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Prepn process of superfine zeolite powder

A zeolite and powder technology, applied in the fields of oil refining and petrochemical catalyst preparation, can solve the problems of restricting the development and utilization of ultrafine zeolite materials, energy consumption, low time-consuming efficiency, unfavorable large-scale production, etc. Efficient effect

Inactive Publication Date: 2003-08-20
DALIAN LIGONG QIWANGDA CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to repeated high-speed centrifugal separation and / or freeze-drying methods consume energy, time, low efficiency and require special equipment, it is not conducive to large-scale production. Therefore, the existing separation and recovery methods of ultra-fine zeolite restrict the development and utilization of ultra-fine zeolite materials

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Embodiment 1: prepare ultrafine ZSM-5 zeolite powder (comparative example) from the colloidal suspension of ultrafine ZSM-5 zeolite

[0024] Aluminum sulfate (Al 2 (SO 4 ) 3 18H 2 O), water glass (Na 2 O%wt.=8.87, SiO 2 %wt.=26.88,H 2 O%wt.=64.25), 9.8% concentrated sulfuric acid (H 2 SO 4 ), sodium chloride (NaCl), n-butylamine (n-Bu-NH 2 ) and deionized water as raw materials (all industrial products), according to the molar ratio: 1.0Al 2 o 3 : 31.2SiO2 2 : 2.0Na 2 O:833.3H 2 O: 12.2 n-Bu-NH 2 : 18.0 NaCl to prepare about 400 ml of silica-alumina gel. After 1.0 hour of strong mechanical gelling treatment (300 rpm), the gel is sealed into a 500 ml stainless steel crystallization kettle with mechanical stirring for two-stage variable temperature crystallization . Two-stage variable temperature crystallization refers to: at the beginning of crystallization, the gel is heated to 100°C at a heating rate of 1°C / min, and aged at 100°C for 24 hours. Then, the...

Embodiment 2

[0026] Example 2: Preparation of Ultrafine ZSM-5 Zeolite Powder from Colloidal Suspension of Ultrafine ZSM-5 Zeolite

[0027] Repeat Example 1, but when the colloidal suspension of the obtained ultrafine ZSM-5 zeolite is cooled to 50°C in the synthesis kettle, the synthesis kettle is opened, and the contents (about 400 milliliters) are transferred to a belt with heat preservation and mechanical Stirring plastic bucket. At a mechanical stirring speed of 100 rpm, 98% concentrated sulfuric acid was added dropwise to the suspension until the pH value detected by wide pH test paper reached about 2.0. Then according to the total liquid volume (about 400 milliliters), according to urea 8 grams per liter, the molar ratio of formaldehyde and urea is 1.2, add 3.2 grams of urea to the suspension under stirring, and then add 5.44 milliliters of 36 to the suspension after 5 minutes. % formaldehyde solution, continue to stir for 5 minutes, then stop stirring, and let stand for 2 hours afte...

Embodiment 3

[0028] Example 3: Preparation of Ultrafine ZSM-5 Zeolite Powder from Colloidal Suspension of Ultrafine ZSM-5 Zeolite

[0029] Repeat Example 2, but when 98% concentrated sulfuric acid is added dropwise to the suspension, the pH value of the suspension is successively made to reach 3.0, 4.0, and 5.0. Then the actual weight of the ultrafine ZSM-5 zeolite powder that exists in the form of agglomerates finally obtained is 42.04 grams, 41.17 grams and 38.35 grams (theoretical product weight is 42.11 grams), and the product recovery rate is successively> 99%, ≈98% and ≈91%.

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Abstract

The present invention belongs to the technology field of preparing oil refining and petrochemical catalyst and relates to the preparation process of superfine zeolite powder from the superfine zeolite particle-mother liquid colloid suspension formed through hydrothermal process. Technologically, the present invention features that the said suspension is mixed with formaldehyde and urea in certain proportion to obtain mixture solution of pH 2-5; the mixture solution is let stand at 30-80 deg.c for 0.5-24 hr before the solid matter is collected through filtering; and the solid matter is washed, dried and roasted to obtain the superfine zeolite powder. The superfine zeolite powder has regular pore canal system, is silicate (aluminosilicate) crystal containing hetero metal atoms and has primary particle size below 100 nm.

Description

technical field [0001] The invention belongs to the technical field of oil refining and petrochemical catalyst preparation, and mainly relates to a method for preparing ultrafine zeolite powder from ultrafine zeolite particles formed by hydrothermal synthesis-mother liquid colloidal suspension. Said ultra-fine zeolite is crystalline silicate with regular pore system, aluminosilicate and crystalline silicon (aluminum) salt containing metal heteroatoms other than silicon-aluminum atoms, and their primary particle size is between 500 Below nanometers, especially below 100 nanometers. Background technique [0002] Crystalline silicates, aluminosilicates, and crystalline silicon (aluminum) salts containing metal heteroatoms other than silicon-aluminum atoms are an important class of zeolite molecular sieve catalytic materials, and are widely used as catalysts or catalyst supports. According to a large number of studies in recent years, if the grain size of the above-mentioned ze...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/06C01B39/02
Inventor 郭洪臣王祥生
Owner DALIAN LIGONG QIWANGDA CHEM TECH
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