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Method for synthesizing high-crystallinity ZSM-35 molecular sieve without amine and ZSM-35 molecular sieve

A ZSM-35, high crystallinity technology, applied in molecular sieve catalysts, chemical instruments and methods, crystalline aluminosilicate zeolites, etc., can solve the problems of large ferrierite crystal grains, etc., and achieve environmental protection and molecular sieve production. Effect

Active Publication Date: 2022-02-01
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Ferrierite obtained by conventional methods tends to have relatively large grains [SzostaK R.Hand book of Molecular Sieves; Van NostrandReinhold: New York, 1992]

Method used

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  • Method for synthesizing high-crystallinity ZSM-35 molecular sieve without amine and ZSM-35 molecular sieve
  • Method for synthesizing high-crystallinity ZSM-35 molecular sieve without amine and ZSM-35 molecular sieve

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Embodiment approach

[0049] According to a preferred embodiment of the present invention, preferably H 2 O / SiO 2 25-28.

[0050] According to a preferred embodiment of the present invention, preferably SiO 2 / Al 2 o 3 15-300.

[0051] In the present invention, there is no special requirement on how to control the pH value of the mixture C, and common methods for adjusting the pH value can be used in the present invention, for example, an alkaline solution can be used to adjust the pH value of the mixture A and / or the mixture B above 9 To control the pH value of the mixture C above 9, according to a preferred embodiment of the present invention, it is preferred to use an alkaline solution to simultaneously adjust the pH values ​​of the mixture A and the mixture B to be above 11 respectively to control the pH value of the mixture C above 11 , more preferably the pH of the mixture C is 11-13.5. Thus, the crystallinity of the molecular sieve synthesized by the present invention can be improved. ...

Embodiment 1

[0097] (1) Dissolve 1.233 g of sodium aluminate in 25 g of deionized water to obtain a clear solution, add 1.04 g of ZSM-35 molecular sieve seed crystals, and age at 60° C. for 4 hours to obtain mixture A;

[0098] (2) Add 13.9 g of silica sol to 5 g of deionized water under stirring, then add 4.23 g of sodium fluoride, and continue stirring for 1 hour to obtain mixture B;

[0099] (3) Dissolve 0.08 gram of sodium hydroxide and 0.8 gram of potassium hydroxide in 9 gram of deionized water, after obtaining the clear solution, divide it into two parts, add in the above-mentioned mixture A and mixture B respectively;

[0100] (4) Add mixture B to mixture A under stirring to obtain mixture C, and the pH value of mixture C is measured to be 12;

[0101] (5) The obtained mixture C was put into a stainless steel reaction kettle lined with polytetrafluoroethylene, and crystallized at 175° C. for 40 hours. Filter, wash, dry after crystallization is finished, obtain solid product 7.2 gr...

Embodiment 2

[0105] (1) Dissolve 0.12 g of sodium aluminate in 10 g of deionized water to obtain a clear solution, add 1.04 g of ZSM-35 molecular sieve seed crystals, and age at 60° C. for 4 hours to obtain mixture A;

[0106] (2) Add 0.4 g of sodium fluoride to 13.9 g of silica sol under stirring, and continue stirring for 1 hour to obtain mixture B;

[0107] (3) 0.08 gram of sodium hydroxide and 0.18 gram of potassium hydroxide were dissolved in 9 grams of deionized water, and after obtaining a clear solution, they were equally divided into two parts and added to the above-mentioned mixture A and mixture B respectively;

[0108] (4) Add mixture B to mixture A under stirring to obtain mixture C, and the pH value of mixture C is measured to be 11;

[0109] (5) The obtained mixture C was put into a stainless steel reaction kettle lined with polytetrafluoroethylene, and crystallized at 140° C. for 7 days. After the crystallization was completed, it was filtered, washed, and dried to obtain ...

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Abstract

The invention relates to the field of molecular sieve synthesis, and particularly provides an amine-free method for synthesizing a high-crystallinity ZSM-35 molecular sieve, which comprises the following steps: (1) aging a solution containing an aluminum source and a seed crystal at 40-99 DEG C to obtain a mixture A; (2) in the presence of a water-containing solvent, mixing a silicon source with fluoride to obtain a mixture B; (3) mixing the mixture B with the mixture A to obtain a mixture C; (4) crystallizing the obtained mixture C, then carrying out solid-liquid separation and heat treatment, and controlling the pH value of the mixture C to be 9 or above. The invention provides the ZSM-35 molecular sieve synthesized by the method disclosed by the invention, wherein no organic template agent is used, so that environmental protection and molecular sieve production are facilitated; and the crystallinity of the obtained ZSM-35 molecular sieve is obviously higher than that of a product obtained by a general amine-free method.

Description

technical field [0001] The invention relates to a method for synthesizing ZSM-35 molecular sieve with high crystallinity without amine, and the ZSM-35 molecular sieve obtained by the method. Background technique [0002] Molecular sieves with FER structure are a class of molecular sieves defined by the International Molecular Sieve Association. Representative of this class of molecular sieves. [0003] Ferrierite is a natural mineral, and ZSM-35 molecular sieve was artificially synthesized for the first time by hydrothermal method in 1977 by Plank et al. K. Crystalline zeolite and method of preparing same, US 4016245.1977]. The pore structure of ZSM-35 molecular sieve is a two-dimensional intersecting channel system composed of five-membered rings, eight-membered rings and ten-membered rings. The diameter of the ten-membered ring parallel to the [001] direction is 0.42nm×0.54nm, which is the same as [010] ] The diameter of the eight-membered ring channel parallel to the d...

Claims

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Application Information

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IPC IPC(8): C01B39/44B01J29/65
CPCC01B39/44B01J29/65Y02P20/52
Inventor 祁晓岚王煜石张平
Owner CHINA PETROLEUM & CHEM CORP
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