacuum and dried for 3 h at 110oC, resulting in received of 1.37 g of the complex of fumaric acid with copper. In this case, the resulting material had a large specific surface area and manifested adsorption capacity in relation to methane.

/III/ 1,74 g of fumaric acid was dissolved in a solvent mixture of 100 cm3methanol and 8 cm3formic acid. Then the above solution under stirring at normal temperature was introduced dropwise to another solution in which to 3.38 g of copper formate was dissolved in 100 cm3of methanol. After that, leave the solution in>, resulting in received of 1.23 g of the complex of fumaric acid with copper. This substance had a specific surface area equal to 480 m3/,

/IV/ 1,74 g of formic acid was dissolved in a solvent mixture of 100 cm3methanol and 1 cm3formic acid. Then the above solution under stirring at normal temperature was introduced dropwise to another solution in which 3,74 g of copper sulfate /CuS45H2O/ was dissolved in 100 cm3methanol and left at rest for one day. After that, the product precipitate was filtered under vacuum and dried for 4 hours at a temperature of 120oC, which was obtained 0.3 g of the complex fumaric acid with copper.

/V/ 0.58 g of fumaric acid was dissolved in a solvent mixture of 40 cm3methanol and 12 cm3formic acid. Then the above solution under stirring at normal temperature was introduced dropwise to another solution in which 1.0 g of copper acetate was dissolved in 80 cm3of methanol. After that, leave the solution undisturbed for a few days. The product precipitate was filtered under vacuum and dried for 4 h at 110oC, which was obtained 0.3 g of the complex fumaric acid and m is copper had a pore diameter of about 5.4

[c] 1,4-TRANS-cyclohexanecarbonyl acid - copper

/1/ 2,53 g of 1,4-TRANS-cyclohexanedicarboxylic acid when heated, dissolved in a solvent mixture of 100 cm3methanol and 14 cm3formic acid. After this solution was cooled to normal temperature. In this solution under stirring was introduced dropwise to another solution in which to 3.38 g of copper formate was dissolved in 100 cm3methanol, and was then left at rest for one day. After that, the product precipitate was filtered under vacuum and dried for 4 h at 120oC, resulting in a received 1,71 g of the complex of 1,4-TRANS-cyclohexanedicarboxylic acid with copper. This substance had a specific surface area of 480 m3/g and a pore diameter of 4.7

/II/ 2.58 g of 1,4-TRANS-cyclohexanedicarboxylic acid when heated, dissolved in a solvent mixture of 100 cm3methanol and 20 cm3formic acid. After cooling this solution to its normal temperature where stirring was introduced dropwise to another solution in which to 3.38 g of copper formate was dissolved in 100 cm3methanol, and then was left alone for a few days. After that, the product precipitate was filtered under vacuum and dried in techy acid with copper

[d] 2,6-natalijagolosova acid - copper

/1/ 0.40 g of 2,6-naphthaleneboronic acid when heated, dissolved in a solvent of a mixture of 4000 cm3methanol and 5 cm3formic acid. After cooling this solution to its normal temperature where stirring was introduced dropwise to another solution, which is 3.00 g of copper formate was dissolved in 100 cm3methanol, and then was left alone for a few days. After that, the product precipitate was filtered under vacuum and dried for 4 hours at a temperature of 110oC, which was obtained 0.35 g of the complex of 2,6-naphthaleneboronic acid with copper.

[e] p-phenylendiamine acid - copper

/1/ 2.58 g p-phenylendiamine acid when heated, dissolved in a solvent of a mixture of 100 cm3methanol and 2.5 cm3formic acid. After cooling this solution to its normal temperature where stirring was introduced dropwise to another solution in which a 2.00 g of copper formate was dissolved in 150 cm3methanol, and then was left alone for a few days. After that, the product precipitate was filtered under vacuum and dried for 4 h at 110oC, resulting in a received 1.40 g sets the dicarboxylic acid prepared by dissolving 0.25 g of 4,4'-biphenyldicarboxylic acid in a solution of a mixture of 60 cm3of dimethylformamide and 1 cm3formic acid. A solution of copper formate were prepared by dissolving 0.5 g fumarata copper in methanol. Then a solution of copper formate was introduced dropwise and mixed with a solution of dicarboxylic acid, stirring the last at normal temperature. After that, the mixture solution was left at rest for one day, and in the form of sludge received a complex of 4,4'-biphenyldicarboxylic acid with copper. Then the product precipitate was filtered under vacuum and dried for 4 h at 100oC, resulting in a received 0,29 g of 4-4'-biphenyldicarboxylic acid with copper.

B. a Solution of dicarboxylic acids were prepared by dissolving 0.25 g of 4,4'-biphenyldicarboxylic acid in 60 cm3of dimethylformamide. On the other hand, to prepare a solution of copper sulphate by dissolving 0.25 g of copper sulfate /CuSO45H2O/ in dimethylformamide. Then the copper sulfate solution was introduced dropwise and mixed with a solution of dicarboxylic acid, stirring the last at normal temperature. After that, the mixture solution was left at rest for one day, and in the form of sludge received a complex of 4,4'-biphenyldicarboxylic acid with copper. Then the product precipitate was filtered under WAC is Oh acid with copper.

/2/ the Structure of complexes

The presence of a one-dimensional channel structure in the above complexes confirmed by powder x-ray and distribution of pore diameters. Measurement of the magnetic susceptibility found that these complexes have resettodobar two-dimensional structure in which a number of core structures with dicarboxylic acids, coordinated around the copper ion, connected to each other through mutual communication of their neighboring copper ions through dicarboxylic acid. Copper ions are present in the intersection points A, A, A, . . . the lattice. In addition, it is believed that many of the above-described two-dimensional structures must be crystallized so that the corresponding points of intersection of the vertically stacked arrays vertically flush with the clearances B, B ... between adjacent points of intersection, forming together a one-dimensional channel structure /for example, in Fig. 2 shows the proposed structure of the complex of terephthalic acid with copper/. In addition, on the basis of the above results it can be assumed that the diameter of the pore can change with the type of dicarboxylic acid.

/3/ properties of various ORGANOMETALLIC kollichestvo methane, adsorbed on ORGANOMETALLIC complexes obtained by the ways described above, was measured in the interval of absolute pressure 0 - 32 kg/cm3.

The measurement results shown in Fig. 3 - 7. In each of these figures, the horizontal axis denotes the pressure (kg/cm3abs.), and the vertical axis is the number of adsorbed methane, measured at 25oC /ie isotherm adsorption/. This figures is an example /1/ section of /a/ is denoted as a1. Similar notations are used for other examples.

As shown, it was found that all of these complexes of dicarboxylic acid with copper adsorb methane at high pressure and normal temperature (for example, 25oC/.

/3/-2. The dependence of the number of adsorbed gaseous methane from pressure molding

In the case of use of the device for gas storage or in the car on gaseous fuel ORGANOMETALLIC complex obtained as described above, is subjected to molding under pressure to obtain a given value of the density in the molded state. Next will be described the changes that occur in adsorbtsionnykh characteristics as a result of such processes research densities of the corresponding complexes of dicarboxylic acid with copper, molded under pressure, i.e., the complex of terephthalic acid with copper /a1/, fumaric acid with copper /b1/ and complex cyclohexanedicarboxylic acid with copper /c1/. Incidentally, in the study of pressure-dependent formation compared the results when the pressure molding 650 kg/cm2and 250 kg/cm2. However, activated carbon is not formed under the pressure of 650 kg/cm2.

In the following table. 1 shows a comparison of the bulk density of the corresponding substances in the absence of their molding under pressure and density after molding under pressure.

In Fig. 8 shows the changes caused by molding under pressure, getaccountinfo capacity per unit volume of complex terephthalic acid with copper /a1/, fumaric acid with copper /b1/, and activated charcoal. In this figure, the horizontal axis denotes the pressure (kg/cm2abs.) and the vertical axis is the number of adsorbed methane per unit volume. In addition, each graph refers to adsorption and retention of the materials indicated below.

complex terephthalic acid with copper /a1/, not molded under pressure.

complex terephthalic acid with copper /a1/, Ford pressure of 650 kg/cm2.

complex fumaric acid with copper /b1/, molded under a pressure of 650 kg/cm2.

- activated charcoal, not molded under pressure.

the activated carbon molded under a pressure of 250 kg/cm2.

As can be seen from this figure, the complexes of dicarboxylic acid is subjected to molding, high density after molding and have more getaccountinfo ability compared with activated carbon.

When the main objective is the adsorption of methane is preferred that the ORGANOMETALLIC complex had a specific surface area ranging from a few up to 1500 m2/g, preferably 50 to 1000 m2/g, can provide a high adsorption capacity. If the specific surface area of less than a few m2/g, there is a significant reduction of adsorption capacity. On the contrary, if the area of more than 1500 m2/g, decreases the amount of complex.

On the other hand, the diameter of the pores should preferably be in the range of 3 to 13 , and more preferably in the range of 5 to 12 . If this diameter is less than 3 , then there is a significant reduction of adsorption capacity. Nisimoto amount of adsorption of methane on temperature

These inventors investigated the adsorption ability with respect to methane complex fumaric acid with copper in the temperature range 5 - 60oC for use in the car on gaseous fuel, comparing it with the adsorption capacity of activated carbon.

The results of the study shown in Fig. 9 - 10. In each of these figures, the horizontal axis represents temperature, and the vertical axis is the number of adsorbed methane. In Fig. 9 shows the amount of adsorbed methane per unit weight, and Fig. 10 - the amount of adsorbed methane per unit volume. In addition, the icon indicates the results obtained with the complex fumaric acid with copper, while the other indicates the results obtained with activated carbon. In these cases, all materials were in powdered form.

As can be seen from Fig. 9 and 10, with the increase of temperature decreases the amount of adsorbed methane. However, for complex fumaric acid with copper reducing this amount is less than for activated carbon. In addition, the complex fumaric acid with copper initially has a higher volumetric adsorption capacity than activerow barberousse-retaining substance to use in the car on gaseous fuel, in a given volume can store a large number of, for example, automotive natural gas. Or on a smaller scale, you can store the same amount of gas. Therefore, this substance will be very useful for this application.

/3/-4. The adsorption effect in relation to other gases

We also analyzed that are above complexes of dicarboxylic acid with copper adsorption capacity in relation to other gases other than methane.

I Investigated the adsorption ability of terephthalic acid with copper [aII] and complex fumaric acid with copper [bIII] in respect of gaseous hydrocarbons. The results of the study shown in Fig. 11 and 12.

As can be seen from Fig. 11 and Fig. 12, complexes of dicarboxylic acid with copper, as installed, show in General a high getaccountinfo ability in terms of fuel gases.

/II/ in Addition, investigated the adsorption ability of fumaric acid with copper [bV] in relation to gaseous oxygen and hydrogen. The results of the study shown in Fig. 13.

As can be seen from Fig. 13, this complex dicarboxylic acid with copper, as installed, can adsorbiroval copper

a/ the specific surface Area of a complex of 4,4'-biphenyldicarboxylic acid with copper, synthesized in the preceding example, [f] A method Braunauer-Emmett-teller. The study showed that this complex has a specific surface area of 900 m2/,

b/ the Average diameter of pores in the complex of 4,4'-biphenyldicarboxylic acid with copper, synthesized in the preceding example, [f] A method of NDT. As shown in the study, this complex has a pore diameter of equal to 7, 8 (see Fig. 17/.

/ Investigated the adsorption-holding capacity of a complex of 4,4'-biphenyldicarboxylic acid with copper in the ratio of gaseous methane. The results of the study shown in Fig. 18.

As found, this complex of 4,4'-biphenyldicarboxylic acid with copper can adsorb and retain gaseous methane at high pressure and, therefore, can be effectively used as materials for adsorption and retention of gaseous methane.

g/ Investigated the adsorption-holding capacity of a complex of 4,4'-biphenyldicarboxylic acid with copper, synthesized in the preceding example, [f] , in respect of gaseous ethane, propane and butane. Rezultatai can adsorb and hold various gases under high pressure and consequently, it can be effectively used as materials for adsorption and retention of the fuel gas when it is applied in the fuel tank of the vehicle gaseous fuel, etc.

d/ additionally, also investigated the adsorption effect against oxygen and nitrogen. The results of the study shown in Fig. 20. As shown, in addition to the fuel gas, the complex can effectively adsorb and hold various gases, when subject to retention of gases are introduced in a one-dimensional channel structure. Thus, using a complex of 4,4'-biphenyldicarboxylic acid with copper to support various catalysts, it can be assumed that this complex provides a catalytic reaction for various introduced in the gas.

/4/ Other complexes of dicarboxylic acids with metal

/4/-1. Some examples of synthesis of

a/ Fumaric acid - molybdenum

0,597 g /5,14 mmole/ fumaric acid and 1000 g /2,34 mmole/ molybdenum acetate was dissolved in 900 ml of methanol. After stirring the solution for three days at room temperature, it was left alone for a few days. Then the product precipitate was filtered under vacuum, sufficiently washed with methanol and after the substance had a specific surface area, equal 469 m2/year Measurement NDT method using argon showed that the substance has a pore diameter of 5.8 .

b/ Terephthalic acid - molybdenum

0,854 g /5,14 mmole/ terephthalic acid and 1000 g /2.34 mmole/ molybdenum acetate was dissolved in 900 ml of methanol. After stirring the solution for three days at room temperature, it was left alone for a few days. After that, the product precipitate was filtered under vacuum, sufficiently washed with methanol and then dried under vacuum for 4 hours at 60oC, resulting in a received 1,387 g of the desired substance. This substance had a specific surface area equal to 519 m2/year Measurement NDT method using argon showed that the substance has a pore diameter of equal to 5.7 .

c/ Cyclohexanecarbonyl acid - molybdenum

0,885 g /5,14 mmole/ cyclohexanedicarboxylic acid and 1000 g /2,34 mmole/ molybdenum acetate was dissolved in 900 ml of methanol. After stirring the solution for three days at room temperature, it was left alone for a few days. After that, the product precipitate was filtered under vacuum, sufficiently washed with methanol and then dried under vacuum for 4 charnoski, equal to 212 m2/year Measurement NDT method using argon showed that the substance has a pore diameter of equal to 5.2 .

d/ Fumaric acid - chrome

0,597 g /5,14 mmole/ fumaric acid and 0,880 g /2,24 mmole/ chromium acetate (II) was dissolved in 900 ml of methanol. After stirring the solution for three days at room temperature, it was left alone for a few days. After that, the product precipitate was filtered under vacuum, sufficiently washed with methanol and then dried under vacuum for 4 hours at 60oC, resulting in a received 0,805 g of the desired substance. This substance had a specific surface area equal to 183 m2/year Measurement NDT method using argon showed that the substance has a pore diameter of equal to 5.0 .

e/ 1,4-TRANS-cyclohexanecarbonyl acid - rhodium plated

0,885 g /5,14 mmole/ 1,4-TRANS-cyclohexanedicarboxylic acid and 0,517 g /1,17 mmole/ dimer of rhodium acetate

/(Rh2CH3COO)4/ was dissolved in 900 ml of methanol. After stirring the solution for three days at room temperature, it was left alone for a few days. After that, the product precipitate was filtered under vacuum, sufficiently washed with methanol and C is ptx2">

/4/-2. The dependence of the number of adsorbed gaseous methane from pressure

For some ORGANOMETALLIC complexes, obtained by the above-described method, in the range 0-36 kg/cm2measured by weight, the amount of methane adsorbed by them.

The measurement results shown in Fig. 21. In this figure, the icon graphically specifies a set of fumaric acid with copper, o - complex terephthalic acid with molybdenum complex of 1,4-TRANS-cyclohexanedicarboxylic acid with molybdenum. The horizontal axis corresponds to the pressure (kg/cm2abs. ), and the vertical axis is the number of adsorbed methane, measured at 25oC /ie isotherm adsorption/.

As shown, all of these ORGANOMETALLIC complexes, as found, showed good properties by adsorption of methane.

Essentially similar results were obtained for complexes of 4,4'-biphenyldicarboxylic acid - molybdenum, terephthalic acid - chromium, fumaric acid - chromium, 1,4-TRANS-cyclohexane acid - chromium, biphenyldicarboxylic acid - chromium, terephthalic acid, rhodium, biphenyldicarboxylic acid - rhodium, terephthalic acid - palladium fumaric acid - palladium, 1,4 the PTA - tungsten, fumaric acid - tungsten, 1,4-TRANS-cyclohexanecarbonyl acid - tungsten and biphenyldicarboxylic acid - tungsten. However, these results are not shown.

In addition, it was confirmed that the complexes of dicarboxylic acid with tungsten and dicarboxylic acids with palladium on properties to adsorb methane superior to activated charcoal.

The invention may be embodied in other specific forms without departure from its essence or essential features. Therefore, these embodiments of the invention should in all respects be considered as illustrative and non-restrictive. The limits of the invention is indicated rather attached formula than the previous description, and therefore means that it covers all modifications which fall under the concept and limits of equivalence formulas.

1. Device for the storage of gas, including methane as a main component, containing the pressure vessel, which can constantly maintain at normal temperature, the input/output hole to provide entrance or exit of gas to be stored, a gas-tight mechanism capable of maintaining the gas Vij complex, having a one-dimensional channel structure.

2. Device for storing gas under item 1, characterized in that the ORGANOMETALLIC complex is used, at least one complex selected from the group consisting of terephthalic acid copper, fumaric acid, copper, 1,4-TRANS-cyclohexanedicarboxylic acid - copper, biphenyldicarboxylic acid copper, fumaric acid, molybdenum, terephthalic acid - molybdenum, 1,4-transnislegalization acid - molybdenum, biphenyldicarboxylic acid - molybdenum, terephthalic acid - chromium, fumaric acid, chromium, 1,4-transnislegalization acid - chromium, biphenyldicarboxylic acid - chromium, terephthalic acid, rhodium, fumaric acid, rhodium, 1,4-TRANS-cyclohexanedicarboxylic acid, rhodium, biphenyldicarboxylic acid, rhodium, terephthalic acid - palladium, fumaric acid - palladium, 1,4-transnislegalization acid - palladium, biphenyldicarboxylic acid - palladium, terephthalic acid, tungsten, fumaric acid, tungsten, 1,4-transnislegalization acid - tungsten and biphenyldicarboxylic acid - tungsten.

3. Device for storing gas under item 2, characterized in that stdragon solvent, containing a salt of divalent copper.

4. Device for storing gas under item 3, characterized in that the solution biphenyldicarboxylic acid introduced additive containing organic acid.

5. Device for storing gas under item 4, wherein the organic acid is used, at least one acid selected from the group consisting of formic acid, acetate, triptoreline and propionic acid.

6. Device for storing gas under item 3, characterized in that as the copper salt used, at least one salt selected from the group consisting of copper sulfate, copper nitrate and carbonate of copper.

7. Device for storing gas under item 4, characterized in that as the copper salt used, at least one salt selected from the group consisting of copper formate and acetate of copper.

8. Device for storing gas under item 3, characterized in that the solvent in the solution containing the copper salt used, at least one organic solvent selected from the group consisting of methanol, ethanol, propanol, benzene, toluene, acetonitrile, tetrahydrofuran, dimethyl sulfoxide, dimethylformamide, dim is este biphenyldicarboxylic acid used 4,4'-biphenyldicarboxylic acid.

10. Device for storing gas at PP.1 and 2, characterized in that it is used as a fuel tank in the vehicle gaseous fuel.

11. The method of storing gas, characterized in that the desired gas adsorb and hold at high pressure and normal temperature, and adsorbiruya-retaining substance as a main component contains an ORGANOMETALLIC complex having a one-dimensional channel structure.

12. The method of storing gas under item 11, characterized in that as the ORGANOMETALLIC complex is used, at least one complex selected from the group consisting of terephthalic acid copper, fumaric acid, copper, 1,4-TRANS-cyclohexanedicarboxylic acid - copper, biphenyldicarboxylic acid copper, fumaric acid, molybdenum, terephthalic acid - molybdenum, cyclohexanedicarboxylic acid - molybdenum, biphenyldicarboxylic acid - molybdenum, terephthalic acid - chromium, fumaric acid, chromium, 1,4-TRANS-cyclohexanedicarboxylic acid - chromium, biphenyldicarboxylic acid - chromium, terephthalic acid, rhodium, fumaric acid, rhodium, 1,4-TRANS-cyclohexanedicarboxylic acid, rhodium, biphenyldicarboxylic acid - p - alladia, biphenyldicarboxylic acid - palladium, terephthalic acid, tungsten, fumaric acid, tungsten, 1,4-TRANS-cyclohexanedicarboxylic acid - tungsten and biphenyldicarboxylic acid - tungsten.

13. Agent for adsorption and retention of methane, which is obtained by mixing dicarboxylic acid, dissolved in an organic solvent, with a solution containing at least one salt selected from the group consisting of salts of copper, molybdenum, chromium, rhodium, tungsten and palladium, and containing as a main component ORGANOMETALLIC complex having a one-dimensional channel structure.

14. Agent p. 13, characterized in that the ORGANOMETALLIC complex obtained by mixing the dicarboxylic acid dissolved in an organic solvent, with a solution containing at least one salt selected from the group consisting of salts of copper, molybdenum, chromium, rhodium, tungsten and palladium.

15. Agent p. 14, characterized in that as a solution containing a salt of copper, using at least one solution selected from the group consisting of a solution of copper formate, copper sulfate, copper nitrate and carbonate of copper.

16. Agent p. 13, is great for the s with copper, obtained by mixing the solution biphenyldicarboxylic acid with another solution containing the salt of divalent copper.

17. Agent p. 16, characterized in that as the copper salt used, at least one salt selected from the group consisting of copper sulfate, copper nitrate and carbonate of copper.

18. Complex dicarboxylic acid with copper, which is obtained by mixing solution biphenyldicarboxylic acid with another solution containing the salt of divalent copper.

19. Complex dicarboxylic acid with copper under item 18, characterized in that the solution biphenyldicarboxylic acid injected additive containing organic acid.

20. Complex biphenyldicarboxylic acid with copper under item 19, characterized in that the organic acid is used, at least one acid selected from the group consisting of formic acid, acetate, triptoreline and propionic acid.

21. Complex biphenyldicarboxylic acid with copper under item 18, characterized in that as the copper salt used, at least one salt selected from the group consisting of copper sulfate, copper nitrate and carbonate of copper.

22. Complex biphenyldicarboxylic acid the C group, consisting of copper formate and acetate of copper.

23. Complex biphenyldicarboxylic acid with copper under item 18, characterized in that the solvent in the solution containing the copper salt used, at least one organic solvent selected from the group consisting of methanol, ethanol, propanol, benzene, toluene, acetonitrile, tetrahydrofuran, dimethylsulfoxide, dimethylformamide, dimethylacetamide, hexane and acetone.

24. Complex biphenyldicarboxylic acid with copper under item 18, characterized in that as biphenyldicarboxylic acid used 4,4'-biphenyldicarboxylic acid.

Priority points and features:

13.02.95 on PP.1, 10, 11, 15;

13.11.95 on PP.3 - 9, 16 - 24;

13.02.95 on PP.2, 12 - terephthalic acid copper, fumaric acid copper, 1,4-TRANS-cyclohexanecarbonyl acid - copper;

13.11.95 on PP.2, 12 - biphenyldicarboxylic acid - copper;

12.02.96 on PP.2, 12 - ORGANOMETALLIC complexes of metals other than copper;

13.02.95 on PP.13, 14 - magisteriate substance;

12.02.96 on PP.13, 14 - other metal-containing substances.

 

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