Rare earth-containing Li-LSX zeolite as well as preparation method and application thereof

A zeolite and rare earth technology, applied in the chemical industry, can solve the problems of poor oxygen adsorption performance, low lithium exchange degree, high cost, etc., and achieve the effects of reduced condition control requirements, simple and easy-to-control preparation process, and reduced consumption and cost.

Pending Publication Date: 2021-11-26
REZEL CATALYSTS CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This type of prior art mainly uses kaolin as a binder. After high-temperature roasting, a mixed solution of sodium hydroxide or sodium silicate is used for aging crystallization. The kaolin product is mainly converted into A-type zeolite or X-type zeolite, but its Smaller adsorption capacity than LSX zeolite
[0012] Chinese patent CN101524637A also discloses a preparation method of a binder-free adsorbent rich in LSX zeolite. This patent uses NaLSX as an active component and kaolin as a binder, by adding an alkali source and a silicon source (which can be (without adding) for molding and roasting, and crystallization by adding sodium hydroxide lye to convert the kaolin binder into X-type zeolite, but the product has a relatively high silicon-alumina ratio, which affects the adsorption capacity
In a Li-modified X molecular sieve disclosed in Chinese patent ZL201110305323.8 and its preparation method, the original X zeolite powder is first exchanged with ammonium salt, and then the lithium salt solution is impregnated on the zeolite by an impregnation method, and then dried and roasted to obtain LiX, but it is still an X-type zeolite, and its adsorption performance is still poor
[0034] Chinese patents CN101125664A, CN100556808C, and ZL200710121786.2 all disclose an ion exchange method for preparing lithium-type low-silicon-aluminum X-type zeolite. F

Method used

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  • Rare earth-containing Li-LSX zeolite as well as preparation method and application thereof
  • Rare earth-containing Li-LSX zeolite as well as preparation method and application thereof
  • Rare earth-containing Li-LSX zeolite as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0099] This example is used to illustrate the implementation process of the preparation method of the present invention and the prepared rare earth-containing Li-LSX zeolite.

[0100] In 0.6 liters of deionized water, add 0.4 liters of water glass (industrial grade, SiO 2 =250g / L, modulus 3.2, Leshan Branch of Runhe Catalyst Co., Ltd.) and 0.5 liters of low alkalinity sodium metaaluminate (industrial grade, Al 2 o 3 = 100 g / L, Na 2 O=150 g / L, same as above), after uniform stirring, static crystallization at 95° C. for 6 hours.

[0101] After filtration, exchange with 4wt% cerium nitrate solution (prepared by industrial grade cerium nitrate, as above) at 85°C for 1 hour at a liquid / solid ratio of 5:1, dry and roast at 450°C for 1 hour, and then Next exchange once, the filtrate is collected and reserved for reuse next time.

[0102] After filtering, mix with 800 grams of zirconium beads with a diameter of 1 mm in a micro-stirring mill and grind for 2 hours at a speed of 80 r...

Embodiment 2

[0119] This example is used to illustrate the convenient and controllable increase of the rare earth content of the rare earth-containing Li-LSX zeolite prepared under the high exchange degree of lithium ions by adopting the method of the present invention.

[0120] Add 0.7 liters of water glass (same as above) and 1 liter of low-basic sodium metaaluminate (same as above) to 1.5 liters of deionized water and mix well, then add at room temperature, mix and stir and statically crystallize at 92°C for 8 hours.

[0121] After filtering, use the reclaimed filtrate that contains cerium nitrate earlier, exchange it at 80°C for 2 hours by the ratio of liquid / solid 20:1, dry and roast at 400°C for 2 hours, then use 4wt% cerium nitrate solution ( Same as above) exchanged at 80° C. for 2 hours, and recovered the filtrate exchanged with rare earth.

[0122] After filtering, mix and grind with 1.5 kg of zirconium beads with a diameter of 1 mm in a small stirring mill for 2 hours at a speed...

Embodiment 3

[0126] This example is used to illustrate the method of the present invention, under the condition of high exchange degree of lithium ions, it is convenient and controllable to prepare Li-LSX zeolite with higher rare earth content.

[0127] Add 1.5 liters of water glass (same as above) and 2 liters of low-alkalinity sodium metaaluminate (same as above) into 2.5 liters of deionized water and mix evenly. After mixing and stirring evenly, statically crystallize at 96° C. for 5 hours.

[0128] After filtration, exchange the filtrate with the recovered cerium ion at 90°C for 1 hour at a ratio of liquid / solid 10:1, and repeat the exchange once, dry and roast at 420°C for 1.5 hours, and then use 4wt% cerium nitrate solution Exchange under the same temperature conditions for 1 hour at the ratio of liquid / solid 5:1.

[0129] After filtering, mix and grind with 3 kg of zirconium beads with a diameter of 1 mm in a small stirring mill for 2 hours at a speed of 60 rpm. After sieving the zi...

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Abstract

The invention relates to rare earth-containing Li-LSX zeolite and a preparation method thereof, and belongs to the technical field of chemical engineering. The preparation method comprises the following steps: (1) adding a silicon source, an aluminum source and caustic alkali according to the molar ratio of M2O/SiO2 = 1-1.5, the molar ratio of SiO2/Al2O3 = 2.5-5 and the molar ratio of H2O/SiO2 = 45-50, mixing and stirring, and crystallizing at 80-100 DEG C for 5-10 hours; (2) after filtering, exchanging a product with a rare earth salt solution for 1-2 times, and roasting at 350-550 DEG C for 0.5-3 hours after primary exchange; (3) after grinding, supplementing and adding a silicon source, an aluminum source and caustic alkali according to the proportion of 40%-95% of the total mass of a dry basis, enabling the total molar ratio of materials to be M2O/SiO2 = 3.5-4 (the molar ratio of Na/K of alkali metal M is 2.5-3.5), SiO2/Al2O3 = 1.5-2 and H2O/SiO2 = 70-75, stirring, aging for 1-3 days, and crystallizing again at 60-80 DEG C for 10-25 hours; and (4) after filtration and ammonium salt exchange, carrying out ion exchange for 2-5 times by using a lithium compound solution, and roasting for 1-2 times at intervals at 300-430 DEG C/0.5-3 hours. The lithium salt utilization rate is high in preparation, the product composition and performance are easy to adjust, and the product has better adsorption separation performance when being used as an oxygen production adsorbent.

Description

technical field [0001] The invention relates to a rare earth-containing Li-LSX zeolite and its preparation method and application, in particular to a low-silicon-aluminum-ratio X-type zeolite containing cerium and lithium, its preparation method and the process of oxygen separation and purification The application belongs to the field of chemical technology. Background technique [0002] The fields of application of oxygen and nitrogen are becoming more and more extensive, and the demand is also increasing. Among them, oxygen is the basis for human survival, and because of its strong oxidizing properties and life-sustaining properties, as an important chemical raw material, it is widely used in petrochemical, chemical synthesis, iron and steel smelting, nonferrous metallurgy, metal cutting and welding , paper industry, fish farming, plateau operations, tunnel construction, wastewater treatment and environmental protection and other aspects. With the continuous improvement ...

Claims

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Application Information

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IPC IPC(8): B01J20/18B01J20/30B01D53/047
CPCB01J20/18B01D53/047
Inventor 卓润生杜爱华张明远刘新生
Owner REZEL CATALYSTS CORP
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