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Macroporous 24-ringlet germanium oxide molecular sieve and its prepn

A germanium oxide and molecular sieve technology, applied in the field of molecular sieves, can solve the problem that germanium molecular sieve is not synthesized.

Inactive Publication Date: 2004-10-20
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, so far, ultra-large-pore germanium molecular sieves have not been synthesized

Method used

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  • Macroporous 24-ringlet germanium oxide molecular sieve and its prepn
  • Macroporous 24-ringlet germanium oxide molecular sieve and its prepn
  • Macroporous 24-ringlet germanium oxide molecular sieve and its prepn

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Embodiment 1. in a 50ml beaker, add 5.010 grams of distilled water, then add 8.01 grams of N, N-dimethylformamide (DMF), weigh GeO 2 Pour 0.413 g into the mixed solvent, stir slightly, and then add 2.35 g of tris(2-aminoethyl)amine (TREN). The prepared solution was stirred overnight at room temperature until a homogeneous gel formed. The reactant molar ratio is n(GeO 2 ):n(TREN):n(DMF):n(H 2 (0) = 1:4.08:27.8:70.4. The pH of the reaction gel was 12.2. This was transferred to a polytetrafluoroethylene autoclave with a capacity of 23 ml, and crystallized at 180° C. for 7 days. Take out, filter, wash and dry. The target product was detected by X-ray single crystal structure.

Embodiment 2

[0018] Embodiment 2. Add 5.102 grams of distilled water in a 50ml beaker, then add 8.090 grams of DMF, weigh GeO 2 0.406 g, In(NO 3 ) 3 41 / 2H 2 O 0.339 gram, add in the mixed solvent successively, add TREN 2.361 gram again, stir overnight to become uniform gel, reactant molar ratio is n(GeO 2 ):n(In(NO 3 ) 3 41 / 2H 2 O):n(TREN):n(DMF):n(H 2 (0) = 1:0.227:4.15:26.6:72.8. The pH of the reaction gel was 11.2. This was transferred to a polytetrafluoroethylene autoclave with a capacity of 23 ml, and crystallized at 180° C. for 7 days. Take out, filter, wash and dry. The target product was detected by X-ray single crystal structure.

Embodiment 3

[0019] Embodiment 3. takes GeO in the beaker of 50ml 2 3.767 g, InCl 3 4H 2 O 2.434 grams, add DMF33.998 grams, dubbed solution 1, stir well. Take 5.033 grams of this solution in another beaker, then add 5.010 grams of distilled water, 3.75 grams of DMF, and 2.405 grams of TREN, and stir overnight until a uniform gel is formed. The molar ratio of the reactants is n(GeO 2 ):n(InCl 3 4H 2 O):n(TREN):n(DMF):n(H 2 (0) = 1:0.231:3.63:22.7:61.7. The pH of the reaction gel was 10.6. This was transferred to a polytetrafluoroethylene autoclave with a capacity of 23 ml, and crystallized at 180° C. for 7 days. Take out, filter, wash and dry. The target product was detected by X-ray single crystal structure.

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Abstract

The present invention uses organic polyamine tri(5-aminoethyl) amine as structural guide agent, and adopts mixed solver N, N-dimethyl for mamide (DMF) and water, and controls water content to synthesize pure-phase germanium oxide molecular sieve. Said molecular sieve possesses smallast skeletal desinty and ultralarge pore size, and three-D cross pore canel structure. It is a germinium oxide molecualr sieve possessing zeolite-like structure with 24 metacircle pore canal large pore size.

Description

technical field [0001] The invention belongs to the technical field of molecular sieves, and in particular relates to a novel germanium oxide molecular sieve (FDU-4) with a 24-membered ring macropore three-dimensional channel structure and a preparation method thereof. technical background [0002] Microporous molecular sieves have a wide range of application values ​​in catalysis, gas separation, ion exchange and other fields due to their special and regular pore structure. With the development of industry, many fields have put forward higher requirements for the performance and structure of microporous molecular sieves. For example, the separation of some macromolecules in the field of life, heavy oil cracking, pharmaceuticals and other fields require microporous molecular sieves with ultra-large pore diameters (10-20 Å). This makes the synthesis of new microporous molecular sieve materials with ultra-large pores (greater than 12-membered rings) a hot spot in current rese...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G17/02C01B37/06
Inventor 陈珍霞周亚明赵东元
Owner FUDAN UNIV