CN114988427A - Preparation method and application of small-grain low-silicon X-type molecular sieve - Google Patents
Preparation method and application of small-grain low-silicon X-type molecular sieve Download PDFInfo
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- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
- 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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- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
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Abstract
The invention discloses a preparation method and application of a small-grain low-silicon X-type molecular sieve, which mainly comprises the following steps: s1, SiO (16-17) 2 :Al 2 O 3 :(12～18)Na 2 O:(3～6)K 2 O:(300～350)H 2 Preparing a directing agent according to the molar ratio of O; s2, SiO (1.95-2.05) 2 :Al 2 O 3 :(4.8～6)Na 2 O:(1.8～2.3)K 2 O:(130～140)H 2 Crystallizing the molar ratio of O to obtain a seed crystal solution; s3, centrifugal washing; and S4, flash evaporation drying to obtain a sample. Compared with the LSX molecular sieve synthesized by the prior art, the small-grain low-silicon X molecular sieve with the size of 1 mu m is prepared by optimizing the molar ratio of the formula, and the water adsorption of the molecular sieve is not less than 32Percent, carbon dioxide adsorption is more than or equal to 24ml/g, and when the catalyst is applied to gas separation, N is 2 The adsorption capacity is more than or equal to 11ml/g, and the oxygen generation performance is further improved.
Description
Technical Field
The invention relates to the technical field of X-type molecular sieves, in particular to a preparation method and application of a small-grain low-silicon X-type molecular sieve.
Background
The molecular sieve is an artificially synthesized hydrated aluminosilicate or natural zeolite with the function of screening molecules, is one of important inorganic porous materials, and has important application in the fields of gas separation and purification. Nitrogen and oxygen are important chemical raw materials, and high-purity oxygen is widely applied to the fields of steel industry, chemical industry, medical care, papermaking, sewage treatment and the like; high purity nitrogen is mainly used as a sealing gas, a purge gas and a shielding gas for food processing. The efficient and low-cost separation of oxygen and nitrogen from air is of great commercial and practical significance. The main method for air separation at present is a low-temperature rectification method, and the principle of the method is that air is liquefied at low temperature and is separated according to different boiling points of components, however, the boiling points of the components in the air are very close, and a large number of distillation trays are needed for achieving an excellent separation effect, so that the method has the defect of high energy consumption; the principle of the pressure swing adsorption method is that nitrogen, oxygen or argon is selectively adsorbed by an adsorbent to realize nitrogen-oxygen-argon separation, and the mechanism of a molecular sieve in the PSA air separation oxygen production process is mainly as follows: using air as raw material, molecular sieve pair N 2 Has an adsorption capacity greater than that of O 2 Adsorption capacity of (2) that the molecular sieve adsorbs N as much as possible under high pressure 2 Thereby enriching O 2 Then the molecular sieve is desorbed and activated under lower pressure to carry out effective continuous gas separation to reach N 2 、O 2 The purpose of the separation is. The pressure swing adsorption method has the advantages of low energy consumption, high product purity, simple equipment, energy conservation, economy and high degree of automation, is rapidly developed in recent years, has more and more extensive application, and gradually becomes a main technology of the air separation industry.
Passing LSX type molecular sieve through Li + The Li-LSX molecular sieve prepared after exchange can obviously improve the nitrogen-oxygen separation coefficient and increase the nitrogen adsorption capacity, and is suitable for N in the air separation industry 2 、O 2 The separation effect is better, the adsorption separation performance is better, and the adsorbent is the most ideal pressure swing adsorption nitrogen-oxygen separation adsorbent at present, so the adsorbent has important significance for the research of the LSX type molecular sieve. The low-silicon LSX molecular sieve synthesized by the prior art has larger size of 3-5 mu m, and the oxygen generation performance, the nitrogen adsorption capacity, the water adsorption capacity and the carbon dioxide adsorption capacity need to be improvedFurther lifting is to be performed.
Disclosure of Invention
In order to solve the problem that the size of the low-silicon LSX molecular sieve is larger in the prior art and further improve the oxygen production performance, the nitrogen adsorption capacity, the water adsorption capacity and the carbon dioxide adsorption capacity, a preparation method and application of the small-grain low-silicon X-type molecular sieve are provided.
A preparation method of a small-grain low-silicon X-type molecular sieve comprises the following steps:
s1, preparing a guiding agent: according to (16-17) SiO 2 :Al 2 O 3 :(12～18)Na 2 O:(3～6)K 2 O:(300～350)H 2 According to the molar ratio of O, sequentially adding NaOH, a potassium source and an aluminum source into pure water while stirring until the NaOH, the potassium source and the aluminum source are completely dissolved, continuously stirring for cooling, adding a silicon source after cooling, continuously stirring for 0.5-1 h, refrigerating, and keeping the temperature for 24h to prepare a guiding agent;
s2, crystallization: according to (1.95-2.05) SiO 2 :Al 2 O 3 :(4.8～6)Na 2 O:(1.8～2.3)K 2 O:(130～140)H 2 Adding NaOH, a potassium source and an aluminum source into a solvent in sequence while stirring until the NaOH, the potassium source and the aluminum source are completely dissolved, stirring and cooling, adding a silicon source and a directing agent prepared from S1, stirring at normal temperature for 0.5-1 h, stopping stirring, aging for 3h, continuously stirring, heating to 40-80 ℃, stopping stirring, standing, keeping the temperature for 5-8 h, continuously stirring, heating to 80-100 ℃, stopping stirring, and standing, keeping the temperature for 3-6 h;
s3, centrifugal washing: centrifugally washing the crystallized material in a centrifuge until the pH value of the material is less than or equal to 11;
s4, flash drying: and (4) carrying out flash evaporation drying on the centrifugally washed material in a flash evaporation machine.
Preferably, the addition amount of the directing agent in S2 is 10% to 20% of the weight of the silicon source.
Preferably, the silicon source is water glass, the aluminum source is sodium metaaluminate, and the potassium source is potassium hydroxide.
Preferably, the mixing temperature of the materials in the S4 in the flash evaporation machine is 120-150 ℃, and the air outlet temperature is 60-90 ℃.
Preferably, the refrigerating temperature in S1 is 0-10 ℃.
The application of small-grain low-silicon X-type molecular sieve is characterized by being applied to the field of nitrogen or oxygen production, wherein N is 2 The adsorption capacity is more than or equal to 32 ml/g.
Has the advantages that:
compared with the LSX molecular sieve synthesized by the prior art, the small-grain low-silicon X molecular sieve with the size of 1 mu m is prepared by optimizing the proportion of the components, the water absorption of the molecular sieve is more than or equal to 32 percent, the carbon dioxide absorption is more than or equal to 24ml/g, and N is N when the small-grain low-silicon X molecular sieve is applied to gas separation 2 The adsorption capacity is more than or equal to 11ml/g, and the oxygen generation performance is further improved.
Drawings
Fig. 1 is an SEM image a of a small-grained low-silicon type X molecular sieve.
Fig. 2 is SEM image B of small-grained low-silicon type X molecular sieve.
Fig. 3 is SEM image C of small-grained low-silicon type X molecular sieve.
Fig. 4 is SEM image D of small-grained low-silicon type X molecular sieve.
Detailed Description
For the purpose of enhancing the understanding of the present invention, the present invention will be further described in detail with reference to the following examples and the accompanying drawings, which are only used for explaining the present invention and are not to be construed as limiting the scope of the present invention.
The first embodiment is as follows:
weighing 205.8g of pure water in a 1L beaker, adding magnetons, placing on a magnetic stirring platform, respectively weighing and adding 37g of sodium hydroxide, 32g of potassium hydroxide and 13.6g of sodium metaaluminate while stirring for dissolving, stirring and cooling, adding 237g of water glass after the temperature is reduced to be below 40 ℃, stirring for half an hour, stopping stirring, placing the beaker into a refrigerator, setting the temperature to be 0-10 ℃, and preserving the heat for 24 hours to obtain the guiding agent.
Adding 2122g of water into a 5L reaction kettle, starting stirring, respectively weighing and adding 255g of sodium hydroxide, 264g of potassium hydroxide and 204g of sodium metaaluminate while stirring for dissolving, stirring and cooling to below 40 ℃, adding 440g of water glass and 11.88g of directing agent, stirring at normal temperature for 30 minutes, stopping stirring, aging for 3 hours, continuing stirring and heating to 50 ℃, stopping stirring, standing and keeping the temperature for 6 hours, continuing stirring and heating to 90 ℃, stopping stirring, standing and keeping the temperature for 4 hours, discharging, performing suction filtration and washing to obtain the sample molecular sieve.
Example two:
weighing 205.8g of pure water in a 1L beaker, adding magnetons, placing on a magnetic stirring platform, respectively weighing and adding 37g of sodium hydroxide, 32g of potassium hydroxide and 13.6g of sodium metaaluminate while stirring for dissolving, stirring and cooling, adding 237g of water glass after the temperature is reduced to be below 40 ℃, stirring for half an hour, stopping stirring, placing the beaker into a refrigerator, setting the temperature to be 0-10 ℃, and preserving the heat for 24 hours to obtain the guiding agent.
Adding 2030g of water into a 5L reaction kettle, starting stirring, respectively weighing 296g of sodium hydroxide, 216g of potassium hydroxide and 225g of sodium metaaluminate while stirring for dissolving, stirring and cooling to below 40 ℃, adding 445g of water glass and 18g of directing agent 1, stirring at normal temperature for 1 hour, stopping stirring, aging for 3 hours, continuing stirring and heating to 60 ℃, stopping stirring, standing and keeping the temperature for 5 hours, continuing stirring and heating to 95 ℃, stopping stirring, standing and keeping the temperature for 3 hours, discharging, performing suction filtration and washing to obtain the sample molecular sieve.
Example three:
265.8g of pure water is weighed in a 1L beaker, magnetons are added and placed on a magnetic stirring platform, 31.59g of sodium hydroxide, 40g of potassium hydroxide and 13.6g of sodium metaaluminate are respectively weighed and added while stirring for dissolving, the temperature is reduced to below 40 ℃, 237g of water glass is added, the stirring is stopped after half an hour, the beaker is placed in a refrigerator, the temperature is set to be 0-10 ℃, and the temperature is kept for 24 hours to obtain the guiding agent.
Adding 2203g of water into a 5L reaction kettle, starting stirring, respectively weighing and adding 335g of sodium hydroxide, 353g of potassium hydroxide and 204g of sodium metaaluminate while stirring for dissolving, stirring and cooling to below 40 ℃, adding 455g of water glass and 24g of directing agent, stirring at normal temperature for 1 hour, stopping stirring, aging for 3 hours, continuing stirring and heating to 50 ℃, stopping stirring, standing and keeping the temperature for 7 hours, continuing stirring and heating to 90 ℃, stopping stirring, standing and keeping the temperature for 3 hours, discharging, performing suction filtration and washing to obtain the sample molecular sieve.
The SEM image of the small-grain low-silicon X-type molecular sieve is shown in the attached drawing, the size of the small-grain low-silicon X-type molecular sieve prepared by the embodiment is 1 mu m, the water adsorption of the molecular sieve is more than or equal to 32 percent, the carbon dioxide adsorption is more than or equal to 24ml/g, and when a sample is applied to gas separation through lithium salt exchange, N is added 2 The adsorption capacity is more than or equal to 11ml/g, and the oxygen generation performance is further improved.
As a further improvement, the above-mentioned is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (6)
1. A preparation method of a small-grain low-silicon X-type molecular sieve is characterized by comprising the following steps:
s1, preparing a guiding agent: according to (16-17) SiO 2 :Al 2 O 3 :(12～18)Na 2 O:(3～6)K 2 O:(300～350)H 2 Sequentially adding NaOH, a potassium source and an aluminum source into pure water while stirring until the NaOH, the potassium source and the aluminum source are completely dissolved, continuously stirring for cooling, adding a silicon source after cooling, continuously stirring for 0.5-1 h, refrigerating, and keeping the temperature for 24h to prepare a guiding agent;
s2, crystallization: according to (1.95-2.05) SiO 2 :Al 2 O 3 :(4.8～6)Na 2 O:(1.8～2.3)K 2 O:(130～140)H 2 Adding NaOH, a potassium source and an aluminum source into a solvent in sequence while stirring until the NaOH, the potassium source and the aluminum source are completely dissolved, stirring and cooling, adding a silicon source and a directing agent prepared from S1, stirring at normal temperature for 0.5-1 h, stopping stirring, aging for 3h, continuously stirring, heating to 40-80 ℃, stopping stirring, standing, keeping the temperature for 5-8 h, continuously stirring, heating to 80-100 ℃, stopping stirring, and standing, keeping the temperature for 3-6 h;
s3, centrifugal washing: centrifugally washing the crystallized material in a centrifuge until the pH value of the material is less than or equal to 11;
s4, flash drying: and (4) carrying out flash evaporation drying on the centrifugally washed material in a flash evaporation machine.
2. The method for preparing the small-grained low-silicon X-type molecular sieve according to claim 1, wherein the guiding agent in S2 is added in an amount of 10-20% by weight based on the weight of the silicon source.
3. The method as claimed in claim 1, wherein the silicon source is water glass, the aluminum source is sodium metaaluminate, and the potassium source is potassium hydroxide.
4. The method for preparing the small-grain low-silicon X-type molecular sieve of claim 1, wherein the mixing temperature of the materials in the S4 in a flash evaporation machine is 120-150 ℃, and the air outlet temperature is 60-90 ℃.
5. The method for preparing the small-grained low-silicon X-type molecular sieve according to claim 1, wherein the refrigeration temperature in S1 is 0-10 ℃.
6. Use of a small-grained low-silicon X-type molecular sieve according to any one of claims 1 to 5 in the field of nitrogen or oxygen production, N 2 The adsorption capacity is more than or equal to 11 ml/g.
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