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Bi-metal atom modified MCM-41 mesoporous molecular sieve and preparation method thereof

A technology of mesoporous molecular sieve, MCM-41, applied in the direction of crystalline aluminosilicate zeolite, etc., can solve the problems of low hydrothermal stability, application limitation, and less lattice defects.

Inactive Publication Date: 2009-02-18
SHANGHAI INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is to solve the problems in the prior art, due to the few lattice defects in the MCM-41 skeleton, the lack of protonic acid and L acid center, and the mesoporous molecular sieve hole wall is an amorphous state, resulting in its (Al-MCM-41 Such as single atom substituted molecular sieve) hydrothermal stability is relatively low, the problem that the application in catalytic reaction is limited

Method used

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  • Bi-metal atom modified MCM-41 mesoporous molecular sieve and preparation method thereof
  • Bi-metal atom modified MCM-41 mesoporous molecular sieve and preparation method thereof
  • Bi-metal atom modified MCM-41 mesoporous molecular sieve and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0044] Preparation of Double Metal Atom Modified Co-La-MCM-41

[0045] The molar proportions of the reactants are respectively:

[0046] 1. n(CTAB):n(TEOS):n(Co(NO 3 ) 3 ·6H 2 O):n(La(NO 3 )·6H 2 O):

[0047] n(NaOH):n(H 2 O)=1:3.75:0.1125:0.1125:1.64:434

[0048] 2. n(CTAB):n(TEOS):n(Co(NO 3 ) 3 ·6H 2 O):n(La(NO 3 )·6H 2 O):

[0049] n(NaOH):n(H 2 O)=1:3.75:2.0:2.0:1.64:434

[0050] 3. n(CTAB):n(TEOS):n(Co(NO 3 ) 3 ·6H 2 O):n(La(NO 3 )·6H 2 O):

[0051] n(NaOH):n(H 2 O)=1:3.75:3.75:3.75:1.64:434

[0052] Preparation:

[0053] At room temperature, mix 4g of cetyltrimethylammonium bromide (CTAB) and 9mL of 2mol·L -1 Sodium hydroxide solution (dissolve 0.72g sodium hydroxide in 9mL deionized water to form a solution) in 75mL deionized water was stirred, mixed and dissolved; then slowly added dropwise 8.56gTEOS and continued to stir; at the same time, slowly added dropwise cobalt nitrate aqueous solution (molar ratio 0.1125 0.3593g --- molar ratio 2.0 is ...

Embodiment 2

[0055] Preparation of Double Metal Atom Modified Fe-La-MCM-41

[0056] The molar ratio of reactants is:

[0057] 1. n(CTAB):n(TEOS):n K 3 [Fe(CN) 6 ]:n(La(NO 3 )·6H 2 O):n(NaOH):

[0058] n(H 2 O)=1:3.75:0.1125:0.1125:1.64:434

[0059] 2. n(CTAB):n(TEOS):n K 3 [Fe(CN) 6 ]:n(La(NO 3 )·6H 2 O):n(NaOH):

[0060] n(H 2 O)=1:3.75:2.0:2.0:1.64:434

[0061] 3. n(CTAB):n(TEOS):n K 3 [Fe(CN) 6 ]:n(La(NO 3 )·6H 2 O):n(NaOH):

[0062] n(H 2 O)=1:3.75:3.75:3.75:1.64:434

[0063] Preparation

[0064] At room temperature, mix 4g of cetyltrimethylammonium bromide (CTAB) and 9mL of 2mol·L -1 Sodium hydroxide solution (dissolve 0.72g sodium hydroxide in 9mL deionized water to form a solution) in 75mL deionized water was stirred, mixed and dissolved; then slowly added dropwise 8.56g TEOS and continued to stir; at the same time, slowly added dropwise hexacyanoferric (III ) Potassium chloride aqueous solution (use 0.4065g potassium hexacyanoferrate (III) potassium hexacyanof...

Embodiment 3

[0066] Preparation of Bimetallic Atom Modified Cr-La-MCM-41

[0067] The molar ratio of reactants is:

[0068] 1. n(CTAB):n(TEOS):n(Cr(NO 3 )·9H 2 O, AR):n(La(NO 3 )·6H 2 O):

[0069] n(NaOH):n(H 2 O)=1:3.75:0.1125:0.1125:1.64:434

[0070] 2. n(CTAB):n(TEOS):n(Cr(NO 3 )·9H 2 O, AR):n(La(NO 3 )·6H 2 O):

[0071] n(NaOH):n(H 2 O)=1:3.75:2.0:2.0:1.64:434

[0072] 3. n(CTAB):n(TEOS):n(Cr(NO 3 )·9H 2 O, AR):n(La(NO 3 )·6H 2 O):

[0073] n(NaOH):n(H 2 O)=1:3.75:3.75:3.75:1.64:434

[0074] Preparation

[0075] At room temperature, mix 4g of cetyltrimethylammonium bromide (CTAB) and 9mL of 2mol·L -1 Sodium hydroxide solution (dissolve 0.72g sodium hydroxide in 9mL deionized water to make a solution) in 75mL deionized water, stir and mix and dissolve; then slowly add 8.56g TEOS dropwise and continue stirring; ——2.0 is 8.7836g; 3.75 is 16.4693g of chromium nitrate dissolved in 5mL of deionized water to make a solution) and lanthanum nitrate aqueous solution (use 0....

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Abstract

The invention relates to an improved MCM-41 mesoporous molecular sieve and a preparation method thereof, in particular relates to a dual-metal-atom improved MCM-41 mesoporous molecular sieve and the preparation method thereof. The molecular sieve consists of hexadecyl trimethyl ammonium bromide, ethyl orthosilicate, sodium hydroxide, Me metal salt (Co, Ni, Cr, Fe, Cu, V), lanthanum nitrate and water. The molecular sieve is prepared in the steps: at the room temperature, hexadecyl trimethyl ammonium bromide is mixed and dissolved with the sodium hydroxide, and is added with TEOS in dropping way, and simultaneously added with Me metal salt water solution and lanthanum nitrate solution in dropping way; the pH value of the mixed solution is adjusted by acetic acid to be 10 to 11, and is mixed for 1 to 2 hours after being stabilized; the sol is moved into a polyfluortetraethylene bottle to be heated and crystallized for 2 days in the oven at the temperature of 100 DEG C; after filtering, washing and drying for nights, and being calcined in a muffle at the temperature of 550 DEG C for 3 to 7 hours, the dual-metal-atom improved MCM-41 mesoporous molecular sieve is obtained. The product can simultaneously improve the acid performance and the water heating stability of the MCM-41 mesoporous molecular sieve, and can enlarge the actual application of the MCM-41 mesoporous molecular sieve in the catalyst filed.

Description

technical field [0001] The invention relates to an MCM-41 mesoporous molecular sieve and a preparation method thereof, in particular to a double metal atom modified MCM-41 mesoporous molecular sieve and a preparation method thereof. Background technique [0002] Mesoporous molecular sieves (also known as mesoporous molecular sieves) refer to surfactants as templates, using chemical processes such as sol-gel (sol-gel), emulsification (emulsion) or microemulsion (micromulsion), through organic and inorganic A class of inorganic porous materials with a pore size between 1.3 and 30 nm, a narrow pore distribution and a regular pore structure assembled by the interface interaction between them. [0003] In 1992, scientists from Mobile Corporation in the United States synthesized the M41S series mesoporous molecular sieves for the first time. Because this material has certain chemical and thermodynamic stability, regular channels, adjustable pore size, stable skeleton structure, ce...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/02
Inventor 项婷婷俞磊王宇红
Owner SHANGHAI INST OF TECH
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