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X zeolite molecular sieve and preparation method thereof

A zeolite molecular sieve and alkaline technology, which is applied in the field of molecular sieves, can solve the problems of high energy consumption and complicated process of high-temperature roasting, and achieve the effects of good crystallinity, simple process and reduced energy consumption

Active Publication Date: 2020-04-03
JILIN UNIV
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Problems solved by technology

For example, Hu Ting et al. (see Hu Ting et al., Synthetic NaX Molecular Sieve Structural Characterization and Adsorption Properties Research [J]. University Chemical Engineering Journal, 2013, 27 (4) 708-713) disclosed the preparation of NaX molecular sieves by using lithium slag. Wash the lithium slag with water to remove the quartz contained in it, roast the obtained lithium slag and sodium hydroxide solid at high temperature (600°C) for alkali fusion, mix the alkali-fused lithium slag and water evenly, age for 10-18 hours, and then crystallize to obtain NaX Molecular sieve; the process is complex and high-temperature roasting consumes a lot of energy

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  • X zeolite molecular sieve and preparation method thereof

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preparation example Construction

[0026] The present invention provides a kind of preparation method of X zeolite molecular sieve, comprises the following steps:

[0027] The lithium slag and the sodium-containing alkaline compound are first mixed and activated to obtain an activated material; the activation temperature is 180-220°C;

[0028] Mixing the activated material and water for the second time to obtain a sol;

[0029] The sol is hydrothermally crystallized to obtain X zeolite molecular sieve.

[0030] In the present invention, unless otherwise specified, all raw material components are commercially available products well known to those skilled in the art.

[0031] In the invention, the lithium slag and the sodium-containing alkaline compound are first mixed and activated to obtain an activated material; the activation temperature is 180-220°C.

[0032] In the present invention, the composition of the lithium slag is preferably based on spodumene and quartz; the lithium slag preferably includes the ...

Embodiment 1

[0060] Mix and grind 0.715g of lithium slag and 1.12g of sodium hydroxide until no obvious sodium hydroxide particles are observed, add it to a closed activation reaction vessel, activate it at 140°C for 1 hour, then let it stand and cool to room temperature to obtain the activated material.

[0061] Transfer the activated material to a crystallization reaction kettle, add 7.5 mL of distilled water, and stir evenly for 4 hours under airtight and room temperature conditions to obtain a sol, and the molar ratio of active ingredients in the obtained sol is SiO 2 :Al 2 o 3 : Na 2 O: H 2 O=5.67:1:13:300.

[0062] The sol was statically crystallized at 100°C for 6 hours, the resulting system was filtered, the obtained solid was washed with water until its pH value was 9, and then dried at 120°C for 6 hours to obtain X zeolite molecular sieve (abbreviated as A1).

[0063] The XRD pattern of A1 is as follows figure 1 As shown in curve 1, by figure 1 It can be seen that the curve...

Embodiment 2

[0067] 0.715g of lithium slag and 1.45g of sodium hydroxide were mixed and ground until no obvious sodium carbonate particles were observed, then added to a closed activation reaction vessel, activated at 180°C for 4 hours, then allowed to stand and cooled to room temperature to obtain an activated material.

[0068] The activated material was transferred to a crystallization reaction kettle, 20mL of distilled water was added, stirred evenly for 4h under airtight conditions at room temperature, and 0.38g of silica sol (SiO 2 Content 30wt%), stir evenly, obtain sol, the active ingredient molar ratio in the gained sol is SiO 2 :Al 2 o 3 : Na 2 O: H 2 O=7:1:13:800.

[0069] The sol was dynamically crystallized at 120°C for 12 hours, the resulting system was filtered, the obtained solid was washed with water until its pH value was 9, and then dried at 120°C for 6 hours to obtain X zeolite molecular sieve (abbreviated as A2).

[0070] The XRD pattern of A2 is as follows figur...

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Abstract

The invention provides an X zeolite molecular sieve and a preparation method thereof, and belongs to the technical field of molecular sieves. The preparation method of the X zeolite molecular sieve provided by the invention comprises the following steps: mixing lithium slag and a sodium-containing alkaline compound for primary mixing, and activating to obtain an activated material, wherein the activation temperature ranges from 180 DEG C to 220 DEG C; mixing the activated material with water for secondary mixing to obtain a sol; and carrying out hydrothermal crystallization on the sol to obtain the X zeolite molecular sieve. According to the method, in the process of activating lithium slag with the sodium-containing alkaline compound, high-temperature roasting treatment is not needed, activation of lithium ore can be achieved under the low-temperature condition of 180-220 DEG C, and energy consumption is remarkably reduced; moreover, the lithium slag does not need to be pretreated, aging is not needed before crystallization, and the process is simple. Moreover, the prepared X zeolite molecular sieve is high in crystallinity and static water adsorption rate, and can reach the excellent grade or above of the industrial standard.

Description

technical field [0001] The invention relates to the technical field of molecular sieves, in particular to an X zeolite molecular sieve and a preparation method thereof. Background technique [0002] Zeolite molecular sieves are microporous aluminosilicate materials with a regular and open porous structure, commonly used in gas adsorption and separation, ion exchange and catalytic processes. Among them, X-type molecular sieve can adsorb more than less than Any molecule can realize the co-adsorption of water and carbon dioxide, and the co-adsorption of water and hydrogen sulfide gas. It is mainly used in the drying of medicine, air compression system and catalyst carrier, etc., and has a wide range of applications. [0003] Lithium slag is rich in silicon and aluminum, which can be used to prepare X-type molecular sieves. For example, Hu Ting et al. (see Hu Ting et al., Synthetic NaX Molecular Sieve Structural Characterization and Adsorption Properties Research [J]. Unive...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/22B82Y40/00
CPCB82Y40/00C01B39/22C01P2002/72C01P2004/03C01P2004/41C01P2006/16
Inventor 闫文付王彬宇任立靳科研于吉红徐如人
Owner JILIN UNIV
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