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Li-modified X molecular sieve and preparation method thereof

A molecular sieve and modification technology, applied in chemical instruments and methods, other chemical processes, octahedral crystalline aluminum silicate zeolite, etc., can solve problems such as excessive Na ions, existence, and uneven Li+ exchange, and reduce production costs Effect

Inactive Publication Date: 2012-06-20
于向真
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Patent CN101125664A has announced the Li of a kind of sodium type low silicon X time-consuming molecular sieve + In the exchange method, Na-X molecular sieves are first roasted, then exchanged with Li+ aqueous solution, and finally LiNa-X molecular sieves with a certain degree of exchange are mixed with solid lithium salt powder for solid-phase exchange to obtain Li-modified materials with an exchange degree of more than 96%. X molecular sieve, but this method has problems such as uneven Li+ exchange and excessive Na ions
[0006] The method announced by the patent CN101766987A is to obtain the Li-LSX molecular sieve powder with a Li exchange degree greater than 95% after the commercially available low-silicon molecular sieve powder is modified by one-cross-one-baking, two-cross-two-baking and three-cross-Li; the method requires Roasting at 400~450 for 2 times, 2~3 hours each time, there is a problem that the X molecular sieve will reduce the crystallinity of the molecular sieve due to dealumination

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Take 2Kg molecular sieve raw powder (Si / Al=1.1) for ammonium exchange, that is, add the molecular sieve raw powder to 6 liters of ammonium sulfate solution with a concentration of 8%wt, raise the temperature to 60°C, keep the temperature for 30 minutes, and then filter to obtain a filter cake ;The filter cake was replaced with the former powder of molecular sieve, and the above steps were repeated 3 times, and the obtained filter cake was dried at 200°C for 6 hours to obtain 1900gNH 4 NaX molecular sieve sample A, the measured water content is 8%wt, Na 2 The O content is 1.5%, and the calculated ammonium ion exchange degree is 95.3%.

[0027] Mix 1900g of ammonium exchange sample A with 2380ml of lithium nitrate solution with a concentration of 2.5M, heat and evaporate water under stirring until the surface of the material is dry, take it out and dry it at 250°C for 8 hours, and roast it at 600°C for 4 hours to obtain Dry the Li-modified X molecular sieve sample A1, an...

Embodiment 2

[0029] Take 2Kg molecular sieve raw powder (Si / Al=1.1) for ammonium exchange, that is, add the molecular sieve raw powder to 6 liters of ammonium chloride solution with a concentration of 8%wt, raise the temperature to 60°C, keep the temperature for 30 minutes, and then filter to obtain the filtered cake; the filter cake was replaced by the molecular sieve powder, the above steps were repeated 5 times, and the obtained filter cake was dried at 200°C for 6 hours to obtain 1800g NH 4 NaX molecular sieve sample B, the measured water content is 8%wt, Na 2 The O content is 0.21%, and the calculated ammonium ion exchange degree is 99.5%.

[0030] Divide 2320ml of lithium nitrate solution with a concentration of 2.5M into 4 parts, take one part each time and mix with 1800g of ammonium exchange sample B evenly, dry at 250°C for 4 hours to drive out the water, then add another part of lithium nitrate solution, mix, Drying Repeat the above process until the molecular sieve completely a...

Embodiment 3

[0032] After mixing 500g of sample B1 with kaolin and field green powder at a weight ratio of 1:0.10:0.05 on a dry basis, use an extruder to make strips with a diameter of about 2mm, then dry at 250°C for 4 hours, and roast at 550°C for 2 hours, to obtain LiX adsorbent B 2 , low temperature N 2 Its specific surface area is 608m2 as measured by adsorption. 2 / g, the pore volume is 0.32ml / g, the measured N 2 The gas adsorption capacity is 24.3ml / g (25°C, 1atm), and the nitrogen and oxygen separation coefficient is 8.6 (25°C, 1atm).

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Abstract

The invention relates to a Li-modified X molecular sieve and a preparation method of the Li-modified X molecular sieve. The Li-modified X molecular sieve is characterized in that the host structure of the Li-modified X molecular sieve is X molecular sieve, and the Li-modified X molecular sieve consists of Li2O, Na2O, SiO2 and Al2O3 with the molar ratio of (0.9 to 1.0):(0 to 0.1):(2.0 to 3.0):1, wherein the exchange degree of Li<+> reaches up to 99% or higher. The preparation method of the Li-modified X molecular sieve comprises the following steps: exchanging X molecular sieve powder with ammonium salt; soaking the molecular sieve in a lithium salt solution; drying; and calcining to obtain the Li-modified X molecular sieve. The Li-modified X molecular sieve has the advantages that Li-modified X molecular sieve with high Li<+> exchange degree can be easily prepared by exchanging NH4<+> with Na<+>; and the lithium salt solution can be fully adsorbed by the molecular sieve by soaking, and the theoretical utilization rate can reach up to 100%, thereby lowering production cost of Li-modified X molecular sieve.

Description

technical field [0001] The invention relates to an X molecular sieve for air nitrogen and oxygen separation and a preparation method thereof, in particular to a lithium-containing modified X-type molecular sieve and a preparation method thereof, belonging to the field of nitrogen and oxygen separation adsorbents. Background technique [0002] Molecular sieves have pores of uniform size, which can adsorb material molecules of the same size as their pores. X molecular sieves, especially X molecular sieves that have been deeply exchanged by Li, have very good adsorption characteristics for nitrogen. Therefore, Li-modified X molecular sieves are used in industry to adsorb and separate nitrogen. Oxygen technology is widely used. [0003] Usually, the method for obtaining Li-modified X molecular sieves is to exchange synthetic or commercially available KNa-X molecular sieves with high-concentration soluble Li salt solutions several times, such as U.S. Patent Nos. 5,464,467, 5,932,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/22B01J20/18B01J20/30
Inventor 于向真
Owner 于向真
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