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Preparation method of nano-scale mcm-49 molecular sieve

A technology of MCM-49 and molecular sieve, which is applied in the direction of crystalline aluminosilicate zeolite, can solve the problems of long crystallization time and narrow range of silicon-aluminum ratio, and achieve short crystallization time, wide range, and reduced crystallization cycle Effect

Active Publication Date: 2017-08-25
SHANGHAI HUAYI GRP CO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved by the present invention is the problem of long crystallization time and narrow range of silicon-aluminum ratio in the prior art, and a new preparation method of nano-scale MCM-49 molecular sieve is provided

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] According to the material ratio of reactants (molar ratio): SiO 2 / Al 2 o 3 =29,Na 2 O / SiO 2 =0.03, PI / SiO 2 =0.26,H 2 O / SiO 2 =18.3, where piperidine is denoted as PI, the same below, prepare a reaction mixture, and then add 0.2% MCM-49 molecular sieve active seed crystals of the dry weight of the mixture to the reaction mixture. The silicon source in the raw material is silica sol; the aluminum source is sodium aluminate; the purity of the template used is greater than 98% of industrial grade piperidine; after the materials are vigorously stirred for 2 hours, the reaction mixture is crystallized at 157°C for 72 hours. The crystallized material was separated from solid and liquid, washed, and dried at 140° C. for 18 hours to obtain MCM-49 molecular sieve; the obtained crystal was MCM-49 molecular sieve as measured by X-ray diffractometer. SiO was obtained by chemical analysis 2 / Al 2 o 3 The molar ratio was 29.8. The crystal is characterized by a scanning el...

Embodiment 2

[0014] According to the material ratio of reactants (molar ratio): SiO 2 / Al 2 o 3 =25,Na 2 O / SiO 2 =0.05, PI / SiO 2 =0.36,H 2 O / SiO 2 =20.4, prepare a reaction mixture, and then add 0.3% MCM-49 molecular sieve active seed crystals to the reaction mixture based on the dry weight of the mixture. The silicon source in the raw material is silica sol; the aluminum source is sodium aluminate; the purity of the template used is greater than 98% of industrial grade piperidine; after the materials are vigorously stirred for 2 hours, the reaction mixture is crystallized at 163° C. for 66 hours. The crystallized material was subjected to solid-liquid separation, washed, and dried at 150° C. for 10 hours to obtain MCM-49 molecular sieve; the obtained crystal was MCM-49 molecular sieve as measured by X-ray diffractometer. SiO was obtained by chemical analysis 2 / Al 2 o 3 The molar ratio was 24.4. The crystal is characterized by a scanning electron microscope as a flaky crystal w...

Embodiment 3

[0016] According to the material ratio of reactants (molar ratio): SiO 2 / Al 2 o 3 =25,Na 2 O / SiO 2 =0.02, PI / SiO 2 =0.45,H 2 O / SiO 2 =25.0, prepare a reaction mixture, and then add 0.4% MCM-49 molecular sieve active seed crystals to the reaction mixture based on the dry weight of the mixture. The silicon source in the raw material is silica sol; the aluminum source is sodium aluminate; the purity of the template used is greater than 98% of industrial grade piperidine; after the materials are vigorously stirred for 2 hours, the reaction mixture is crystallized at 168° C. for 60 hours. The crystallized material was subjected to solid-liquid separation, washed, and dried at 155° C. for 9 hours to obtain MCM-49 molecular sieve; the obtained crystal was determined to be MCM-49 molecular sieve by X-ray diffractometer. SiO was obtained by chemical analysis 2 / Al 2 o 3 The molar ratio was 24.2. The crystal is characterized by a scanning electron microscope as a flaky cryst...

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Abstract

The invention relates to a preparation method of a nanoscale MCM-49 molecular sieve, and aims at solving the problems of relatively long crystallizing time and relatively narrow silica-alumina ratio range in the prior art. The preparation method of the nanoscale MCM-49 molecular sieve comprises the steps of mixing a silicon source, an aluminum source, a template agent and water in ratio; adding MCM-49 molecular sieve active crystal seed which is 0.01 to 1% of the weight of a dry mixture basis to the mixture; crystallizing for 0.1 to 100h at the temperature of 156 to 185 DEG C; performing solid-liquid separating and washing for the crystallizing materials; drying for 1 to 72 hours at the temperature of 140 to 200 DEG C to obtain the nanoscale MCM-49 molecular sieve; in light of the morphology, the nanoscale MCM-49 molecular sieve is in form of a tabular crystal being 50 to 900nm in diameter and 10 to 100nm in thickness. According to the technical scheme, the preparation method of the nanoscale MCM-49 molecular sieve has the advantages that the problems above are solved, and the method can be applied to the preparation of the nanoscale MCM-49 molecular sieve.

Description

technical field [0001] The invention relates to a preparation method of nanometer MCM-49 molecular sieve. Background technique [0002] MCM-49 molecular sieve is a layered molecular sieve with MWW topology, which was first synthesized by Mobil in 1993 under the hexamethyleneimine template system. It has two independent pore systems: interlayer ten-membered ring (0.40 ×0.59nm) connected channel system, ten-membered ring two-dimensional sinusoidal channel system in the layer and twelve-membered ring holes (0.71×0.71×1.82nm) on the outer surface of the crystal. MCM-49 molecular sieves have broad application prospects in reactions such as alkylation, aromatization, catalytic cracking and isomerization due to their unique pore structure. [0003] At present, the synthesis of MCM-49 molecular sieves is mainly a hydrothermal synthesis method, and patents US5236575, US5362697, US5557024, US5827491, CN1397494, and CN103848433 all involve the synthesis methods of MCM-49 molecular sie...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/04
CPCC01B39/04C01P2004/24
Inventor 邢海军尚勤杰李永刚宁春利张春雷
Owner SHANGHAI HUAYI GRP CO