CN113351168A - Efficient separation method for methane in mixed gas - Google Patents
Efficient separation method for methane in mixed gas Download PDFInfo
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- CN113351168A CN113351168A CN202110663653.8A CN202110663653A CN113351168A CN 113351168 A CN113351168 A CN 113351168A CN 202110663653 A CN202110663653 A CN 202110663653A CN 113351168 A CN113351168 A CN 113351168A
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/223—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material containing metals, e.g. organo-metallic compounds, coordination complexes
- B01J20/226—Coordination polymers, e.g. metal-organic frameworks [MOF], zeolitic imidazolate frameworks [ZIF]
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2256/00—Main component in the product gas stream after treatment
- B01D2256/24—Hydrocarbons
- B01D2256/245—Methane
Abstract
The invention relates to a method for efficiently separating methane from mixed gas, which comprises the steps of adsorbing methane from the mixed gas containing methane at a certain temperature and pressure through a container filled with a methane selective adsorbent, and desorbing and regenerating the adsorbent by inert gas purging or vacuumizing at room temperature, wherein the adsorbent is ZSTU-1 (Ti)6(μ3‑O)6(μ2‑OH)6(TCA)2(H2O)(DMF)2). The methane separation method provided by the invention reduces the difficulty of the separation of related gases, enlarges the application range of the adsorption separation method, and can obtain high-purity methane product gas in an adsorption separation mode for low-concentration methane gas in the methane-nitrogen mixed gas; the adsorbent prepared by the method has high methane adsorption to methane-nitrogen mixtureThe method has the advantages of high adsorption quantity, high separation selectivity and good stability, is suitable for industrial production, and has more excellent separation effect on the methane mixed gas than the traditional method.
Description
Technical Field
The invention relates to a gas separation technology, in particular to a high-efficiency separation method of methane in a mixed gas.
Background
Methane is used as a novel clean green energy source, and is widely applied to various aspects of production and life due to the characteristics of high heat value, small pollution and the like. Compared with traditional fossil energy coal, petroleum and the like, the methane consumption is increased year by year. Furthermore, methane is also a strong greenhouse gas, which causes 21 times the greenhouse effect of common carbon dioxide. In the development and utilization process of unconventional natural gas (coal bed gas, shale gas, methane and the like), the production of methane is accompanied by impurity gases such as nitrogen, carbon dioxide, carbon monoxide and the like, and the existence of the impurity gases not only greatly reduces the calorific value of the methane, but also poses great challenges to mining and transportation equipment due to the corrosivity of the associated gases. In the case of coal bed gas, the separation of the two gas components of methane and nitrogen in the produced mixed gas is very difficult due to the similar physicochemical properties and kinetic diameters of the two gas components. In order to obtain a high purity methane product gas, it is often necessary to use the difference between the boiling points of the two components for separation by cryogenic rectification. However, in order to ensure the reduction of the nitrogen concentration in the mixed gas, the cryogenic process generally operates under high pressure and low temperature, and efficient separation can be realized only by passing through a plurality of stages of trays. Therefore, the process has a significant problem of excessive energy consumption while maintaining high separation efficiency. If the novel adsorption separation mode can be adopted to realize the high-efficiency separation and enrichment of the low-concentration impurity gas components in the methane or the low-carbon hydrocarbon components related to the methane, thereby realizing the separation and purification of the unconventional natural gas, the method has great significance.
According to the production process of methane, the main impurity gas component in the application scene related to methane separation is nitrogen. In view of the huge energy consumption in the separation process of the two components of methane and nitrogen, the adsorption separation is expected to become a new energy-saving separation mode and is paid much attention, and the key point of the application of the technology lies in the design and preparation of excellent adsorbent materials. The metal organic framework Material (MOF) has a highly ordered three-dimensional pore channel structure, finely adjustable pore channel sizes and abundant functional pore channel surfaces, and shows great application potential in the field of gas adsorption and separation in recent years. If the MOF material with methane selective adsorption can be developed to be directly used for methane purification, the method has a great application prospect. However, in the prior art, many MOF materials related to methane nitrogen are limited by problems such as low methane adsorption amount and low selectivity, and development of MOF materials having both high methane adsorption amount and selectivity is more advantageous for industrial adsorption and separation.
Disclosure of Invention
The invention provides a high-efficiency separation method of methane in a mixed gas, which improves the gas separation efficiency and the purity of the obtained methane.
The technical scheme adopted by the invention is as follows:
step 1: the mixed gas containing methane passes through a container filled with the prepared adsorbent at a certain temperature and pressure to complete the adsorption of methane;
step 2: the desorption regeneration of the adsorbent is completed by inert gas purging under the condition of room temperature or under the condition of vacuum negative pressure;
the preparation method of the adsorbent comprises the following steps:
1) adding 4,4' -nitrotribenzoic acid into nitrogen, nitrogen-Dimethylformamide (DMF), and uniformly stirring until the mixture is completely dissolved;
2) after stirring uniformly, adding a titanium source, and continuously stirring for reacting for a period of time;
3) after being mixed evenly, the obtained mixed solution is sealed, and is subjected to high-temperature hydrothermal reaction, washing and drying to obtain the chemical formula (Ti)6(μ3-O)6(μ2-OH)6(TCA)2(H2O)(DMF)2) The adsorbent of metal organic framework of (1).
Further, the mixed gas includes methane, nitrogen and carbon dioxide to be separated, and the like.
Furthermore, the volume fraction of the methane in the mixed gas is 0-50%, and zero is not contained.
Further, when methane is adsorbed on the adsorbent, the adsorption temperature is 0-25 ℃, and the pressure in the container is 1bar or more.
Further, when methane is adsorbed on the adsorbent, the reaction space velocity is 5-100 h-1A obtained by adsorption separationThe purity of alkane product gas can reach more than 90%.
Further, in the preparation step of the adsorbent, the total molar concentrations of the titanium source and the 4,4' -nitrotribenzoic acid are as follows: 0.4-0.5 mol/L, and the molar quantity of the titanium source is equal to that of the 4,4' -nitrotribenzoic acid. Further, in the step of preparing the adsorbent, the reaction temperature is controlled at 160-190 ℃, and the reaction time is 24-48 h.
Further, in the preparation step of the adsorbent, the reaction solvent is super-dry anhydrous, and the amount of DMF is controlled to be 5-10 mL.
Further, the titanium source is isopropyl titanate, and the volume ratio of the isopropyl titanate is 1:1 as a precipitation washing solution.
Due to the adoption of the technical scheme, the invention has the beneficial effects that:
1) according to the efficient methane separation method provided by the invention, the adsorbent material prepared by a hydrothermal method is adopted, so that the efficient separation of low-concentration methane in the methane-nitrogen mixed gas can be realized, the application range of the separation method is expanded, the method is not limited by the concentration of nitrogen in the mixed gas, and a high-purity methane recovered substance can be obtained.
2) Compared with the traditional adsorbing material, the methane selective adsorbing material prepared by the invention has stronger adsorption acting force on methane, has excellent methane and nitrogen separation selectivity, and has good methane and nitrogen separation performance within a test pressure range.
3) Compared with the traditional methane selective material, the MOF material prepared by the invention has more excellent water vapor, acid, alkali and thermal stability, and can be better suitable for industrial adsorption and separation.
Drawings
FIG. 1 is an SEM image of the adsorbent material obtained in example 1 at different magnifications.
FIG. 2 is an XRD pattern of the adsorbent obtained in example 1 and a ZSTU-1 theoretical structure crystal form.
FIG. 3 is a graph showing the adsorption and desorption curves of the adsorbent 77K obtained in example 1 for nitrogen.
FIG. 4 is an adsorption curve of the adsorbent obtained in example 1 at 298K for methane nitrogen.
FIG. 5 is a graph showing the breakthrough curves of the adsorbents obtained in example 1 at room temperature under normal atmospheric pressure for various proportions of a mixed gas of methane and nitrogen.
FIG. 6 is an XRD pattern of the adsorbent obtained in example 1 after treatment under different conditions.
FIG. 7 is a multiple methane adsorption isotherm for the adsorbent obtained in example 1.
FIG. 8 shows a multi-cycle mixed gas separation experiment of the adsorbent obtained in example 1.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention clearer, the present invention is described in detail below with reference to specific examples and experimental data, and it should be understood that the specific examples described herein are only for explaining the present invention and are not intended to limit the present invention.
A method for efficiently separating methane in a mixed gas comprises the following steps:
step 1: the mixed gas containing methane passes through a container filled with the prepared adsorbent at a certain temperature and pressure to complete the adsorption of methane;
step 2: the desorption regeneration of the adsorbent is completed by inert gas purging under the condition of room temperature or under the condition of vacuum negative pressure;
the preparation method of the adsorbent comprises the following steps:
1) adding 4,4' -nitrotribenzoic acid into nitrogen, nitrogen-dimethylformamide, and uniformly stirring until the mixture is completely dissolved;
2) after stirring uniformly, adding a titanium source, and continuously stirring for reacting for a period of time;
3) after being mixed evenly, the obtained mixed solution is sealed, subjected to high-temperature hydrothermal reaction, washed and dried to obtain the chemical formula (Ti)6(μ3-O)6(μ2-OH)6(TCA)2(H2O)(DMF)2) An adsorbent of a Metal Organic Framework (MOF) of (a).
In the synthesis process, different titanium precursor metal salts are selected, the hydrolysis rate of the titanium precursor metal salts in the hydrothermal reaction process is controlled, a sample with high crystallinity can be better synthesized, and the yield of the sample is improved, so that the cost is saved, and the method is favorable for industrial preparation of the adsorbent. The titanium source in the embodiment can be selected from isopropyl titanate, titanium n-butoxide and other titanium sources, preferably isopropyl titanate, so that the cost is saved and the yield of the MOF is high.
The method for efficiently separating the methane has simple steps, and when the methane is recovered as the product gas, the methane is desorbed on the adsorbent by a vacuumizing method to realize the regeneration of the adsorbent.
In some embodiments, the mixed gas comprises a methane and nitrogen mixed gas.
In some specific embodiments, the volume fraction of the methane in the mixed gas is 0-50%, and the mixed gas does not contain zero value, so that the concentration range applicability of the methane is wide.
In some embodiments, the adsorption of methane on the adsorbent occurs at an adsorption temperature of 0-25 ℃ and a pressure in the vessel of 1bar or more.
In some embodiments, when methane is adsorbed on the adsorbent, the reaction space velocity is 5-100 h-1The purity of the methane product gas obtained by adsorption separation can reach more than 90%. The invention has wide applicable airspeed range under the condition of ensuring the selective adsorption of methane, and the obtained methane has higher concentration and can improve the economic benefit.
In some embodiments, the total molar concentration of the titanium source and the 4,4',4 "-nitrotribenzoic acid is: 0.4-0.5 mol/L, the molar weight of the titanium source is equal to that of the 4,4' -nitrotribenzoic acid, the reaction temperature is controlled at 190 ℃, the reaction time is 24-48 h, and the yield of the MOF is improved.
In some embodiments, in the step of preparing the adsorbent, the reaction solvent is completely anhydrous, and the amount of DMF is controlled to be 5-10 mL. The titanium source is isopropyl titanate, and the volume ratio is 1:1 as a precipitation washing solution. Under the mixing proportion, impurities and residual reactants on the MOF surface can be effectively and quickly washed and removed, so that the purity of the product is improved. The sources of the two washing solutions are readily available, and the present invention is not limited to such washing solutions at this ratio, and other organic, inorganic or mixed solutions capable of effectively washing MOF precipitates are equally suitable for use in the present invention.
Specific examples are exemplified below.
Example 1
0.377mg of 4,4',4 "-nitrotribenzoic acid was added to 5.0mL of DMF and after stirring to complete dissolution, 0.31mL of isopropyl titanate was added and stirred well to form a homogeneous orange solution. Sealing the mixed solution in a 25mL high-pressure hydrothermal reaction kettle, reacting at 180 ℃ for 24h, washing with a DMF/methanol (1:1) mixed solution, and centrifugally drying to obtain the product.
Example 2
Before testing the adsorptive separation performance of the prepared samples, solvent exchange and washing were performed using methanol. And performing Soxhlet extraction on the prepared orange sample powder by using methanol, washing for 12h, and drying in vacuum to obtain the adsorbent material for removing the guest molecules.
Example 3
The activation condition of the test sample is 120 ℃, degassing and activating for 4h under vacuum, and then the gas adsorption separation performance test of the sample is carried out, wherein the pressure range of the test sample is 0-1 bar.
In order to characterize the microscopic morphology of the ZSTU-1 material, the product obtained in example 1 was subjected to SEM characterization, and the results are shown in FIG. 1. The two graphs a and b in fig. 1 are SEM images of example 1 at different magnifications, and it can be seen from the graphs that the prepared zsttu-1 sample has small particle size of about 200nm, has a hexagonal prism shape, has a loose structure, and is more beneficial to mass transfer and diffusion of gas.
In order to confirm the crystal structure of the synthesized sample, XRD characterization was performed on the sample synthesized in example 1, and the result was compared with the simulated peak of the zsttu-1 theoretical crystal structure, and the comparison result is shown in fig. 2. As can be seen from the figure, the XRD diffraction peak of the ZSTU-1 prepared by the method is consistent with the simulated peak of the theoretical crystal structure of the original structure, which shows that the ZSTU-1 material is successfully synthesized by the method.
In order to characterize the adsorption capacity of the zstt-1 material to different gases, the adsorption performance of the product obtained in example 1 was tested by using Micromeritics ASAP 2020 instrument, and the adsorption curve of the product obtained in example 1 to each gas was measured at 298K, fig. 3 is the nitrogen adsorption and desorption curve of the material at 77K, and fig. 4 is the corresponding methane nitrogen adsorption and desorption curve. As can be seen from fig. 3 to 4, zsttu-1 has a higher BET specific surface area, and exhibits adsorption performance of selectively adsorbing methane than nitrogen over the test temperature range, and exhibits a higher methane adsorption capacity at room temperature under normal atmospheric pressure.
In order to test the practical effect of the ZSTU-1 material on the separation of methane and nitrogen mixed gas in different proportions, the product obtained in example 1 was taken as an example, and a methane and nitrogen mixed gas separation experiment was carried out on the product obtained in example 1. The specific process is as follows: accurately controlling the mixed gas to pass through an adsorption column (with the size of phi 4 multiplied by 95mm) filled with an adsorbent (sample amount: 0.67g) at the pressure of 1.0bar and the flow rate of 2mL/min by a pressure reducing valve and a gas mass flowmeter, controlling the temperature of the adsorption column to be 298K, starting timing when the mixed gas starts to enter the adsorption column, monitoring the tail gas concentration in real time by a chromatograph (GC-2014C, TCD detector) at the tail end of the adsorption column, recording data until the concentration of the two components of gas reaches the initial concentration, and considering that the two gases completely pass out, and considering that the adsorption is finished.
When the mixed gas is methane nitrogen (with volume fraction ratio of 1/1 and 2/8), the penetration curves of the adsorbent material are respectively shown in figures 5a-b, and as can be seen from figure 5b, the material can effectively realize the selective adsorption of methane in the methane nitrogen mixed gas and realize the low-concentration CH4/N2(volume fraction ratio 2/8).
In order to test the stability of the ZSTU-1 material, taking the product prepared in example 1 as an example, the water vapor, acid and alkali, XRD pattern after adsorption penetration and cyclic adsorption performance of the material are tested. After the sample is respectively exposed to different humidity environments or soaked in different pH solutions, common solvents for two days, the original crystal structure of the sample is still maintained as can be seen from the XRD pattern shown in figure 6. Fig. 7 and 8 show the cyclic adsorption isotherm of methane gas and the methane-nitrogen mixed gas separation experiment, respectively, and it can be seen that the performance of the zsttu-1 material is completely maintained through multiple adsorption-desorption cyclic breakthrough experiments.
Claims (9)
1. The efficient separation method for methane in the mixed gas is characterized by comprising the following steps of:
step 1: the mixed gas containing methane passes through a container filled with the prepared adsorbent at a certain temperature and pressure to complete the selective adsorption of methane;
step 2: the desorption regeneration of the adsorbent is completed by using inert gas purging under the condition of room temperature or under the condition of vacuum negative pressure;
the preparation method of the adsorbent comprises the following steps:
1) adding 4,4' -nitrotribenzoic acid into nitrogen, nitrogen-dimethylformamide, and uniformly stirring until the mixture is completely dissolved;
2) adding a titanium source into the uniformly stirred clear solution, and continuously stirring and reacting for a period of time;
3) after being mixed evenly, the obtained mixed solution is sealed, and is subjected to high-temperature hydrothermal reaction, washing and drying to obtain the chemical formula (Ti)6(μ3-O)6(μ2-OH)6(TCA)2(H2O)(DMF)2) An adsorbent material of a Metal Organic Framework (MOF).
2. The method for efficiently separating methane from a mixed gas according to claim 1, wherein the mixed gas comprises methane and impurity gas to be separated.
3. The method for efficiently separating methane from a mixed gas according to claim 1, wherein the volume fraction of methane in the mixed gas is 0-50% and does not contain a zero value.
4. The method for efficiently separating methane from a mixed gas according to claim 1, wherein when methane is adsorbed on the adsorbent, the adsorption temperature is 0 to 25 ℃, and the pressure in the container is 1bar or more.
5. The method for efficiently separating methane from a mixed gas as claimed in any one of claims 1 to 4, wherein when methane is adsorbed on the adsorbent, the adsorption reaction space velocity is 5 to 100h-1。
6. The method for efficiently separating methane from a mixed gas according to claim 1, wherein in the step of preparing the adsorbent, the total molar concentrations of the titanium source and the 4,4',4 "-nitrotribenzoic acid are as follows: 0.4-0.5 mol/L, and the molar quantity of the titanium source is equal to that of the 4,4' -nitrotribenzoic acid.
7. The method for separating methane from a mixed gas as claimed in claim 1 or 6, wherein in the step of preparing the adsorbent, the reaction temperature is controlled at 190 ℃ and the reaction time is 24-48 h.
8. The method for efficiently separating methane from a mixed gas as claimed in claim 1, 6 or 7, wherein in the step of preparing the adsorbent, the reaction solvent is all ultra-dry and anhydrous, and the amount of DMF is controlled to be 5-10 mL.
9. The method for efficiently separating methane from a mixed gas according to claim 8, wherein the titanium source is isopropyl titanate, and the volume ratio of the isopropyl titanate is 1:1 as a precipitation washing solution.
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| CN115010948A (en) * | 2022-07-01 | 2022-09-06 | 太原理工大学 | DMOF- (CF) 3 ) 2 Synthetic method and application of efficient separation of propane and propylene under humid condition |
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| CN116375037A (en) * | 2023-04-17 | 2023-07-04 | 江苏中能硅业科技发展有限公司 | Monosilane recovery system and monosilane recovery method |
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Cited By (4)
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| CN115010948A (en) * | 2022-07-01 | 2022-09-06 | 太原理工大学 | DMOF- (CF) 3 ) 2 Synthetic method and application of efficient separation of propane and propylene under humid condition |
| CN115010948B (en) * | 2022-07-01 | 2024-03-08 | 太原理工大学 | DMOF- (CF) 3 ) 2 Synthesis method of (C) and application of (C) in high-efficiency separation of propane propylene under humid condition |
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Application publication date: 20210907 |