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Method for preparing 13X molecular sieve through using high-alumina fly ash, and 13X molecular sieve

A high-alumina fly ash and molecular sieve technology, applied in the field of 13X molecular sieve, can solve the problems of low overall conversion rate of zeolite, low molecular sieve purity, low yield per reactor, etc., so as to promote green production, reduce raw material costs, and improve single reactor. Yield effect

Inactive Publication Date: 2013-12-18
DATANG INT CHEM TECH RESINST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, since the crystalline quartz and mullite in the fly ash are not easy to be activated, the molecular sieves synthesized by this method have low purity; the two-step method mainly uses lye to dissolve the soluble active components in the fly ash, and then filters And adjust the silicon-aluminum ratio of the filtrate, and then obtain a high-purity molecular sieve through hydrothermal reaction, but this method only utilizes the soluble silica in the fly ash, so the overall conversion rate of fly ash to form zeolite is on the low side
[0005] The method of preparing molecular sieves from the desiliconization solution produced in the pre-desilication process in the process of extracting alumina from high-alumina fly ash is consistent with the two-step hydrothermal method. Although the synthesized molecular sieve has the advantage of high purity, due to the di The silicon oxide content generally does not exceed 85g / L, which makes the single-pot yield of molecular sieve synthesis low, resulting in high energy consumption per unit output

Method used

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  • Method for preparing 13X molecular sieve through using high-alumina fly ash, and 13X molecular sieve
  • Method for preparing 13X molecular sieve through using high-alumina fly ash, and 13X molecular sieve
  • Method for preparing 13X molecular sieve through using high-alumina fly ash, and 13X molecular sieve

Examples

Experimental program
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Effect test

Embodiment 1

[0039] This example is used to illustrate the method for preparing 13X molecular sieve and the 13X molecular sieve of the present invention.

[0040] Weigh 1kg of high-alumina fly ash (among which, Al 2 O 3 45wt%, SiO 2 accounting for 37wt%), after magnetic separation, screening and other common impurity removal steps, 2kg of 25wt% NaOH solution was added, and a pre-desilication reaction was carried out in a high pressure reactor at 120 ° C for 4h, and the material obtained after the reaction was filtered, The filter residue is washed until the pH value of the washing solution is about 8, and the filtrate and the washing solution are combined to obtain a desilication solution. The composition of the desilication liquid is shown in Table 1.

[0041] Table 1 Composition of desilication solution

[0042] component

Al 2 O 3

SiO 2

Na 2 O

CaO

Fe 2 O 3

CuO

Content (g / L)

2.04

50.4

117.2

0.015

0.0039 ...

Embodiment 2

[0049] This example is used to illustrate the method for preparing 13X molecular sieve and the 13X molecular sieve of the present invention.

[0050] Weigh 1kg of high-alumina fly ash (among which, Al 2 O 3 45wt%, SiO 2 37wt%), after magnetic separation, screening and other common impurity removal steps, 3kg of 10wt% NaOH solution was added, and pre-desilication reaction was carried out in a high pressure reactor at 100 ° C for 8h, and the material obtained after the reaction was filtered, The filter residue is washed until the pH value of the washing solution is about 8, and the filtrate and the washing solution are combined to obtain a desilication solution.

[0051] Pass CO into the desilication solution at 60°C 2 When the pH of the desilication solution reached 8.5, aeration was stopped. SiO to be generated 2 The precipitate was filtered, washed, and then dried at 100°C to obtain white powdery white carbon black. Due to SiO 2 The filtrate obtained during precipitati...

Embodiment 3

[0054] This example is used to illustrate the method for preparing 13X molecular sieve and the 13X molecular sieve of the present invention.

[0055] Weigh 1kg of high-alumina fly ash (among which, Al 2 O 3 42wt%, SiO 2 39wt%), after magnetic separation, screening and other common impurity removal steps, 2kg of 30wt% NaOH solution was added, and the pre-desilication reaction was carried out in a high pressure reactor at 150 ° C for 1 h, and the material obtained after the reaction was filtered, The filter residue is washed until the pH value of the washing solution is about 8, and the filtrate and the washing solution are combined to obtain a desilication solution.

[0056] Limestone and sodium carbonate solution are added to the filter residue (also known as desilica fume) to make raw material slurry, and the raw material slurry is roasted to obtain clinker, which is then dissolved with deionized water and filtered to obtain a filtrate. For the crude solution of sodium alu...

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PUM

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Abstract

The invention provides a method for preparing a 13X molecular sieve through using high-alumina fly ash, and the 13X molecular sieve. The preparation method comprises the following steps: mixing the high-alumina fly ash with an alkali solution for a pre-desiliconization reaction, and filtering to obtain a desiliconized solution; mixing the desiliconized solution with white carbon black to obtain a modified desiliconized solution; mixing the modified desiliconized solution with an aluminum sauce to obtain a silicon and aluminum sol; and crystallizing the silicon and aluminum sol, filtering, washing, and drying to prepare the 13X molecular sieve. The invention also provides the 13X molecular sieve prepared through the preparation method.

Description

technical field [0001] The invention relates to a method for preparing 13X molecular sieve and 13X molecular sieve, in particular to a method for preparing 13X molecular sieve by using high-alumina fly ash and 13X molecular sieve. Background technique [0002] As an industrial waste, the output of fly ash is astonishing, and the accumulated amount in China has reached billions of tons. Therefore, how to properly handle or utilize fly ash has become an urgent problem to be solved at present. In industry, industrial raw materials containing silicon and aluminum or silicate minerals are generally used as raw materials to prepare molecular sieves, and the production cost is relatively high. Fly ash contains a small amount of Fe 2 O 3 In addition to impurities such as CaO and MgO, it contains a large amount of SiO 2 and Al 2 O 3 (The content of the two can reach more than 80%). Therefore, people try to utilize fly ash as a resource according to its characteristics to prepare...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/22B09B3/00
Inventor 李春启梅长松李德炳陈元应陈爱平孙旭光刘俊峰吕燕南
Owner DATANG INT CHEM TECH RESINST
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