CN112675811A - High-efficiency separation N2O/CO2Silver exchange molecular sieve adsorbent and preparation method thereof - Google Patents
High-efficiency separation N2O/CO2Silver exchange molecular sieve adsorbent and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of separation materials, and discloses a method for efficiently separating N2O/CO2The silver exchange molecular sieve adsorbent and the preparation method thereof, which take 13X and 5A molecular sieves as basic framework materials and prepare a certain amount of Ag by adjusting the composition of balanced cations+AgX and AgA molecular sieves of exchange degree. In the present invention, the balance cation is changed from alkali metal or alkaline earth metal to Ag+Shows excellent N2Preferential adsorption capacity of O to N2O/CO2Has high selectivity and adsorption capacity. The invention can be applied to N in tail gas generated in the industrial production process of nitric acid, adipic acid and the like2The separation and recovery of O have good application prospect and important practical value.
Description
Technical Field
The invention belongs to the technical field of separation materials, and relates to N2O and CO2A preparation method of a separation material, in particular to a method for efficiently separating N2O/CO2Silver exchange molecular sieve adsorbent and preparation method thereofThe method is carried out.
Background
Nitrous oxide (N)2O, laughing gas) is six kinds of gas relay carbon dioxide (CO) discharged by the restriction of the protocol of the Kyoto protocol2) Methane (CH)4) The third largest greenhouse gas, which causes 298 times as much greenhouse effect as carbon dioxide and which causes damage to stratospheric ozone. In addition, N2O has important application in the fields of medicine, food and spaceflight. Thus, for N2The recycling of O has double meanings. N is a radical of2The emission of O is 40% of that caused by human activities, mainly agriculture, transportation and industry. In the industrial production of adipic acid and nitric acid, N2O is often emitted as a by-product. At present, the industry is on N2There are three main methods for treating O, one of which is used as an oxidant and CH4Combustion of gases but with generation of CO2Secondary pollution caused by gas; second, for low concentration N in tail gas2O, can be substituted by N2Direct catalytic decomposition of O into N without environmental pollution2And O2But N is2High temperature is required for O decomposition, energy consumption is high, and N is generated after decomposition2O cannot be used as a valuable intermediate for the production of other fine chemicals; thirdly for high concentration of N2O, can be substituted by N2O as an oxidant, industrially, benzene is oxidized in one step to produce phenol, but usually N is present in the tail gas2The concentration of O is not up to the requirement, and further enrichment is needed. Therefore, an economical and effective method for separating or enriching N is found2O is necessary to make it useful for other industrial processes. In the tail gas from adipic acid and nitric acid production, except for N2In addition to O, there is also CO whose properties are very similar to those of O2。CO2And N2O, although composed of different elements, has the same relative molecular mass and kinetic diameter, similar liquefaction temperature and polarizability, and so on, and thus N2O/CO2Have significant challenges. The pressure swing adsorption separation (PSA) technology has the advantages of low energy consumption, simple operation and the like, and is more and more popular in recent yearsThe more attention is paid. The most important part of pressure swing adsorption separation is the selection of adsorbent, and the adsorbents commonly used in the adsorption separation process are carbon materials (activated carbon and carbon molecular sieve), molecular sieves, silica sol, Metal Organic Frameworks (MOFs), and the like. Comparing these several types of adsorbents findings: the carbon material does not have a uniform pore structure, the MOFs material has poor stability, and in comparison with the molecular sieve, the molecular sieve has a uniform pore structure and pore size, good thermal stability and adjustable specific surface area and pore volume, so that the molecular sieve adsorbent is researched and applied more. The type of counter cation, an important factor affecting the molecular sieve properties, also has a large impact on the adsorptive separation of gases. The X-type molecular sieve and the A-type molecular sieve have lower silicon-aluminum ratio (1.15 and 1.00 respectively), and have more balancing cations in pore channels, so that the two molecular sieves are selected for silver ion exchange to realize N2O/CO2The adsorption separation of (3).
Disclosure of Invention
In order to solve the problem of N in tail gas generated by adipic acid and nitric acid2O and CO2The invention discloses a method for efficiently separating N2O/CO2The silver exchange molecular sieve adsorbent can be prepared from N2O and CO2Preferential adsorption of N in mixed tail gas2O and has better N2O/CO2And (4) separation effect.
The invention is realized by the following technical scheme:
in one aspect, the invention discloses a method for efficiently separating N2O/CO2The silver exchange molecular sieve adsorbent is prepared by carrying out silver exchange on a molecular sieve with the silicon-aluminum ratio not more than 1.2 to obtain Ag+Silver exchange molecular sieve with exchange degree not less than 66%.
Further, the molecular sieve is a 13X molecular sieve or a 5A molecular sieve, the silica-alumina ratio of the 13X molecular sieve is 1.15, and the 13X molecular sieve is subjected to silver exchange to obtain Ag+Silver exchange 13X molecular sieve adsorbent with exchange degree more than or equal to 84%; the silicon-aluminum ratio of the 5A molecular sieve is 1, and the 5A molecular sieve is respectively subjected to silver exchange to obtain Ag+The exchange degree is more than or equal to 66 percent of the silver exchange 5A molecular sieve adsorbent.
On the other hand, the invention also discloses a method for efficiently separating N2O/CO2The preparation method of the silver exchange molecular sieve adsorbent is realized by the following steps:
(1) adding a molecular sieve with the silicon-aluminum ratio not more than 1.2 into AgNO3Heating and stirring the aqueous solution, and carrying out silver exchange for at least one time;
(2) washing the molecular sieve subjected to silver exchange in the step (1) by deionized water, filtering and drying to obtain Ag+Silver exchange molecular sieve with exchange degree not less than 66%;
(3) vacuumizing and activating the silver exchange molecular sieve obtained in the step (2) at the temperature of 150-2O/CO2The silver exchange molecular sieve adsorbent with adsorption reverse action;
wherein the molecular sieve is a 13X molecular sieve or a 5A molecular sieve.
As a preferred embodiment, 13X molecular sieves and AgNO3The mass-volume ratio of the solution is 1 g/(50-100) mL, and the 5A molecular sieve and AgNO are3The mass-to-volume ratio of the solution is 1 g/(50-100) mL, the heating temperature is 60-80 ℃, and the stirring time is 1-3 h; further, in the step (1), AgNO3The concentration of the aqueous solution is 0.05-0.4 mol/L.
As a preferred embodiment, in step (1), AgNO3The concentration of the aqueous solution is 0.05-0.4 mol/L, the heating and stirring temperature is 60-80 ℃, and the time is 1-3 h.
In a preferred embodiment, in the step (2), the drying temperature is 80-120 ℃ and the time is 24 hours.
In a preferable embodiment, in the step (3), the vacuumizing activation time of the silver exchanged 13X and 5A molecular sieves is 5-10 h; further, the silver of the 13X molecular sieve is exchanged to obtain Ag +13X molecular sieve adsorbent with exchange degree more than or equal to 84 percent, and 5A molecular sieve silver exchange to obtain Ag +5A molecular sieve adsorbent with exchange degree not less than 66%.
In addition, the high efficiency separation of N prepared by the invention2O/CO2The silver exchange molecular sieve adsorbent is used for separating CO in nitric acid or adipic acid tail gas2And N2O mixtureThe use of (1).
Compared with the prior art, the invention has the following beneficial effects:
(1) the invention realizes N by silver exchange of 13X and 5A molecular sieves and AgA (exchange degree is more than or equal to 66%) and AgX (exchange degree is more than or equal to 84%) molecular sieves obtained by controlling the exchange degrees2O/CO2Reversal of adsorption; balancing Ag+The introduction of ions replaces the original alkaline earth metal (Ca)2+) Or alkali metal (Na)+) Balancing cations, introducing pairs of N2Ag with O having stronger affinity+Thereby realizing N2Preferential adsorption of O, thereby effecting N2O/CO2Separating;
(2) the AgA and AgX molecular sieve adsorbent prepared by silver exchange of 13X and 5A molecular sieves has the advantages of simple preparation method, easy batch production, good stability, reusability and good application prospect, and is particularly suitable for N in tail gas generated in the industrial production process of nitric acid, adipic acid and the like2O/CO2Separation of (2) to realize N2And (4) effectively utilizing O.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 shows the realization of N by 13X and 5A molecular sieves after silver exchange in the invention2O and CO2Schematic representation of adsorption reversal of (1).
FIG. 2 is a PXRD diffraction pattern of the A-4 and X-4 molecular sieves obtained in examples 5 and 6 and the original powders 13X and 5A. from FIG. 1, it can be seen that the A-4 and X-4 molecular sieves obtained after silver exchange of the 13X and 5A molecular sieves are complete in structure and are not destroyed.
FIG. 3 is the N at 77K of A-4 and X-4 and the raw powders 13X and 5A obtained in examples 5 and 62Adsorption and desorption curve diagramIt shows that the larger Ag is added+By replacement of original Na+Or Ca2+The specific surface area of the material is then reduced.
FIG. 4 is the CO at 298K of X-4 and the original powder 13X obtained in example 52And N2Adsorption isotherm of O. As can be seen from the adsorption isotherms, the CO in the original 13X powder2Is greater than N2O, expressed as CO2Selectively adsorbing the material while replacing the equilibrium cations in 13X with Ag+And reached a certain degree of exchange (84%), expressed as N2Selective adsorbent for O, and at 89% exchange degree, N2Amount of adsorbed O and CO2Is the largest.
FIG. 5 is the CO at 298K of A-4 obtained in example 6 and of the original powder 5A2And N2Adsorption isotherm of O. As can be seen from the adsorption isotherms, the CO in the original 5A powder2Is greater than N2O, expressed as CO2Selectively adsorbing the material while replacing the equilibrium cations in 5A with Ag+And when a certain degree of exchange is reached (66%), it is expressed as N2Selective adsorbent for O, and at 79% degree of exchange, N2Amount of adsorbed O and CO2Is the largest.
FIG. 6 is a graph of the ideal solution adsorption theory (IAST) calculated material versus binary N for A-4 and X-4 and the raw powders 13X and 5A obtained in examples 5 and 62O/CO2Adsorption selectivity of mixed gases, CO on samples by Langmuir-Freundlich isotherm model2And N2And fitting the gas adsorption isotherm of the O pure gas component. Further validation of Ag from IAST selectivity+After switching realize N2Selective adsorption of O.
FIG. 7 shows the CO of A-4 and X-4 after Ag exchange in examples 5 and 62And N2Breakthrough profile of O-mix (1: 1 v/v). As can be seen from the breakthrough curves, CO is present on A-4 and X-42All pass through the Ag layer preferentially+After switching, it is represented as N2Selective adsorption material of O to realize N2O/CO2The adsorption of (1) is reversed.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
High-efficiency separation N2O/CO2The preparation method of the silver exchange molecular sieve adsorbent is realized by the following steps:
(1) 1g of 13X molecular sieve was added to 60mL of 0.1mol/mL AgNO3Heating and stirring the solution for 1h at 80 ℃ in the aqueous solution, carrying out silver exchange for one time, and keeping the total amount of the solution unchanged in the heating process;
(2) washing the molecular sieve subjected to silver exchange in the step (1) by using deionized water, filtering, and drying at 120 ℃ for 24 hours to obtain a 13X molecular sieve subjected to silver exchange;
(3) vacuumizing and activating the silver-exchanged 13X molecular sieve obtained in the step (2) for 5 hours at the temperature of 200 ℃ to obtain Ag+An X-2 molecular sieve adsorbent with an exchange degree of 84%; the X-2 molecular sieve was then tested for N2O/CO2The gas adsorption separation performance of (1).
Example 2
High-efficiency separation N2O/CO2The preparation method of the silver exchange molecular sieve adsorbent is realized by the following steps:
(1) 1g of 5A molecular sieve was added to 60mL of 0.1mol/mL AgNO3Heating and stirring the solution for 1h at 80 ℃ in the aqueous solution, carrying out silver exchange for one time, and keeping the total amount of the solution unchanged in the heating process;
(2) washing the molecular sieve subjected to silver exchange in the step (1) by using deionized water, filtering, and drying at 120 ℃ for 24 hours to obtain a 5A molecular sieve subjected to silver exchange;
(3) vacuumizing and activating the 5A molecular sieve obtained in the step (2) for 5 hours at 200 ℃ to obtain Ag+Degree of exchange of73% of a-2 molecular sieve adsorbent; the A-2 molecular sieves were then tested for N2O/CO2The gas adsorption separation performance of (1).
Example 3
High-efficiency separation N2O/CO2The preparation method of the silver exchange molecular sieve adsorbent is realized by the following steps:
(1) 1g of 13X molecular sieve was added to 70mL of 0.3mol/mL AgNO3In the solution, heating and stirring for 2h at 60 ℃, carrying out silver exchange for the first time, and keeping the total amount of the solution unchanged in the heating process;
(2) washing the molecular sieve subjected to silver exchange in the step (1) by using deionized water, filtering, and drying at 100 ℃ for 24 hours to obtain a silver exchange 13X molecular sieve;
(3) vacuumizing and activating the silver-exchanged 13X molecular sieve obtained in the step (2) for 10 hours at 180 ℃ to obtain Ag+An X-3 molecular sieve adsorbent with an exchange degree of 88%; the X-3 molecular sieve was then tested for N2O/CO2The gas adsorption separation performance of (1).
Example 4
High-efficiency separation N2O/CO2The preparation method of the silver exchange molecular sieve adsorbent is realized by the following steps:
(1) 1g of 5A molecular sieve was added to 70mL of 0.3mol/mL AgNO3In the solution, heating and stirring for 2h at 60 ℃, carrying out silver exchange for the first time, and keeping the total amount of the solution unchanged in the heating process;
(2) washing the molecular sieve subjected to silver exchange in the step (1) by using deionized water, filtering, and drying at 100 ℃ for 24 hours to obtain a silver exchange 5A molecular sieve;
(3) vacuumizing and activating the silver-exchanged 5A molecular sieve obtained in the step (2) for 10 hours at 180 ℃ to obtain Ag+An A-3 molecular sieve with an exchange degree of 78%; the A-3 molecular sieves were then tested for N2O/CO2The gas adsorption separation performance of (1).
Example 5
High-efficiency separation N2O/CO2The preparation method of the silver exchange molecular sieve adsorbent is realized by the following steps:
(1) 1g of 13X molecular sieve was added to 50mL of 0.4mol/mL AgNO3Heating and stirring the solution at 80 ℃ for 1h, carrying out silver exchange for one time, and keeping the total amount of the solution unchanged in the heating process;
(2) washing the 13X molecular sieve subjected to silver exchange in the step (1) by using deionized water, filtering, and drying at 100 ℃ for 24 hours to obtain the silver exchange 13X molecular sieve;
(3) vacuumizing and activating the silver-exchanged 13X molecular sieve obtained in the step (2) for 10 hours at 200 ℃ to obtain Ag+An X-4 molecular sieve adsorbent with an exchange degree of 89%; the X-4 molecular sieve was then tested for N2O/CO2The gas adsorption separation performance of (1).
Example 6
High-efficiency separation N2O/CO2The preparation method of the silver exchange molecular sieve adsorbent is realized by the following steps:
(1) 1g of 5A molecular sieve was added to 50mL of 0.4mol/mL AgNO3Heating and stirring the solution at 80 ℃ for 1h, carrying out silver exchange for one time, and keeping the total amount of the solution unchanged in the heating process;
(2) washing the 5A molecular sieve subjected to silver exchange in the step (1) by using deionized water, filtering, and drying at 100 ℃ for 24 hours to obtain a silver exchange 5A molecular sieve;
(3) vacuumizing and activating the silver-exchanged 5A molecular sieve obtained in the step (2) for 10 hours at 200 ℃ to obtain Ag+An A-4 molecular sieve adsorbent with an exchange degree of 79%; the A-4 molecular sieves were then tested for N2O/CO2The gas adsorption separation performance of (1).
(1) The basic matrix material was 13X and 5A powders purchased from Aladdin.
(2) Adding 1g of 13X and 5A molecular sieves obtained in the step (1) into 0.4M AgNO3In the aqueous solution, it was then stirred with heating at 80 ℃ for 1h, and the total amount of the solution was kept constant during the heating.
(3) And (3) washing and filtering the silver exchanged molecular sieve in the step (2) by deionized water, and drying the obtained sample at 100 ℃ for 24 hours.
(4) Will be described in detail(3) The obtained samples X-4 and A-4 are vacuumized and activated for 10 hours at the temperature of 200 ℃ to obtain Ag+X-4 and A-4 molecular sieve materials with respective degrees of exchange of 89% and 79%, were tested for N2O/CO2The gas adsorption separation performance of (1).
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are merely illustrative of the principles of the invention, but that various changes and modifications may be made without departing from the spirit and scope of the invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (9)
1. High-efficiency separation N2O/CO2The silver exchange molecular sieve adsorbent is characterized in that: the Ag is obtained by silver exchange of a molecular sieve with the silicon-aluminum ratio not more than 1.2+Silver exchange molecular sieve with exchange degree not less than 66%.
2. Efficient separation of N as claimed in claim 12O/CO2The silver exchange molecular sieve adsorbent is characterized in that: the molecular sieve is a 13X molecular sieve or a 5A molecular sieve, the silica-alumina ratio of the 13X molecular sieve is 1.15, and the 13X molecular sieve is subjected to silver exchange to obtain Ag+Silver exchange 13X molecular sieve adsorbent with exchange degree more than or equal to 84%; the silicon-aluminum ratio of the 5A molecular sieve is 1, and the 5A molecular sieve is respectively subjected to silver exchange to obtain Ag+The exchange degree is more than or equal to 66 percent of the silver exchange 5A molecular sieve adsorbent.
3. High-efficiency separation N2O/CO2The preparation method of the silver exchange molecular sieve adsorbent is characterized by comprising the following steps:
adding a molecular sieve with the silicon-aluminum ratio not more than 1.2 into AgNO3Heating and stirring the aqueous solution, and carrying out silver exchange for at least one time;
removing the silver exchanged molecular sieve in the step (1)Washing with ionized water, filtering and drying to obtain Ag+Silver exchange molecular sieve with exchange degree not less than 66%;
vacuumizing and activating the silver exchange molecular sieve obtained in the step (2) at the temperature of 150-2O/CO2Silver exchange molecular sieve adsorbent with adsorption reversal function;
wherein the molecular sieve is a 13X molecular sieve or a 5A molecular sieve.
4. High efficiency separation of N as claimed in claim 32O/CO2The preparation method of the silver exchange molecular sieve adsorbent is characterized by comprising the following steps: in the step (1), 13X molecular sieve and AgNO3The mass-volume ratio of the solution is 1 g/(50-100) mL, and the 5A molecular sieve and AgNO are3The mass-to-volume ratio of the solution is 1 g/(50-100) mL.
5. High efficiency separation of N as claimed in claim 32O/CO2The preparation method of the silver exchange molecular sieve adsorbent is characterized by comprising the following steps: in step (1), AgNO3The concentration of the aqueous solution is 0.05-0.4 mol/L, the heating and stirring temperature is 60-80 ℃, and the time is 1-3 h.
6. Efficient separation of N as claimed in claim 22O/CO2The preparation method of the silver exchange molecular sieve adsorbent is characterized by comprising the following steps: in the step (2), the drying temperature is 80-120 ℃ and the time is 24 h.
7. Efficient separation of N as claimed in claim 22O/CO2The preparation method of the silver exchange molecular sieve adsorbent is characterized by comprising the following steps: in the step (3), the vacuumizing activation time of the silver exchange 13X molecular sieve and the vacuumizing activation time of the silver exchange 5A molecular sieve are both 5-10 h.
8. Efficient separation of N as claimed in claim 22O/CO2The preparation method of the silver exchange molecular sieve adsorbent is characterized by comprising the following steps: in the step (3), Ag is obtained after the silver exchange of the 13X molecular sieve+13X molecular sieve adsorbent with exchange degree of more than or equal to 84 percent, 5A molecular sieve silver exchangeThen obtain Ag+5A molecular sieve adsorbent with exchange degree not less than 66%.
9. Efficient separation of N as claimed in claim 12O/CO2The silver exchange molecular sieve adsorbent is used for separating CO in nitric acid or adipic acid tail gas2And N2And (3) application of the O mixture.
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