Preparation method of binderless ZSM-5 molecular sieve

A ZSM-5, binder-free technology, applied in the direction of crystalline aluminosilicate zeolite, borane silicone crystalline aluminosilicate zeolite, etc., can solve the problem of pollution environment, no binder ZSM-5 molecular sieve preparation The process is complicated and other problems, so as to achieve the effect of reducing production cost, simple and environmentally friendly preparation process, and good technical effect.

Active Publication Date: 2013-04-10
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The technical problem to be solved by the present invention is that the preparation process of binder-free ZSM-5 molecular sieve is complex and pollutes the environment

Method used

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  • Preparation method of binderless ZSM-5 molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1～5

[0020] Add 30 milliliters of deionized water to the reaction kettle in advance, place 10 grams of sample A in Comparative Example 1 above the porous stainless steel mesh in the reaction kettle and seal it, and then treat it at 180°C for 24 hours, 48 ​​hours, 72 hours, and 96 hours , 120 hours. The sample numbers are respectively marked as A-24-water, A-48-water, A-72-water, A-96-water, A-120-water.

[0021] The product was first dried at 110°C, and then calcined in a muffle furnace at 550°C for more than 4 hours. The calcined product was characterized by X-ray powder diffraction (XRD) and nitrogen adsorption. The results are shown in Table 1 and Table 2. The XRD pattern of the product treated for 24 hours shows that the relative crystallinity and specific surface area of ​​the sample have increased, indicating that part of the amorphous silica binder has been transformed into a ZSM-5 molecular sieve. After 72 hours of treatment, the relative crystallinity of the product is al...

Embodiment 6～9

[0023] Take by weighing 40 grams of ZSM-5 molecular sieves (silicon-aluminum ratio 600, template agent tetrapropyl ammonium bromide content 11.5% in the channel), add 31 grams of 40% (weight) silica sol and mix evenly, extrude into strips, Dry at 110°C to obtain sample B.

[0024] 30 milliliters of ammonia water was added to the reaction kettle in advance, and 10 grams of sample B was placed in the reaction kettle above the porous stainless steel mesh and sealed, and then treated at 180°C for 48 hours, 72 hours, 96 hours, and 120 hours. The sample numbers are marked as B-48-Ammonia, B-72-Ammonia, B-96-Ammonia, B-120-Ammonia.

[0025] The product was first dried at 110°C, and then calcined in a muffle furnace at 550°C for 4 hours. The calcined product was characterized by X-ray powder diffraction (XRD) and nitrogen adsorption, and the results are shown in Table 1 and Table 2. The XRD pattern of the product treated for 24 hours shows that the relative crystallinity and specifi...

Embodiment 10～11

[0029] Take by weighing 20 grams of ZSM-5 molecular sieves (silicon-aluminum ratio 300, template agent tetrapropylammonium bromide content 11% in the channel), add 15 grams of 40% (weight) silica sol and mix evenly, extrude into strips, Dry at 110°C to obtain sample C.

[0030] Add 30 ml of ammonia water to the reaction kettle in advance, place 10 grams of sample B in the reaction kettle above the porous stainless steel mesh and seal it, and then treat it at 170 and 190°C for 72 hours, and the sample numbers are marked as C-1 and C-2 .

[0031] The product was first dried at 110°C, and then calcined in a muffle furnace at 550°C for 4 hours. The calcined products were characterized by X-ray powder diffraction (XRD) and nitrogen gas adsorption. The results are shown in Table 1 and Table 2. The samples treated at 170°C and 190°C all have higher relative crystallinity and specific surface area.

[0032] Table 1

[0033]

[0034] Table 2

[0035] Example

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Abstract

The invention relates to a preparation method of a binderless ZSM-5 molecular sieve, and is mainly to solve the problem that the employment of organic amine in the production process of binderless molecular sieve leads to contaminations easily in the prior art. The preparation method of the binderless ZSM-5 molecular sieve of present invention comprises the following steps: firstly, mixing and molding the ZSM-5 molecular sieve powder and an amorphous silica binder, drying, processing by water vapor or inorganic ammonia-containing vapor to convert into the binderless ZSM-5 molecular sieve to get the binderless ZSM-5 molecular sieve, wherein the binder content is from 0 to 10%, the specific surface area of BET is from 330 to 380 m<2>/g, Langmuir specific surface area is from 440 to 500 m<2>/g, and the relative crystallinity is from 87 to 100%. The technical solution solves the problem well, and can be used for the industrial production of ZSM-5 molecular sieve catalyst.

Description

technical field [0001] The invention relates to a method for preparing a binder-free ZSM-5 molecular sieve. Background technique [0002] ZSM-5 zeolite is a kind of high silica zeolite that has been widely studied. It was first synthesized by Argauer et al. of Mobil Company in 1972. ZSM-5 has a two-dimensional ten-membered ring channel, the space group is Pmna, and the orthorhombic crystal system. Cell parameters: alpha=90.000°, beta=90.000°, gamma=90.000°, the skeleton density (FDSi) is The ideal unit cell composition of ZSM-5 molecular sieve can be expressed as Na n (H 2 O) 16 Al n Si 96-n o 192 , where the number of Al atoms varies from 0 to 27. ZSM-5 has two intersecting pore systems. The ten-membered ring channel parallel to the a-axis direction is Z-shaped, and the pore diameter is linear. The ten-membered ring channel parallel to the b-axis direction is linear, and the pore diameter is ZSM-5 is a high-silicon molecular sieve rich in five-membered ...

Claims

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Application Information

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IPC IPC(8): C01B39/38
Inventor 赵国良滕加伟徐建军杨为民
Owner CHINA PETROLEUM & CHEM CORP
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