Modification treatment method of Y-type zeolite

A treatment method and zeolite technology, applied in the direction of crystalline aluminosilicate zeolite, octahedral crystalline aluminosilicate zeolite, etc., can solve the problems of reducing the sodium content of zeolite, and the silicon-aluminum ratio does not increase too much, so as to reduce the sodium content, Improved stability and high specific surface area

Active Publication Date: 2015-05-20
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] CN1284402A discloses a Y-type zeolite with a secondary pore structure and a preparation method thereof. After impregnating the Y-type zeolite and a silicon-containing solution, drying, and then treating with water vapor, the Y-type zeolite with high hydrothermal stability is obtained, but the silicon-alumina not much better than
[0010] The above modification methods are only for the investigation of the special properties of the treated samples, such as the preparation of zeolite containing secondary mesoporous or increasing the silicon-aluminum ratio to increase the stability of zeolite or reduce the sodium content of zeolite, etc.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] (1) Ammonium exchange for NaY zeolite

[0019] The NaY zeolite (sodium content Na 2 O%: 12.8%; silicon aluminum ratio SiO 2 / Al 2 o 3 : 5.4; specific surface area: 721m 2 g -1 ) 10g with 500ml of NH 4 NO 3 (1M) The solution was exchanged at 80°C for 5 hours, then the filtered and washed zeolite sample was placed in a muffle furnace, and roasted at 400°C for 5h; the above process was repeated 3 times, and the silicon-aluminum ratio of the obtained HY zeolite was 7.2 , the specific surface area is 661m 2 g -1 , sodium content (Na 2 O) is 1.8%.

[0020] (2) High temperature steam treatment

[0021] Put 6g of roasted and exchanged HY zeolite on a quartz boat, put it into a tube furnace and raise the temperature to 550°C, then pass in water vapor to maintain a certain flow rate (30-40ml / min), and treat for 5 hours to obtain high-temperature steam-treated Y-type zeolite.

[0022] (3) Citric acid solution treatment

[0023] Weigh 5g of Y-type zeolite treated with...

Embodiment 2

[0025] (1) Ammonium exchange for NaY zeolite

[0026] With 10g NaY zeolite (sodium content NaO%: 12.8%; silicon aluminum than SiO 2 / Al 2 o 3 : 5.4; specific surface area: 721m 2 g -1 ) with 500ml of NH 4 NO 3 (1.5M) solution was exchanged at 80°C for 5 hours, then filtered and washed, and the obtained zeolite sample was placed in a muffle furnace and roasted at 400°C for 5 hours; after repeating the above process 3 times, the silica of the obtained HY zeolite The aluminum ratio is 7.5 and the specific surface area is 652m 2 g -1 , sodium content (Na 2 O) is 0.9%.

[0027] (2) High temperature steam treatment

[0028] Put 6g of roasted and exchanged HY zeolite in a quartz boat, put it in a tube furnace and raise the temperature to 600°C, then pass in water vapor to maintain a certain flow rate of 30-40ml / min, and treat for 5 hours to obtain a Y-type treated with high-temperature water vapor Zeolite.

[0029] (3) Citric acid solution treatment

[0030] Weigh 5g of ...

Embodiment 3

[0032] (1) Ammonium exchange for NaY zeolite

[0033] With 10g NaY zeolite (sodium content Na O%: 12.8%; Si-aluminum ratio SiO 2 / Al 2 o 3 :5.4; specific surface area: 721m 2 g -1 ) with 500ml of NH 4 NO 3 (1.0M) solution was exchanged at 100°C for 5 hours, then filtered and washed, and the obtained zeolite sample was placed in a muffle furnace and roasted at 400°C for 5 hours. The above process was repeated three times, and the obtained HY zeolite silicon The aluminum ratio is 7.3 and the specific surface area is 648m 2 g -1 , sodium content (Na 2 O) is 1.5%.

[0034] (2) High temperature steam treatment

[0035] Put 6g of roasted and exchanged HY zeolite in a quartz boat, then put it in a tube furnace and raise the temperature to 500°C, feed water vapor to maintain a certain flow rate of 40-50ml / min, and treat for 5 hours to obtain a Y-type treated with high-temperature steam Zeolite.

[0036] (3) Citric acid solution treatment

[0037] Weigh 5g of the Y-type ze...

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Abstract

The invention relates to a modification treatment method of a Y-type zeolite. The method comprises the following steps: carrying out ammonium exchange and direct burning on industrially-produced common NaY zeolite, repeating the ammonium exchange and direct burning for at least three times, then subjecting the NaY zeolite to a water steam treatment at a high temperature, and finally processing the NaY zeolite by a critic acid solution. The silicon/aluminum ratio of processed Y-type zeolite is in a range of 9 to 11, and the specific surface area of the processed Y-type zeolite is in a range of 550 to 650 m2/g. Furthermore, the zeolite stability is improved, the sodium content is decreased, at the same time the amorphous aluminum out of the skeleton is removed, secondary mesopores (3-20 nm) are generated in the Y-type zeolite, strong acid centers are generated at the meantime, no environmental pollutant is generated during the treatment process, the efficiency is high, the modification treatment method is environment-friendly, the whole process is carried out on the basis of conventional modification treatments, and the provided method is suitable for massive preparation of Y-type zeolite with a high silicon/aluminum ratio through modification on NaY zeolite.

Description

technical field [0001] The invention relates to a modification treatment method of zeolite molecular sieve material, in particular to the modification treatment of industrially produced conventional NaY type zeolite. Background technique [0002] Because of its unique pore structure, Y-type zeolite is widely used in the fields of adsorption, separation, and catalysis, especially in petrochemical industry, and is the main active component of fluid catalytic cracking (FCC) catalysts. The silicon-aluminum ratio of the Y-type zeolite unit cell framework directly affects the hydrothermal stability and acidity of the zeolite molecular sieve. However, with the heavy and inferior quality of petroleum, conventional zeolites can no longer meet the harsh reaction-regeneration conditions of catalytic cracking; increase the silicon-aluminum ratio of the Y-type zeolite framework, reasonably reduce the acid center density, and increase the relative strength of the acid center , and increa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/24
Inventor 李海岩秦丽红袁忠勇刘优林李敏吕倩王亮王燕谢彬于春梅孙发民张全国席忠亮刘丽军高善彬董春明杨晓东谢方明夏恩东马宝利
Owner PETROCHINA CO LTD
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