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13X-type molecular sieve and preparation method thereof

A technology of molecular sieve and gel, which is applied in the chemical industry, can solve the problems of not finding a way to use it, and achieve the effect of reducing synthesis cost and environmental pollution

Inactive Publication Date: 2010-06-16
DATANG INT CHEM TECH RESINST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the process of extracting alumina from fly ash, a large amount of desiliconization liquid is produced by the fly ash through the pre-desilication process, and the main component is sodium silicate. This by-product has not found a suitable way of utilization.

Method used

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  • 13X-type molecular sieve and preparation method thereof
  • 13X-type molecular sieve and preparation method thereof
  • 13X-type molecular sieve and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0060] High alumina fly ash (with Al 2 o 3 In terms of weight percentage, the aluminum content is 50%) finely ground to 500 mesh, weighed 20 grams, put it into a high-pressure reactor with stirring, and added 40 grams of 25% ash / alkali mass ratio of 1:0.5 NaOH solution (calculated as NaOH, mass concentration), heat desiliconization at 130°C for 2 hours, after the reaction time is up, take out the mixed material and filter, wash the filter cake until the pH of the lotion is 9, and the lotion is the result of the first filtration. In the filtrate, the filtrate is desiliconized liquid.

Embodiment 2

[0062] Get the desiliconization solution of A batch (desiliconization solution A) and carry out inductively coupled plasma (ICP) emission spectrum analysis, its composition is as shown in Table 1, by molar ratio, Na in the desiliconization solution 2 O / SiO 2 = 1.3, SiO 2 / Al 2 o 3 =756.5,H 2 O / Na 2 O=60. Take 100mL of the desiliconization solution and put it into a polytetrafluoroethylene beaker, and place it in a constant temperature water bath at 40°C. Then add 4.9 g of AlCl to the Teflon beaker 3 , the molar composition of the resulting mixture is: 5Na 2 O:Al 2 o 3 : 4SiO 2 : 300H 2 O, the mixture was stirred for 3 hours to form a gel, and the stirring was stopped. Transfer the gel to a closed crystallization tank and age at 70°C for 5 hours, then raise the temperature to 90°C for 5 hours to crystallize, after cooling, filter the product, wash with water until the pH is 10, and dry the filter cake at 90°C to obtain product. XRF and XRD tests show that SiO 2 / ...

Embodiment 3

[0066] Take 100 mL of the desiliconization solution A in Example 2, put it into a polytetrafluoroethylene beaker, and place it in a constant temperature water bath at 30°C. Then add 3.8 grams of NaAlO to the tetrafluoroethylene beaker 2 , the resulting mixture has a molar composition of 4.9Na 2 O:Al 2 o 3 : 3.2SiO2 2 : 247H 2 O, the mixture was stirred for 3 hours to form a gel, and the stirring was stopped. Transfer the gel to a closed crystallization tank and age at 60°C for 6 hours, then raise the temperature to 80°C for 5 hours to crystallize, after cooling, filter the product, wash with water until the pH is 10, and dry the filter cake at 100°C to obtain product. XRF and XRD tests show that SiO 2 / Al 2 o 3 The molar ratio is 2.8, and its crystal phase structure is X-type molecular sieve, and SEM shows that its crystal grain is about 1 micron ( image 3 Shown), the relative crystallinity is 142%.

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Abstract

The invention provides a method for preparing a 13X-type molecular sieve. The method is characterized by desilicating high-aluminum fly ash to obtain a desilicated liquid as a silicon source and an aluminum source to prepare the 13X-type molecular sieve. The invention further provides the 13X-type molecular sieve prepared by the method of the invention. By adopting the synthesis method of the 13X-type molecular sieve provided in the invention, not only the synthesis cost is reduced, but also the fly ash, in particular the fly ash with high aluminum content, is more effectively used for extracting the desilicated liquid and sodium aluminate crude liquid, wherein the desilicated liquid is generated in the desilication process of alumina.

Description

technical field [0001] The invention relates to a 13X type molecular sieve and a preparation method of the molecular sieve, belonging to the technical field of chemical industry. Background technique [0002] NaX molecular sieves are generally called 13X molecular sieves, with a pore size of Can absorb less than any molecule. 13X type molecular sieve has higher water and CO 2 Co-adsorption characteristics, water and H 2 S co-adsorption, commonly used in air drying in air separation units, as well as drying and desulfurization of natural gas, liquefied petroleum gas, liquid hydrocarbons, etc., hollow glass desiccant, non-food desiccant, etc. In addition, 13X molecular sieves are widely used as adsorbents in PSA oxygen production, CO 2 separation and purification etc. The general method for synthesizing 13X molecular sieves is to mix commercial silicon sources (such as silicon dioxide, sodium silicate, etc.), aluminum sources (such as sodium aluminate, aluminum sulfate...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/02B01J20/18
Inventor 李春启陈爱平梅长松李德炳忻仕河
Owner DATANG INT CHEM TECH RESINST
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