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Fractional crystallization synthesis method for high-content skeleton iron ZSM-35 molecular sieve

A ZSM-35, chemical synthesis technology, applied in the direction of iron conglomerate crystalline aluminosilicate zeolite, crystalline aluminosilicate zeolite, etc., can solve the problems of complex synthesis method, low crystallinity, long crystallization time, etc. , to achieve the effect of simplifying the operating conditions, simplifying the synthesis process, and reducing the difficulty of production

Inactive Publication Date: 2013-01-02
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The synthesis methods are relatively complicated, such as crystallization under dynamic conditions, adjustment of the initial gel pH value, and longer crystallization time, etc.
The synthesized product also has some defects, such as the introduction of iron atoms is not high, there are inactive extra-framework iron species, and the crystallinity is not high.

Method used

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  • Fractional crystallization synthesis method for high-content skeleton iron ZSM-35 molecular sieve
  • Fractional crystallization synthesis method for high-content skeleton iron ZSM-35 molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] The first stage (I): Add 0.52ml of 1M NaOH solution and 0.44ml of 1M KOH solution to 2.02g of silica sol, add 5.50g of water after dissolving the silica sol by increasing heat; dissolve 0.08g of sodium aluminate in 5.00g of water, Add 0.51ml 1M NaOH solution and 0.43ml 1M KOH solution dropwise; slowly add sodium aluminate solution dropwise into the silicon source solution under stirring conditions to obtain a white colloid, then add 0.63ml FeCl 3 The solution was added to the white colloid, stirred for 2 hours, and finally 0.55ml of cyclohexylamine was added to obtain the initial gel. The material was placed in a stainless steel reactor lined with polytetrafluoroethylene, and crystallized at 220°C for 5 hours.

[0044] The first stage (II): In addition to adding FeCl 3 Solution, the remaining steps are the same as the first stage (I), and finally the material is placed in a stainless steel reactor lined with polytetrafluoroethylene, and crystallized at 220 ° C for 20 ho...

Embodiment 2

[0047] The first stage (I): Add 0.39ml 1M NaOH solution and 0.44ml 1M KOH solution dropwise to 2.02g silica sol, add 5.5g water after dissolving the silica sol by increasing heat; dissolve 0.11g sodium aluminate in 5.3g water, Add 0.38ml 1M NaOH solution and 0.43ml 1M KOH solution dropwise; slowly add the sodium aluminate solution dropwise into the silicon source solution under stirring conditions to obtain a white colloid, then add 0.16ml FeCl 3 The solution was added to the white colloid, stirred for 2 hours, and finally 0.55ml of cyclohexylamine was added to obtain an initial gel. The material was placed in a stainless steel reactor lined with polytetrafluoroethylene, and crystallized at 220°C for 4 hours.

[0048] The first stage (II): In addition to adding FeCl 3 Solution, the remaining steps are the same as the first stage (I), and finally the material is placed in a stainless steel reactor lined with polytetrafluoroethylene, and crystallized at 220 ° C for 22 hours.

...

Embodiment 3

[0051] The first stage (I): Add 0.43ml 1M NaOH solution and 0.44ml 1M KOH solution dropwise to 2.02g silica sol, add 5.5g water after dissolving the silica sol by increasing heat; dissolve 0.10g sodium aluminate in 5.15g water, Add 0.43ml 1M NaOH solution and 0.43ml 1M KOH solution dropwise; slowly add the sodium aluminate solution dropwise into the silicon source solution under stirring conditions to obtain a white colloid, then add 0.32ml FeCl 3 The solution was added to the white colloid, stirred for 2 hours, and finally 0.55ml of cyclohexylamine was added to obtain an initial gel. The material was placed in a stainless steel reactor lined with polytetrafluoroethylene, and crystallized at 220°C for 6 hours.

[0052] The first stage (II): In addition to adding FeCl 3 Solution, the remaining steps are the same as the first stage (I), and finally the material is placed in a stainless steel reactor lined with polytetrafluoroethylene, and crystallized at 220 ° C for 18 hours.

...

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Abstract

The invention relates to a fractional crystallization synthesis method for synthesizing a high-content skeleton iron ZSM-35 molecular sieve under a static condition. Silica sol, inorganic base, ferric ion solution, cyclohexylamine and deionized water are used as raw materials for synthesizing the molecular sieve. The method has the advantages that iron atoms are introduced into a molecular sieve skeleton in a manner of tetrahedral coordination, introduction quantity of iron is higher, in initial gel, the introduction quantity of the iron reaches Si / Fe=20, the product only has a little or no inactive Fe2O3 impurity phase, crystallization time is short (32 hours), and crystallization degree is higher (more than 90%).

Description

technical field [0001] The invention relates to a synthesis method of molecular sieves, in particular to a step-by-step crystallization synthesis method for synthesizing ZSM-35 molecular sieves with high content of skeleton iron under static conditions. Background technique [0002] Zeolite molecular sieve is a kind of inorganic crystal material with regular pore or cage structure. It has excellent thermal stability, catalytic activity and selectivity, making it an important catalyst in the fields of petroleum refining and fine chemical industry. So far, there are more than 200 topological structures of zeolite molecular sieves found in nature and artificially synthesized. However, only a few of them have been applied industrially (such as LTA, FAU, MOR, MFI, FER, etc.). [0003] The FER structure molecular sieve represented by layered zeolite ZSM-35 (USP4,016,245) is a medium-pore zeolite molecular sieve synthesized by Plank et al. It has 10MR channels and 8MR channels perp...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/44
Inventor 李灿冯兆池鞠晓花范峰滔田福平
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI