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Method for preparing silver-loaded hydrogen sulfide poisoning-resistant 4A molecular sieve from attapulgite serving as raw material

A technology resistant to hydrogen sulfide and attapulgite, applied in separation methods, chemical instruments and methods, molecular sieves and alkali exchange compounds, etc., can solve the problems of reduced catalytic activity, easy poisoning and deactivation, and adsorbent poisoning, and achieves no secondary Secondary pollution, low equipment requirements, strong dispersion effect

Active Publication Date: 2018-08-28
SHANDONG UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] First, the average H in natural gas in my country 2 S content exceeds 1%, while H 2 S is a compound that can easily poison the adsorbent, reducing its catalytic activity;
[0008] Second, the mercury removal catalysts in the above-mentioned prior art are very sensitive to sulfides and are easily poisoned and deactivated

Method used

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  • Method for preparing silver-loaded hydrogen sulfide poisoning-resistant 4A molecular sieve from attapulgite serving as raw material
  • Method for preparing silver-loaded hydrogen sulfide poisoning-resistant 4A molecular sieve from attapulgite serving as raw material
  • Method for preparing silver-loaded hydrogen sulfide poisoning-resistant 4A molecular sieve from attapulgite serving as raw material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] The first step is to grind the attapulgite, wash it with distilled water, filter it, put it into a muffle furnace for calcination at 300°C for 3 hours, then carry out acidification treatment, add 8% sulfuric acid and heat it to boiling for 1 hour, wash it with distilled water until it is neutral, and dry it Finally, grind through a 100-mesh sieve. Attapulgite SiO 2 The content is 57.2%, and the total content of Mg, Al, Fe is 24.1%.

[0052] Step 2: Mix the sieved attapulgite with 30% sodium hydroxide solution, put it into a round-bottomed flask, place it in a microwave oven with a reflux device, and heat it to 80°C for reflux for 4 hours;

[0053] The third step, preparation of sodium aluminate solution: put a certain amount of sodium aluminate in a beaker, add a small amount of water, and stir at 40°C for 2 hours to obtain a certain concentration of sodium aluminate solution;

[0054] The fourth step, crystallization, sodium aluminate solution is added to the attapul...

Embodiment 2

[0058] The difference from Example 1 is that

[0059] In the fifth step, the 4A molecular sieve with a silver loading of 1.5% is controlled.

[0060] Choose simulated natural gas H 2 The S content is 1.2%, and the methane content is 85%. The rest is N 2 Conduct mercury removal experiments. During the experiment CH 4 The flow rate is 600ml / min, and H 2 S control content is about 1.2%, carrier gas N 2 The flow rate was 100ml / min for the mercury removal experiment. The experimental results show that the mercury removal efficiency is 96%.

Embodiment 3

[0062] The difference from Example 1 is:

[0063] In the fifth step, the 4A molecular sieve with a silver load of 2% is controlled.

[0064] Choose simulated natural gas H 2 The S content is 1.2%, and the methane content is 85%. The rest is N 2 Carry out the mercury removal experiment, CH 4 The flow rate is 600ml / min, and H 2 S control content is about 1.2%, carrier gas N 2 The flow rate was 100ml / min for the mercury removal experiment. The experimental results show that the mercury removal efficiency is 96%.

[0065] It can be seen from the above-mentioned Examples 1-3 that the amount of silver loaded in the present invention should be controlled at 1.0%-2.0%.

[0066] The concentration of hydrogen sulfide also affects the mercury removal efficiency.

[0067] The present invention studies the preparation of silver-loaded 4A molecular sieves in different H 2 The effect of mercury removal performance on the resistance to hydrogen sulfide poisoning under the atmosphere ...

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Abstract

The invention discloses a method for preparing a silver-loaded hydrogen sulfide poisoning-resistant 4A molecular sieve from attapulgite serving as a raw material, and belongs to the technical field ofpreparation of a molecular sieve. The method comprises the following steps: firstly, pretreating the attapulgite; mixing the pretreated attapulgite and an alkali liquid and performing microwave heating; preparing a sodium aluminate solution, performing crystallization, and performing silver loading on the 4A molecular sieve obtained through crystallization through supercritical carbon dioxide; and finally obtaining the silver-loaded 4A molecular sieve. The silver-loaded 4A molecular sieve prepared by the method is applied to mercury removing experiment under the simulated natural gas atmosphere, and the 4A molecular sieve with the silver loaded quantity of 1.5 percent is selected. The silver is loaded by other loading methods, the mercury removing efficiency experiment is conducted underthe atmosphere of different H2S concentration through comparison, and the experiment proves that the silver-loaded 4A molecular sieve has high mercury removing efficiency and has H2S poisoning resistance. The silver-loaded molecular sieve can maintain high mercury removing efficiency under the atmosphere containing H2S.

Description

technical field [0001] The invention relates to the technical field of molecular sieve preparation, in particular to a method for preparing a silver-loaded 4A molecular sieve resistant to hydrogen sulfide poisoning by using attapulgite as a raw material. Background technique [0002] 4A molecular sieve is an alkali metal aluminosilicate, which can absorb water, NH 3 、H 2 S, sulfur dioxide, carbon dioxide, C 2 h 5 OH, C 2 h 6 、C 2 h 4 Molecules with a critical diameter not greater than 4A. It has the advantages of large surface area, regular pore structure and flexible modification. The molecular formula of 4A molecular sieve is Na 2 O·Al 2 o 3 2SiO2 2 9 / 2H 2 O, silicon aluminum than SiO 2 / Al 2 o 3 ≈2, the pore size is 4 nm, and its spatial network structure is composed of silicon-oxygen tetrahedral units [SiO 4 ] and alumina tetrahedron [AlO 4 ] Units are arranged in a staggered manner. It is widely used in the field of gas adsorption. [0003] Mercury i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/18C01B39/02C01B33/40B01J20/18B01J20/32B01D53/02
CPCB01D53/02B01D2257/602B01J20/186B01J20/3234C01B33/40C01B39/026C01B39/18C01P2002/72Y02P20/54
Inventor 张华伟张鼎元孙华敏武加峰梁鹏
Owner SHANDONG UNIV OF SCI & TECH
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