Adsorbents for separation of nitrogen from a source of gas

 

(57) Abstract:

The adsorbent for separation of nitrogen from a source gas containing at least one non-nitrogen gas, the size of the molecules which are equal to the sizes of molecules of methane or larger than the molecules of methane, the adsorbent comprises clinoptilolite containing sodium ions in a quantity equal to at least 17 equivalent percent based on the total content of the ion exchange cations, and not necessarily nedovarennye cations of one or more species that, if present, constitute in total, less than 12 equivalent percent based on the total amount of ion exchange of cations, and the balance, if any, takes place, is a monovalent cations of one or more species other than the cations of sodium, and has specific sorption characteristics. Adsorbents have high selectivity and good regeneriruemost. 3 S. and 6 C.p. f-crystals, 3 tables.

This invention relates to clinoptilolite adsorbents suitable for separation of nitrogen from gas mixtures with large molecules, in particular methane, and ethylene, ethane, propylene, butane, butene, etc., These adsorbents are designed for use in cyclic psa) and cyclic fluctuation of temperature (thermal swing adsorption - tsa) (see, for example, D. M. Ruthven, ADSORPTION AND ADSORPTION PROCESSES, Academic Press, 1984, and R. T. Yang. Gas separation by adsorption processes. Butterworths, 1987).

In the industry of natural gas is recognized that the reduction of nitrogen content in natural gas (whether the original or nitrogen introduced by injection into emaciated well) represents a serious technical challenge. The predominant today, the way to solve this problem is by using cryogenic separation, suffers from disadvantages such as high capital and labor costs. The separation of the cyclic adsorption offers a potentially cheaper solution.

The main problem hindering the development process for nitrogen removal from natural gas using cyclic adsorption is the loss of suitable adsorbent selectivity to nitrogen with respect to methane. The well-known cyclic processes of adsorption, such as, for example, air with a high oxygen content (see D. W. Breck, ZEOLITE MOLECULAR SIEVES, Jhon Wiley and Sons, 1974), based on adsorbents with energy or equilibrium selectivity to one or more components of the gas mixture to be separated. Conventional microporous adsorbents altami with respect to methane (the main component of natural gas) relative to the nitrogen. Although they provide a potential means for removal of nitrogen from natural gas, the energy costs associated with the release of adsorbed methane, would be economically unacceptable.

Alternative means of obtaining selectivity of the adsorbents is the attempt of separating molecules on the basis of the size of their molecules. Nitrogen less methane from the point of view of its kinetic diameter and a critical value van-der Waals forces. (see D. W. Breck, ZEOLITE MOLECULAR SIEVES, Jhon Wiley and Sons, 1974. p.636). Consequently, the adsorbent with the same pore size, so that the nitrogen molecules, which have smaller dimensions, he adsorbing would be much faster than the molecules of methane, which have large dimensions. Such material would have a kinetic selectivity of adsorption of nitrogen with respect to methane and would be suitable for use for the removal of nitrogen from natural gas using psa.

T. C. Frankiewicz and R. G. Donelly (Chapter 11, INDUSTRIAL GAS SEPARATIONS, American Chemical Society, 1983) found that, as the mineral clinoptilolite (existing in nature and with a high content of zeolite), and clinoptilolite containing calcium ions, introduced as a direct result of ion exchange, are kinetic selectivity to nitrogen relative to the zhota from methane by the psa method is technically feasible in the case when using a suitable short time cycle. However, if used too long a time cycle, on the clinoptilolite was adsorbirovannoi more methane than to nitrogen. It showed that the zeolite had only speed selectivity to nitrogen in the presence of equilibrium selectivity to hydrocarbon component.

K. lgawa with co-authors (ADSORPTIVE SEPARATING AGENT, Japanese Patent 62-132,542) first showed that clinoptilolite replaced with ions of a calcium in a ratio of CaO/Al2O3in the range of from 0.40 to 0.75 useful for the selection of molecules with kinetic diameters less 3,70 from mixtures containing molecules of large size. It was demonstrated separation of nitrogen and methane using this method.

Further, C. C. Chao (SELECTIVE ADSORPTION OF NITROGEN ON MAGNESIUMCONTAINING CLINOPTILOLITES, European Published Patent Application No 437027) for the first time found that clinoptilolite containing at least five percent of the cations, which can be subjected to ion exchange (as defined in the specified patent), such as magnesium ions, were suitable for the separation of molecules whose size is equal to or smaller than nitrogen molecules, from molecules that are larger than the sizes of the molecules of nitrogen. In this patent the first described propno, produce suitable adsorbents for the above separation.

In the discussion above related publications clinoptilolite, discusses the issues associated mainly with obtaining adsorbents with high speed selectively to nitrogen with respect to methane. However, in the cyclic release of nitrogen from natural gas using psa should also pay attention to methods of regeneration of the adsorbent. In psa-cycle gas mixture to be split, pass through a layer of selective adsorbent at high pressure. Nitrogen is preferentially adsorbed layer, the result is a product with low content of this component. After adsorption for a certain period of time the gas to the layer of adsorbent stop, and the nitrogen adsorbed on the layer, is removed by means of reduced pressure. This restores the ability of the adsorbent to further remove the nitrogen. The effectiveness of such regeneration depends on the magnitude of the reduced pressure on the layer of adsorbent, and the forces of interaction between adsorbent and adsorbate. For tightly bound adsorbates to fully restore the regenerative capacity of the adsorbent may be required extremley, which is necessary for regeneration, obtained using the equilibrium adsorption isotherms of the studied system.

In the well-known psa processes using equilibrium selective adsorbents (e.g., air separation), in addition to reducing pressure to facilitate regeneration, often use a small fraction of the received gas to flush more strongly adsorbed gas from the bed of adsorbent. However, using adsorbents with high speed selectivity to nitrogen for nitrogen removal from natural gas, this choice is not suitable, because the methane molecule is adsorbed more strongly than nitrogen. Thus, in this case, regeneration is possible only by reducing the pressure. The energy associated with the vacuum regeneration, are significant and may even be excessive if it is a pressure less than, for example. 0.1 bar. Therefore, a complete regeneration of the adsorbent may be inefficient from the point of view of cost and increase as the layer thickness, and inventory of adsorbent.

It was found that clinoptilolite obtained according to the methods described in previous publications, and all others need kinetic high level of regeneration when using these materials is impossible, if you do not apply a high vacuum.

In the present invention are disclosed methods of making clinoptilolite with high speed selectively to nitrogen with respect to methane and improved regeneration properties. As previously reported, clinoptilolite get cationic exchange of the mineral clinoptilolite. However, we found that the content of divalent cations that can be exchanged, such as magnesium and calcium, can be reduced to a minimum in the clinoptilolite to improve regeneration in the psa process while maintaining or improving high-speed selectivity of mineral nitrogen. High-speed selectivity in these materials is influenced by regulating the relative quantities of monovalent cations in the clinoptilolite.

Thus, in accordance with one aspect, this invention relates to an adsorbent for separation of nitrogen from a source gas containing at least one non-nitrogen gas, the size of the molecules which are equal to the sizes of molecules of methane or larger than the molecules of methane, the adsorbent comprises clinoptilolite, in which the content of sodium ions is at least 17 equivalent percent based on the total content of ionoobmenom, total $ less than 12 equivalent percent based on the total amount of ion exchange of cations, and the balance, if any occurs, is one or more monovalent cations other than sodium cations.

In accordance with a second aspect, this invention relates to a process for the preparation of the adsorbent for separation of nitrogen from a source gas containing at least one gas other than nitrogen and having the dimensions of molecules equal to the size of molecules of methane or greater than the size of the methane molecule, and the method includes carrying out at least one ion exchange of clinoptilolite with a solution containing a monovalent cation to obtain clinoptilolite containing sodium ions in a quantity equal to at least 17 equivalent percent based on the total number of ion-exchange cations, and not necessarily the one or more neodnopodnykh cations, which, if present, constitute in total, less than 12 equivalent percent based on the total amount of ion exchange of cations, and the balance, if any occurs, is one or more monovalent cations other than sodium ion.

In accordance with a third one of Egypt, other than nitrogen gas, the size of the molecules which are equal to the sizes of molecules of methane or larger than a molecule of methane, the process includes contacting the source gas with clinoptilolite adsorbent to obtain a product gas with a lower nitrogen content relative to another gas or other gases, compared with the source gas, and the adsorbent contains the sodium ion in an amount equal to at least 17 equivalent percent based on the total content of the ion exchange cations, and not necessarily the one or more neodnopodnykh cations, if present, total $ less than 12 equivalent percent based on the total amount of ion exchange of cations, and the balance, if any occurs, is one or more monovalent cations other than sodium ion.

Preferably, the content of sodium ion has a value in the range from 17 to 95 equivalent percent based on the total amount of ion exchange of cations,

More preferably, the content of sodium ion has a value in the range from 26 to 80 equivalent percent based on the total amount of ion exchange of cations.

Single-shaft is UP>, HN4+TO+, Rb+Ce+.

The method used to modify clinoptilolite, includes obtaining intermediate materials, which contain mainly cation of only one type (hereinafter in the description they will be called domainname clinoptilolite). However, you can apply other methods of obtaining the necessary content of cations in the clinoptilolite, which are known qualified personnel.

Homoine clinoptilolite get re cationic exchange mineral clinoptilolite with aqueous solutions of salt, the cation of which is subject to introduction. This salt may be chloride or other suitable salt of the metal, which is subject to the introduction. Hominy intermediate material is then used to obtain clinoptilolite containing cations, mainly, of two or more types, with additional cation-exchange capacity (using aqueous solutions of salts, as described above). Finally, clinoptilolite is subjected to heat treatment (activation) for the dehydration of the zeolite. This activation is necessary for obtaining the micropores of clinoptilolite available for adsorption of nitrogen or methane. In addition, this asset is to Vergata ion exchange, in materials containing them instead of hydrogen ions.

The original mineral clinoptilolite may be subjected to ion exchange granules, or other commercially available form, or may be reduced in flowing powder fine grinding. Clinoptilolite, subjected to ion exchange, can be used to separate nitrogen from methane psa method either in the original form of granules, or other physical forms, such as beads or particles are molded from powder of zeolite fine grinding, and getting balls or molded particles of the powdered zeolite fine grinding is known to specialists engaged in production of molecular sieves. Receiving adsorbent may include the addition of other materials, such as clay, silica, alumina, metal oxides and mixtures thereof.

In this invention the chemical analysis was performed using Inductively Coupled Plasma (ISP) Atomic Absorption Spectroscopy for metal cations. The content of ammonium ion was determined by direct analysis of the content of nitrogen, and thermogravimetric analysis.

Rate of absorption of nitrogen and methane were determined using the method of constant volume. A measured amount of adsorbed gas, Adelino capacity, containing a known amount of activated clinoptilolite, while controlling the pressure in the system. The amount of adsorbed gas was calculated as a function of time using the direct measurement of pressure changes.

Samples activated in place by heating under vacuum at 500oC for three hours. Dosing volume was therefore necessary to obtain in the absence of adsorption final absolute pressure equal to one bar. In practice, depending on the degree of adsorption, the final absolute pressure is in the range from 0.8 to 1.0 bar.

Comparison of the amount of nitrogen and methane adsorbed at the same time, allows us to calculate the velocity selectivity as follows:

R1= Qn/Qm,

where R1high - speed selectivity at time t'; Qn, Qm- number, respectively, of nitrogen and methane adsorbed at time t.

It is believed that the adsorbent with a suitable speed selectivity are such adsorbents have high-speed selectivity to nitrogen with respect to methane after 25 seconds more than 5. Also, consider that the most valuable adsorbents stermy nitrogen adsorption was determined at an absolute pressure in the range of 0-10 bar using an Intelligent Gravimetric Analyzer (IGA). This private thermobalance was delivered from Hiden Analytical of Warrington, UK, and allowed to automatically determine the adsorption equilibrium. Believed that the target absorbents are absorbents that have working adsorption capacity (adsorption capacity) of more than 1.2 mol/kg, which is determined by the formula:

Qw=(N2absorbed at 10 bars)(N2absorbed at 0.1 bar),

where Qw- working adsorption capacity.

In cases where material other than clinoptilolite, has a significant amount of cation requires correction of the composition by determining the content of cations can undergo ion exchange, for example in accordance with the methodology Chao (see above), or re cationic exchange with solutions containing ammonium cations, - the method used in this invention and described below.

The following examples serve only to illustrate the invention and are not intended to limit the scope of the claims attached.

Example 1.

The original mineral clinoptilolite, called clinoptilolite of Laporte (Laporte), receive from Laporte Industry. After grinding in contrary aqueous solution of ammonium chloride at 90oC for six hours. Then the solid product is recovered from the suspension, washed with deionized water to remove chloride ions. This procedure is repeated twice, the result is Hominy ammonium clinoptilolite. It is dried at 110oC, the result is the ammonium form of clinoptilolite of Laporte.

The results of chemical analysis are given in table. 1a, the example 1. The content of cations, with the exception of ammonium cations, expressed as ratios of equivalents of charge to the total number of moles of aluminum and iron, therefore, they cannot be subjected to ion exchange (by our definition), and form the basis of our calculation of the content of the ion exchange cation in examples 4, 5 and 6 in table. 1b.

Example 2.

The original technical mineral clinoptilolite, called East West clinoptilolite receive from H&N Minerals (Glasgow, UK). After grinding it into a powder fine grinding, the material is subjected to ion exchange by mixing 75 g of powder with 1.5 liters of an aqueous solution of ammonium chloride at 90oC for six hours. Then the solid product is recovered from the suspension and washed with deionized water to remove chloride ions. This procedure is carried is the result of receiving ammonium form East West of clinoptilolite.

The results of chemical analysis are given in table. 1a, the example 2. The content of cations, with the exception of ammonium cations, expressed as ratios of equivalents of charge to the total number of moles of aluminum and iron, therefore, (according to our definition) are not able to undergo ion exchange and form the basis of our calculation of the content of cations can undergo ion exchange, for example 7 in table. 1b.

Example 3.

The original technical mineral clinoptilolite, called Adsorbex the clinoptilolite receive from Aquip Products (UK). After grinding to a powder fine grinding material is subjected to ion-exchange ions for introduction of ammonium ions by mixing 75 g of powder with 1.5 liters of an aqueous solution of ammonium chloride at 90oC for six hours. Then the solid product is recovered from the suspension and washed with deionized water to remove chloride ions. This procedure is repeated twice, the result is Hominy ammonium clinoptilolite. The product is then dried at 110oC, the result is the ammonium form Adsorbex of clinoptilolite.

The results of chemical analysis are given in table. 1A, the example 3. The content of cations, for deposits and iron, therefore, (according to our definition) are not capable of ion exchange and form the basis of our calculation of the content of cations can undergo ion exchange in example 8.

Example 4.

Composition powder technical mineral clinoptilolite described in example 1 are shown in table. 1b, the example 4. Thus, from the content of the ion-exchange of sodium in this example and which is equal to the total sodium content, subtract the content of the ion-exchange of sodium, taken from example 1 (table. 1A, example 1) or 0,065 - 0,033 = 0,032 equivalents/mol (Al+Fe). Similarly, the content of the ion exchange cations of ammonium, potassium, magnesium and calcium is 0,000, 0,255, 0,165 and 0,427 equivalents/mol (Al+Fe), respectively, and the total content of the ion exchange cations is 0,879 equivalents/mol (Al-Fe). Therefore, in this sample the content of the ion-exchange of sodium equal to 4 equivalent percent of the total ion exchangeable cations. Cations download that can be exchanged is more than one number 67 equivalent percent based on the total amount of cations that can undergo ion exchange.

The rate of adsorption of nitrogen and methane is measured using the awn equal to 11.8. The equilibrium uptake of nitrogen, shown in the table. 2, example 4, leads to the working of adsorption capacity of 1.00 mol/kg Therefore, the original mineral clinoptilolite shows a suitable speed selectivity, but with a weak regeneration properties.

Example 5.

Powder technical mineral clinoptilolite described in example 1 is subjected to repeated processing for the introduction of potassium ion to form zeolite with a high rate of exchange of potassium ions. In the used method 75 g powdered clinoptilolite mixed with 1.5 liters of aqueous 1M solution of potassium chloride at 90oC for 6 hours. After this time the solid clinoptilolite is washed by decantation with deionized water to remove chloride ions. Ion exchange was repeated twice, as above, before final filtration and drying (at 110oC) product - potassium clinoptilolite. Chemical analysis shows the composition presented in table. 1b, the example 5. Therefore, in this sample the content of the exchange of sodium is 0,038 equivalents/mol (Al+Fe) or 4 equivalent percent of the total content of the ion exchange cations. The content of the ion exchange of cations in loading more than one code adsorption constant volume, presented in table. 2, example 5. Speed selectivity in accordance with the calculations is equal to 1.24. The measurement results of the equilibrium absorption of nitrogen are given in table. 2. Therefore, the working adsorption capacity equal to 1.24 mol/kg Thus, the material has improved properties of regeneration, but the lack of speed selectivity for separation of nitrogen from methane.

Example 6.

Powder technical mineral clinoptilolite described in example 1 is subjected to repeated ion exchange to obtain the sodium form of the zeolite. This method involves boiling under reflux 25 g raw mineral with 0.5 liters of 0.5 M aqueous solution of sodium chloride for 6 hours, followed by washing by decantation with deionized water to remove chloride ions. Just clinoptilolite treated with 5 fresh solutions of sodium chloride before final selection by centrifugation and drying at 110oC. chemical analysis Data is presented in table. 1, example 6. Thus, the content of the ion-exchange of sodium in the sample is 0,732 equivalent/mol (Al+Fe) 83 or equivalent percent of the total ion exchangeable cations.

The results, postively equal to 16.9. The measurement results of the equilibrium absorption of nitrogen are presented in table. 2, example 6. Therefore, the working adsorption capacity equal to 1.14 mol/kg Thus, this material has good speed selectivity to nitrogen with respect to methane and improved regeneration properties. However, the low uptake of nitrogen for 25 seconds does not allow him to become the most valuable adsorbent.

Example 7.

Sodium ions injected into the ammonium zeolite described in example 2 by mixing (rolling in the oven Teche with controlled temperature) 2.5 g solids with 50 ml of aqueous 0.5 M solution of sodium chloride for 3 hours at a temperature of 65oC. then the solid product produce by centrifugation, washed with deionized water until the total absence of chloride ions and dried at a temperature of 110oC. Then ion exchange is repeated twice as described above.

The results of chemical analysis are presented in table. 1, example 7, Thus, the content of the ion-exchange of sodium is of 0.615 equivalent/mol (Al+Fe) or 70 equivalent percent of the total cations. To download no cations with great content. Then the zeolite turn his BS="ptx2">

The results of the adsorption constant volume are presented in table. 2, example 7. The calculated velocity selectivity equal to 9.3. The results of measurements of the equilibrium absorption of nitrogen are given in table. 2, example 7. Thus, the working of the adsorption capacity is equal to 1.57 mol/kg Therefore, the zeolite is the most valuable adsorbent from the point of view of nitrogen absorption after 25 seconds, high selectivity and improved regeneration.

Example 8.

Raw mineral clinoptilolite described in example 3 is used in its original granular form, with the only preprocessing is pre-rinsed with deionized water. The exchange of potassium ions in this material is carried out by mixing 25 kg of clinoptilolite with 130 litres of water 0,61 M solution of potassium nitrate at 95oC for eight hours. Then the solid is washed to remove the metal cations and the described procedure is repeated twice, the result is intermediate potassium clinoptilolite. Then conduct ion exchange for the introduction of sodium ions using the same technique and three separate water 0,82 M solutions of sodium nitrate, volume 130 litres. After washing deionising analysis are given in table. 1, example 8. Thus, the content in this sample of sodium that can undergo ion exchange, as well 0,458 equivalent/mol (Al+Fe) or 53 equivalent percent based on the total amount of ion exchange of cations. Ion exchange cations boot are more than one number 10 equivalent percent based on the total content of cations.

The results obtained by adsorption with constant volume, are presented in table. 2, example 8. The calculated velocity selectivity equal to 9.3. The results of measurements of the equilibrium absorption of nitrogen are presented in table. 2, example 8. Thus, the working adsorption capacity is 1.21 mol/kg Therefore, the zeolite is the most valuable adsorbent from the point of view of nitrogen absorption after 25 seconds, high selectivity and improved regeneration.

1. The adsorbent for separation of nitrogen from a source gas containing at least one non-nitrogen gas, the size of the molecules is equal to or larger than the molecules of methane, the adsorbent comprises clinoptilolite containing sodium ions in a quantity in the range of 17 to 95 equivalent percent based on the total amount of ion exchange of cations and the sum of less than 12 equivalent percent based on the total amount of ion exchange of cations, else, if there is monovalent cations of one or more species other than sodium cations, and the adsorbent has: 1) high-speed selectivity to nitrogen with respect to methane, which exceeds 5 after 25 s, as defined by the expression R1= Qn/Qmwhere R1high - speed selectivity at time t, and Qn, Qm- number, respectively, of nitrogen and methane adsorbed at time t; 2) the ability to adsorb at least 0.2 mol/kg of nitrogen after 25 s, and 3) working adsorption capacity of just over 1.2 mol/kg, as determined by the Qw= (N2absorbed at 10 bars) - (N2absorbed at 0.1 bar), where Qw- working adsorption capacity.

2. The adsorbent under item 1, in which the content of sodium ion is in the range from 26 to 80 equivalent percent based on the total amount of ion exchange of cations.

3. The adsorbent under item 1 or 2, in which monovalent cation other than sodium ion is the cation of one or more kinds from the group comprising H+, NH4+TO+Li+, Rb+and CE+.

4. The method of producing adsorbent for separation of nitrogen from a source gas, soda or larger than the molecules of methane, the method includes processing of clinoptilolite at least one ion exchange with a solution containing monovalent cation, with the receipt of clinoptilolite containing sodium ions in a quantity in the range of 17 to 95 equivalent percent based on the total amount of ion exchange of cations and optional nedovarennye cations of one or more species, if present, constitute in total, less than 12 equivalent percent based on the total amount of ion exchange of cations and the rest, if any, are monovalent cations of one or more species other than sodium cations, and the adsorbent has: 1) speed selectivity to nitrogen with respect to methane, which exceeds 5 after 25 s, as defined by R1= Qn/Qmwhere R1high - speed selectivity at time t and Qn, Qm- number, respectively, of nitrogen and methane adsorbed at time t; 2) the ability to adsorb at least 0.2 mol/kg of nitrogen after 25 s, and 3) working adsorption capacity for nitrogen over 1.2 mol/kg, as determined by the Qw= (N2absorbed at 10 bars) - (N2absorbed at 0.1 bar), where Qw- working adsorption able is about 80 equivalent percent based on the total amount of ion exchange of cations.

6. The method according to p. 4 or 5, in which monovalent cation other than sodium cation is a cation of one or more kinds from the group comprising H+, NH4+TO+Li+, Rb+and CE+.

7. A way of separating nitrogen from a source gas containing at least one non-nitrogen gas having a size of molecules is equal to or greater than the size of molecules of methane, the method comprises contacting the source gas with clinoptilolite adsorbent to obtain a product with a lower nitrogen relative to another gas or gases, than the feed gas and the adsorbent includes the content of sodium ion in an amount in the range of 17 to 95 equivalent percent based on the total amount of ion exchange of cations and optional nedovarennye cations of one or more species that, if present, total $ less than 12 equivalent percent based on the total content of neionogennyh cations, and the rest, if there is monovalent cations of one or more species other than sodium cations, and the adsorbent has: 1) high-speed selectivity to nitrogen with respect to methane, which is more than 5 on the Qn, Qm- number, respectively, of nitrogen and methane adsorbed at time t; 2) the ability to adsorb at least 0.2 mol/kg of nitrogen through 25 and 3) working adsorption capacity for nitrogen over 1.2 mol/kg, as determined by the Qw= (N2absorbed at 10 bars) - (N2absorbed at 0.1 bar), where Qw- working adsorption capacity.

8. The method according to p. 7, in which the content of sodium ion is in the range from 26 to 80 equivalent percent based on the total amount of ion exchange of cations.

9. The method according to p. 7 or 8, in which the monovalent cation other than sodium cation is a cation of one or more kinds from the group comprising H+, NH4+TO+Li+, Rb+and CE+.

 

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EFFECT: the invention ensures increased purification efficiency, possibility to use different sorbents with various properties, operation of the adsorber with changing while in operation volumes of adsorbent.

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