CN113277526A - AHT configuration molecular sieve and preparation method and application thereof - Google Patents
AHT configuration molecular sieve and preparation method and application thereof Download PDFInfo
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- C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
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Abstract
The invention provides an AHT configuration molecular sieve, a preparation method and an application thereof, wherein the preparation method comprises the following steps: (1) mixing an aluminum source, a phosphorus source and a solvent to obtain a mixture precursor, aging the mixture precursor, and adding a template to obtain gel; (2) crystallizing the gel obtained in the step (1) to obtain the AHT-configuration molecular sieve; the template agent in the step (1) comprises any one or the combination of at least two of di-n-butylamine, dipentylamine, di-n-hexylamine, di-n-heptylamine or di-n-octylamine. The method adopts the novel low-toxicity organic template agent, not only can prepare the pure-phase AHT-configuration molecular sieve, reduce the preparation cost of the molecular sieve, but also obviously improves the greenness of the production process of the molecular sieve material.
Description
Technical Field
The invention belongs to the technical field of molecular sieve synthesis, and relates to an AHT-configuration molecular sieve, and a preparation method and application thereof.
Background
Volatile Organic Compounds (VOCs) are organic compounds having a high vapor pressure at room temperature, such as organic chlorides and alcohols, and are mainly produced in petrochemical, paint, spray paint, printing, rubber, pesticides, and other chemical processes. In 2017, the total emission of volatile organic compounds in China reaches 1017.45 ten thousand tons, and the total emission still tends to increase. VOCs not only have direct influence on human health, ecological environment and the like, but also can generate secondary pollutants by participating in atmospheric photochemical reaction to cause the damage of the atmospheric ozone layer. Therefore, the treatment of VOCs pollution is urgently needed. In recent years, many scholars at home and abroad are dedicated to the research on the treatment technology of the pollution of the VOCs, and the adsorption method has become one of the research hotspots for the treatment technology of the pollution of the VOCs due to the advantages of mature process, simple operation, high operation cost, high purification efficiency and the like. Molecular sieves are commonly used adsorbents in the adsorption process of VOCs. The molecular sieve material has a regular and uniform pore channel structure and a certain pore channel system, thereby having larger specific surface area and adsorption capacity. In addition, the molecular sieve material only allows molecules with the diameter smaller than the pore diameter to enter, so that specific components can be adsorbed from the VOCs, and the VOCs can be recycled. Therefore, the molecular sieve material has good application prospect in the field of purification of VOCs.
AHT configuration molecular sieve was an aluminophosphate molecular sieve discovered in 1961 by F.d' Yvoire et al (bull. soc. chim. fr.,1961,1762) from a mixed-phase aluminophosphate hydrate. The molecular sieve is prepared from AlO4Tetrahedron and PO4The tetrahedron is formed by strict alternate connection, has a unique one-dimensional ten-membered ring channel structure and the pore diameter of the channel structure is
Belonging to the AHT configuration. When removing guest water molecules, the AHT-configuration molecular sieve can generate single crystal-single crystal reversible transformation similar to MOFs materials. The dehydrated AHT-configuration molecular sieve has the characteristic of specific recognition of specific guest molecules, such as selective adsorption of methanol and ethanol, and can separate specific components from VOCs, thereby realizing the recycling of the VOCs. Methanol andethanol can be used for fuel cells and as a working fluid of adsorption-driven heat pumps, and can be converted into gasoline through processes of methanol-to-gasoline, methanol-to-olefin and the like. Therefore, from the perspective of environment and energy, the use of the AHT molecular sieve to separate methanol and ethanol from VOCs has a very important application value.
After F.d' Yvoire finds the molecular sieve with AHT configuration for the first time, the synthesis of the molecular sieve is less researched, and only two documents report the synthesis of the molecular sieve. In 1993, Li et al (Journal of the Chemical Society, 1993,89(6):951 965.) synthesized a pure-phase AHT molecular sieve for the first time by a hydrothermal method by using dipentylamine as a template agent, thin aqueous aluminum water as an aluminum source and orthophosphoric acid as a phosphorus source, but the organic template dipentylamine has high toxicity and high price and does not accord with the development trend of green chemistry.
In 2002, Kunii et al (Microporous and Mesoporous Materials,2002,52: 159-.
The AHT molecular sieve prepared by the scheme has the defects of toxic and expensive template agent or high cost of a synthesis method, and the like, so that the development of the preparation method of the AHT molecular sieve which is cheap and nontoxic and has low preparation method cost is necessary.
Disclosure of Invention
The invention aims to provide an AHT-configuration molecular sieve and a preparation method and application thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a method for preparing an AHT-configured molecular sieve, comprising the steps of:
(1) mixing an aluminum source, a phosphorus source and a solvent to obtain a mixture precursor, aging the mixture precursor, and adding a template to obtain gel;
(2) crystallizing the gel obtained in the step (1), and performing post-treatment to obtain the AHT-configuration molecular sieve;
the template agent in the step (1) comprises any one or the combination of at least two of di-n-butylamine, dipentylamine, di-n-hexylamine, di-n-heptylamine or di-n-octylamine.
The invention adopts the novel low-toxicity organic template agent, not only can prepare the pure-phase AHT-shaped molecular sieve, reduce the preparation cost of the molecular sieve, but also obviously improve the greenness of the production process of the molecular sieve material, and the prepared molecular sieve has more uniform particle size distribution and is convenient for the subsequent molding operation.
Preferably, the aluminum source in step (1) comprises any one of activated alumina, pseudoboehmite, aluminum hydroxide, aluminum isopropoxide or aluminum sulfate or a combination of at least two of the same.
Preferably, the source of phosphorus comprises any one of orthophosphoric acid, monoammonium phosphate or monoammonium phosphate, or a combination of at least two of these.
In the present invention, the aluminum source is considered to contain Al2O3In the form of (1), in combination with Al2O3The molar amount of the raw materials is calculated, for example: aluminum hydroxide, i.e., Al (OH)3The two molecules of aluminum hydroxide comprise one molecule of aluminum oxide, and the dosage of the aluminum source is calculated.
The phosphorus source is considered to contain P in the invention2O5In combination with P2O5The molar amount of the raw materials is calculated, for example: orthophosphoric acid, i.e. H3PO3Can be regarded as two molecules of H3PO3Containing a molecule of P2O5And a molecule H2And O, calculating the feeding amount of the aluminum source.
Preferably, the solvent comprises deionized water.
Preferably, the temperature of the aging treatment in step (1) is room temperature.
Preferably, the aging treatment time is 4-24 h, such as: 4h, 8h, 10h, 15h, 20h or 24h and the like.
Preferably, the template is added while stirring.
Preferably, the stirring time is 15-60 min, such as: 15min, 20min, 30min, 40min, 50min or 60min and the like.
Preferably, Al in the aluminum source in the step (1)2O3P in a phosphorus source2O5The molar ratio of the template agent to the solvent is 1 (0.5-1.5) to (0.8-1.5) to (20-100), for example: 1:1.5:0.8: 20. 1:0.8:1.2:50, 1:1.2:1:80, 1:1.3:1.9:60 or 1:1.5:1.5:100, etc., preferably 1: 0.75-1.25: 20-50: 40-80.
Preferably, the crystallization device in step (2) comprises a polytetrafluoroethylene-lined high-pressure reaction kettle.
Preferably, the temperature of the crystallization treatment is 100-130 ℃, for example: 100 ℃, 110 ℃, 120 ℃, 125 ℃, 130 ℃ or the like.
Preferably, the time of the crystallization treatment is 12-48 h, for example: 12h, 15h, 18h, 20h or 24h and the like.
The method has mild reaction conditions, and the crystallization temperature does not exceed 130 ℃ in the crystallization process.
Preferably, the crystallization treatment in the step (2) is followed by post-treatment.
Preferably, the post-treatment comprises suction washing and drying.
Preferably, the washing agent for suction filtration washing comprises deionized water and/or ethanol.
Preferably, the drying temperature is 55-75 ℃, for example: 55 deg.C, 58 deg.C, 60 deg.C, 65 deg.C, 70 deg.C or 75 deg.C.
As a preferable scheme of the invention, the preparation method comprises the following steps:
(1) mixing an aluminum source, a phosphorus source and a solvent to obtain a mixture precursor, aging the mixture precursor for 4-24 hours, and adding a template agent to obtain gel, wherein the molar ratio of the aluminum source to the phosphorus source to the template agent to the solvent is 1 (0.5-1.5) to (0.8-1.5) to (20-100);
(2) and (2) crystallizing the gel obtained in the step (1) at 100-130 ℃ for 12-18 h, and filtering, washing and drying to obtain the AHT-configuration molecular sieve.
In a second aspect, the present invention provides an AHT-configured molecular sieve produced by the process of the first aspect.
In a third aspect, the present invention also provides the use of an AHT-configured molecular sieve according to the second aspect as a specific adsorbent for any one of alcohol, organic chloride or water.
Compared with the prior art, the invention has the following beneficial effects:
(1) compared with the traditional template agent, the novel template agent is adopted, so that not only can the pure-phase AHT molecular sieve be prepared, but also the cost for preparing the AHT type molecular sieve is reduced, and meanwhile, the greenness of the molecular sieve material production process is obviously improved.
(2) The method has mild reaction conditions, the crystallization temperature does not exceed 130 ℃ in the crystallization process, the solvent amount used in the preparation process is small, the wave of the solvent is reduced, the particle size distribution of the prepared molecular sieve is more uniform, and the subsequent molding operation is convenient
Drawings
FIG. 1 is a scanning electron micrograph of the AHT-configured molecular sieve obtained in example 1.
Figure 2 is an XRD pattern of the AHT configuration molecular sieve obtained in example 1.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Example 1
This example provides an AHT-configured molecular sieve, which is prepared as follows:
(1) 6.24g of pseudo-boehmite (78.6 wt% Al)2O3(0.048mol)) was placed in a 50ml beaker, 9g (0.5mol) of deionized water was added, stirring was carried out at room temperature for 15min, and 16.423g of an orthophosphoric acid solution (molecular formula of orthophosphoric acid H) diluted with 9g (0.5mol) of deionized water was added3PO3Can be regarded as two molecules of H3PO3Containing a molecule of P2O5And a molecule H2O, and then gives P2O5The molar weight of the precursor is 0.048mol), stirring for 30min at room temperature to obtain a mixture precursor, placing the mixture precursor in air for aging for 8h, adding 7.334g (0.039mol) of di-n-hexylamine template into the aged mixture precursor, and continuously stirring for 20min to obtain gel;
(2) and (2) pouring the gel obtained in the step (1) into a polytetrafluoroethylene lining hydrothermal reaction kettle, crystallizing at 120 ℃ for 24 hours, carrying out suction filtration, washing for 3 times by using absolute ethyl alcohol, and drying at 60 ℃ to obtain the AHT-shaped molecular sieve.
The scanning electron micrograph of the AHT-configuration molecular sieve is shown in figure 1.
The XRD pattern of the molecular sieve with AHT configuration is shown in figure 2, and as can be seen from figure 2, the molecular sieve has AHT configuration.
Example 2
This example provides an AHT-configured molecular sieve, which is prepared as follows:
(1) 6.24g of pseudo-boehmite (78.6 wt% Al)2O3(0.048mol)) was placed in a 50ml beaker, 10.3g (0.57mol)) of deionized water was added, stirring was carried out at room temperature for 15min, and 20.023g of orthophosphoric acid solution (P) diluted with 10.3g of deionized water was added2O5The molar weight of the gel is 0.058mol), stirring for 30min at room temperature to obtain a mixture precursor, placing the mixture precursor in air for aging for 8h, adding 7.334g (0.039mol) of di-n-hexylamine template agent into the aged gel, and continuously stirring for 20min to obtain gel;
(2) and (2) pouring the gel obtained in the step (1) into a polytetrafluoroethylene lining hydrothermal reaction kettle, crystallizing at 120 ℃ for 24 hours, carrying out suction filtration, washing for 3 times by using absolute ethyl alcohol, and drying at 60 ℃ to obtain the AHT-shaped molecular sieve.
Example 3
This example provides an AHT-configured molecular sieve, which is prepared as follows:
(1) 6.24g of pseudo-boehmite (78.6 wt% Al)2O3(0.048mol)) was placed in a 50ml beaker, 14.4g (0.8mol) of deionized water was added, stirring was carried out at room temperature for 15min, and 23.623g of orthophosphoric acid solution (P) diluted with 14.4g (0.8mol) of deionized water was added2O5The molar weight of the precursor is 0.069mol), stirring for 30min at room temperature to obtain a precursor mixture, putting the precursor mixture in air for aging for 8h, adding 7.334g (0.039mol) of di-n-hexylamine template agent into the aged precursor mixture, and continuously stirring for 20min to obtain gel;
(2) and (2) pouring the gel obtained in the step (1) into a polytetrafluoroethylene lining hydrothermal reaction kettle, crystallizing at 120 ℃ for 24 hours, carrying out suction filtration, washing for 3 times by using absolute ethyl alcohol, and drying at 60 ℃ to obtain the AHT-shaped molecular sieve.
Example 4
This example provides an AHT-configured molecular sieve, which is prepared as follows:
(1) 4.942g of pseudo-boehmite (78.6 wt% Al)2O3(0.038mol)) was placed in a 50ml beaker, 7.2g (0.4mol) of deionized water was added, stirring was carried out at room temperature for 15min, and 16.423g of orthophosphoric acid solution (P) diluted with 7.2g (0.4mol) of deionized water was added2O5The molar weight of the precursor is 0.048mol), stirring for 30min at room temperature to obtain a mixture precursor, placing the mixture precursor in air for aging for 8h, adding 11.001g (0.059mol) of di-n-hexylamine template agent into the aged mixture precursor, and continuously stirring for 20min to obtain gel;
(2) and pouring the gel obtained in the example 1 into a polytetrafluoroethylene lining hydrothermal reaction kettle, crystallizing at 120 ℃ for 24 hours, carrying out suction filtration, washing for 3 times by using absolute ethyl alcohol, and drying at 60 ℃ to obtain the AHT-configuration molecular sieve.
Example 5
(1) 4.942g of pseudo-boehmite (78.6 wt% Al)2O3(0.038mol)) was placed in a 50ml beaker, 9.0g (0.5mol) of deionized water was added, stirring was carried out at room temperature for 15min, and 16.379g (P) diluted with 9.0g (0.5mol) of deionized water was added2O5The molar weight of 0.047mol), stirring for 30min at room temperature to obtain a mixture precursor, and placing the mixture precursor in the airAging for 8h, adding 7.334g (0.039mol) of di-n-hexylamine template agent into the aged mixture precursor, and continuing stirring for 20min to obtain gel;
(2) and (2) pouring the gel obtained in the step (1) into a polytetrafluoroethylene lining hydrothermal reaction kettle, crystallizing at 120 ℃ for 24 hours, carrying out suction filtration, washing for 3 times by using absolute ethyl alcohol, and drying at 60 ℃ to obtain the AHT-shaped molecular sieve.
Example 6
(1) 4.942g of pseudo-boehmite (78.6 wt% Al)2O3(0.038mol)) was placed in a 50ml beaker, 9.0g (0.5mol) of deionized water was added, stirring was carried out at room temperature for 15min, and 20.068g (P) diluted with 9.0g (0.5mol) of deionized water was added2O5The molar weight of the precursor is 0.057mol), stirring for 30min at room temperature to obtain a mixture precursor, putting the mixture precursor in air for aging for 8h, adding 7.334g of di-n-hexylamine template into the aged mixture precursor, and continuously stirring for 20min to obtain gel;
(2) and (2) pouring the gel obtained in the step (1) into a polytetrafluoroethylene lining hydrothermal reaction kettle, crystallizing at 120 ℃ for 24 hours, carrying out suction filtration, washing for 3 times by using absolute ethyl alcohol, and drying at 60 ℃ to obtain the AHT-shaped molecular sieve.
Example 7
This example is different from example 1 only in that the crystallization temperature in step (2) is 100 ℃, and other conditions and parameters are exactly the same as those in example 1.
Example 8
This example is different from example 1 only in that the crystallization temperature in step (2) is 130 ℃, and other conditions and parameters are exactly the same as those in example 1.
Comparative example 1
Slowly adding orthophosphoric acid solution with the mass concentration of 85% into the boehmite slurry under stirring to obtain initial aluminum phosphate gel, and aging the gel for 8 hours; taking the aged gel, dropwise adding dipentamine under stirring to obtain a reaction precursor, wherein the final precursor mixture comprises the following components in molar composition: a12O3：P2O5：xH2O1: 1:1:45, and reacting the precursor at room temperatureStirring for 15min, transferring to high pressure kettle, crystallizing at 120 deg.C for 15 hr, suction filtering and washing the product with distilled water, and drying the washed product at room temperature in air to obtain AHT type molecular sieve.
And (3) performance testing:
the adsorption performance of methanol, ethanol, ethyl acetate and water of the sample is tested by a steam adsorption instrument. Taking the AHT-shaped molecular sieve obtained in the examples 1 to 8 and the comparative example 1, putting the AHT-shaped molecular sieve into a sample tube, activating the sample tube for 5 hours at 60 ℃ under a vacuum condition, removing water and other adsorbates in the sample, then reducing the temperature to 20 ℃ to test the adsorption performance of the AHT-shaped molecular sieve on the sample tube by taking methanol, ethanol, ethyl acetate or water vapor as adsorbate, wherein the test results are shown in Table 1:
TABLE 1
As can be seen from Table 1, the comparison of examples 1-8 shows that the adsorption capacity of methanol and the adsorption capacity of ethanol of the AHT type molecular sieve prepared by the invention can reach more than 1.15mmol/g, the adsorption capacity of ethanol can reach more than 0.75mmol/g, the adsorption capacity of methanol and the adsorption capacity of ethyl acetate are only about 0.40mmol/g and 0.12mmol/g respectively, the adsorption capacity of methanol and the adsorption capacity of ethanol of the AHT type molecular sieve prepared by adjusting the molar ratio of the aluminum source, the phosphorus source, the template agent and the solvent and the crystallization temperature can reach as high as 1.51mmol/g and 1.05mmol/g, and the adsorption capacity of water and ethyl acetate is only 0.47mmol/g and 0.14mmol/g, which shows the specific adsorption of methanol and ethanol.
Comparing the embodiment 1 with the embodiments 7 to 8, the crystallization temperature shown in the step (2) affects the adsorption effect of the prepared AHT molecular sieve, the crystallization temperature is controlled to be 100 to 130 ℃, the AHT molecular sieve with better adsorption cross can be prepared, if the crystallization temperature is too low, the crystallization of the AHT molecular sieve is incomplete, and a part of raw materials which cannot be completely crystallized can be obtained in the product, so that the adsorption performance is reduced; if the crystallization temperature is too high, the AHT molecular sieve can be further transformed into other configuration products, and the adsorption performance can also be reduced.
Comparing example 1 with comparative example 1, the present invention can prepare an AHT type molecular sieve having an adsorption effect not inferior to that of the AHT type molecular sieve prepared by using a template having a low toxicity and a high price.
The applicant declares that the above description is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and it should be understood by those skilled in the art that any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are within the scope and disclosure of the present invention.
Claims (10)
1. A preparation method of an AHT configuration molecular sieve is characterized by comprising the following steps:
(1) mixing an aluminum source, a phosphorus source and a solvent to obtain a mixture precursor, aging the mixture precursor, and adding a template to obtain gel;
(2) crystallizing the gel obtained in the step (1) to obtain the AHT-configuration molecular sieve;
wherein, the template agent in the step (1) comprises any one or the combination of at least two of di-n-butylamine, dipentylamine, di-n-hexylamine, di-n-heptylamine or di-n-octylamine.
2. The method of claim 1, wherein the aluminum source of step (1) comprises any one of activated alumina, pseudoboehmite, aluminum hydroxide, aluminum isopropoxide or aluminum sulfate or a combination of at least two thereof;
preferably, the phosphorus source comprises any one of orthophosphoric acid, ammonium monohydrogen phosphate or ammonium dihydrogen phosphate, or a combination of at least two of the foregoing;
preferably, the solvent comprises deionized water.
3. The method according to claim 1 or wherein the temperature of the aging treatment in step (1) is room temperature;
preferably, the aging treatment time is 4-24 h.
4. The method according to any one of claims 1 to 3, wherein the template is added while stirring;
preferably, the stirring time is 15-60 min.
5. The method of any one of claims 1-4, wherein Al in the aluminum source of step (1)2O3P in a phosphorus source2O5The molar ratio of the template agent to the solvent is 1 (0.5-1.5) to (0.8-1.5) to (20-100).
6. The method according to any one of claims 1 to 5, wherein the crystallization apparatus in the step (2) comprises a polytetrafluoroethylene-lined autoclave;
preferably, the temperature of the crystallization treatment is 100-130 ℃;
preferably, the crystallization treatment time is 12-48 h.
7. The method according to any one of claims 1 to 6, wherein the crystallization treatment in the step (2) is followed by a post-treatment;
preferably, the post-treatment comprises suction filtration washing and drying;
preferably, the washing agent for suction filtration washing comprises deionized water and/or ethanol;
preferably, the drying temperature is 55-75 ℃.
8. The method of any one of claims 1 to 7, comprising the steps of:
(1) mixing an aluminum source, a phosphorus source and a solvent to obtain a mixture precursor, aging the mixture precursor for 4-24 hours, and adding a template to obtain gel, wherein the molar ratio of the aluminum source to the phosphorus source to the template to the solvent is 1 (0.5-1.5) to (0.8-1.5) to (20-100), and the molar ratio of the aluminum source to the phosphorus source to the template to the solvent is preferably 1 (0.75-1.25) to (20-50) to (40-80);
(2) and (2) crystallizing the gel obtained in the step (1) at 100-130 ℃ for 12-18 h, and filtering, washing and drying to obtain the AHT-configuration molecular sieve.
9. An AHT configured molecular sieve, wherein said AHT configured molecular sieve is produced by the method of any one of claims 1 to 8.
10. Use of the AHT-configured molecular sieve of claim 9 as a specific adsorbent for any of an alcohol, an organic chloride, or water.
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