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Molecular sieve containing bismuth and its synthesis and use

A molecular sieve, atomic technology, applied in the field of synthesis of MCM-41 molecular sieve, can solve the problems of low conversion rate and low oxidation activity

Inactive Publication Date: 2007-10-10
FUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The unique oxidation activity of heteroatom-containing MCM-41 has attracted more and more attention, but the oxidation activity of the above-mentioned heteroatom MCM-41 molecular sieves is low, and the general conversion rate is less than 10%.

Method used

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  • Molecular sieve containing bismuth and its synthesis and use

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 0.192molCTAB (cetyltrimethylammonium bromide), 0.9molTEOS (ethyl silicate), 0.01molBi (NO 2 ) 3 ·5H 2 O, 0.3molNaOH and 900ml distilled water are mixed evenly, and the molar composition of the mixture is OH - :Bi:SiO 2 :R:H 2The ratio of O is 0.33:0.011:1:0.21:56, and the mixed solution is transferred into an autoclave lined with polytetrafluoroethylene and allowed to stand for crystallization for 48 hours, and the crystallization temperature is 110°C. After crystallization, the sample was taken out, washed and filtered several times, then dried, and fired at 550°C for 10 hours to obtain Bi-MCM-41 molecular sieve. It is numbered T-1, and its XRD crystal phase diagram is shown in Figure 1. The diffraction peak at 2.36° corresponds to the 100 crystal plane, the diffraction peak at 4.12° corresponds to the 110 crystal plane, and the diffraction peak at 4.62° corresponds to the 200 crystal plane. The diffraction peak at 6.02° corresponds to the 210 crystal plane. The ...

Embodiment 2

[0025] 0.192molCTACl (cetyltrimethylammonium chloride), 1100ml distilled water, 0.25molNaOH, 0.9molTEOS (ethyl silicate), 1×10 -4 mol of AlCl 3 and 0.01molBi(NO 2 ) 3 ·5H 2 O is mixed evenly, and the molar composition of the mixture is OH - :Bi:Al:SiO 2 :CTACl:H 2 O was 0.28:0.011:0.0001:1:0.21:68, and the mixed solution was transferred into an autoclave lined with polytetrafluoroethylene and allowed to stand for crystallization for 72 hours, and the crystallization temperature was 120°C. After crystallization, the sample was taken out, washed and filtered several times, then dried, and fired at 550°C for 10 hours to obtain Bi-Al-MCM-41 molecular sieve. It is numbered as T-2, and the test conditions of its XRD spectrum are the same as in Example 1, and the peak type and position of the crystal phase diagram diffraction peaks are similar to those in Figure 1.

Embodiment 3

[0027] 0.17mol CTAB (cetyltrimethylammonium bromide), 445ml distilled water, 0.24molNaOH, 0.8mol silica sol (SiO 2 Concentration is 1.0mol / L), 2×10 -4 mol of Ti(SO 4 ) 2 and 0.01molBi(NO 2 ) 3 ·5H 2 O is mixed evenly, and the molar composition of the mixture is OH - :Bi:Ti:SiO 2 :CTAB:H 2 O was 0.3:0.012:0.00025:1:0.21:84, and the mixed solution was transferred into a polytetrafluoroethylene-lined autoclave and allowed to stand for crystallization for 36 hours, and the crystallization temperature was 160°C. After crystallization, the sample was taken out, washed and filtered several times, then dried, and fired at 550°C for 10 hours to obtain Bi-Ti-MCM-41 molecular sieve. It is numbered as T-3, and the test conditions of its XRD spectrum are the same as in Example 1, and the peak type and position of the crystal phase diagram diffraction peaks are similar to those in Figure 1.

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Abstract

The Bi-containing MCM-41 molecular sieve features that the molecular sieve contains Bi and optional B, Sn, Sb, Al, Pb, Po, Zn, Mn, Ti, V, and W, and the total atom molar ratio to Bi atom is 0-0.2 and the molar SiO2 / Bi ratio is 10-250. The molecular sieve has the said elements combined to the molecular sieve via hydrothermal synthesis process, and may be used as catalyst for oxidation reaction.

Description

technical field [0001] The invention relates to the synthesis of a molecular sieve MCM-41 with a special crystal structure, in particular to the synthesis of the MCM-41 molecular sieve containing bismuth atoms or bismuth and a small amount of other atoms. Background technique [0002] In 1992, the Mobil Petroleum Company of the United States synthesized the M41S series of new mesoporous SiO for the first time. 2 Materials (C T Kresge, M ELeonowicz, W J Roth, J C Vartuli and J S Back, Nature, 1992, 359, 710), among which the MCM-41 mesoporous molecular sieve is the most attractive. MCM-41 has the following salient features: 1. It has a uniform and regular pore structure with a pore size of 1.5-10nm, and the pore size can be adjusted by selecting appropriate surfactants, auxiliary directing agents and reaction parameters; 2. It has relatively high thermal stability. High; 3. Medium acid strength; 4. Very high BET specific surface area and pore volume; 5. Catalysts based on MC...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/076
Inventor 陈晓晖林性贻魏可镁郑起
Owner FUZHOU UNIV