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Green synthetic method for rare earth-containing ZSM-35 molecular sieve

A ZSM-35, green synthesis technology, applied in the field of material chemistry and catalytic chemistry, can solve the problems of complex process operation, high production cost, serious environmental pollution, etc., and achieve simple operation process, good crystallization quality, and simplified process operation. Effect

Inactive Publication Date: 2012-05-23
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to develop a green synthesis method of rare earth-containing ZSM-35 molecular sieve to solve the problems of high production cost, complicated process operation and serious environmental pollution of the organic template synthesis method, and to improve the stability of the molecular sieve by adding rare earth elements

Method used

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  • Green synthetic method for rare earth-containing ZSM-35 molecular sieve
  • Green synthetic method for rare earth-containing ZSM-35 molecular sieve
  • Green synthetic method for rare earth-containing ZSM-35 molecular sieve

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] (1) Raw material

[0020] A. Silica sol (25.7wt% SiO 2 , 0.3wt%Na 2 O, 0.1wt%Al 2 o 3 ): 59.67g;

[0021] B. Sodium metaaluminate solution (NaAlO 2 : 16.8wt%Al 2 o 3 , 31.2wt% NaOH): 7.37g;

[0022] C. dilute sulfuric acid (25.6wt%H 2 SO 4 ): 1.40g;

[0023] D. Deionized water: 156.5g;

[0024] E. ZSM-35 seed crystal: 0.03g;

[0025] F. Lanthanum nitrate [La(NO 3 ) 3 ·6H 2 O]: 0.11g;

[0026] The molar composition of the reaction mixture is: SiO 2 / Al 2 o 3 =20,OH - / Al 2 o 3 = 4.4, H 2 O / Al 2 o 3 =900, La 2 o 3 / Al 2 o 3 =0.01, the seed crystal addition amount is 0.2% of the raw material silicon aluminum oxide mass.

[0027] (2) Operation steps:

[0028] In the case of stirring, add raw material B, 111.5g deionized water (a part of raw material D), raw material A, raw material C and raw material F to the stainless steel reactor in sequence, and continue to stir to make it mix evenly; then add raw material E to 45.0 g g deionized water, af...

Embodiment 2

[0030] (1) Raw materials:

[0031] A. Silica (95wt% SiO 2 ): 8.89g;

[0032] B. Sodium metaaluminate solution (NaAlO 2 : 16.8wt%Al 2 o 3 , 31.2wt% NaOH): 3.91g;

[0033] C. Sodium hydroxide solution (0.1g NaOH / ml): 2.23ml;

[0034] D. Deionized water: 135.0g;

[0035] E.ZSM-35 seed crystal: 0.10g

[0036] F. Cerium nitrate [Ce(NO 3 ) 3 ·6H 2 O]: 0.84g

[0037] The molar composition of the reaction mixture is: SiO 2 / Al 2 o 3 =23,OH - / Al 2 o 3 =5.6,H 2 O / Al 2 o 3 =1200, Ce 2 o 3 / Al 2 o 3 =0.15, the amount of seed crystal added is 1.0% of the mass of the raw material silicon aluminum oxide.

[0038](2) Operation steps:

[0039] In the case of stirring, add raw material B, 105.0g deionized water (a part of raw material D), raw material C and raw material F to the stainless steel reaction kettle in sequence, and continue to stir to mix them evenly; then add raw material E to 30g deionized water , after ultrasonic dispersion, add to the above mixture, st...

Embodiment 3

[0041] (1) Raw material

[0042] A. Solid silica gel (92wt% SiO 2 ): 10.08g;

[0043] B. Sodium metaaluminate solution (NaAlO 2 : 16.8wt%Al 2 o 3 , 31.2wt% NaOH): 2.34g;

[0044] C. Sodium hydroxide solution (0.1g NaOH / ml): 6.89g;

[0045] D. Deionized water: 130.7g;

[0046] E.ZSM-35 seed crystal: 0.97g;

[0047] F. Lanthanum chloride (LaCl 3 ·6H 2 O): 0.27g;

[0048] The molar composition of the reaction mixture is: SiO 2 / Al 2 o 3 =40,OH - / Al 2 o 3 =9.2,H 2 O / Al 2 o 3 =2000, La 2 o 3 / Al 2 o 3 =0.10, the amount of seed crystal added is 10.0% of the mass of the raw material silicon aluminum oxide.

[0049] (2) Operation steps:

[0050] Under the condition of stirring, add raw material B, 100.7g deionized water (raw material D), raw material C and raw material F to the stainless steel reaction kettle in sequence, continue to stir to make it mix evenly; then add raw material E to 30g deionized water, ultrasonic After dispersing, add it to the above mi...

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Abstract

The invention provides a green synthetic method for a rare earth-containing ZSM-35 molecular sieve, which is characterized in that silicon source, aluminum source, deionized water, salt of rare earth element, seed and inorganic acid or inorganic base are taken as initial raw materials; wherein the mol ratio of the initial raw materials comprises: SiO2: Al2O3 is 15-40, OH<->:Al2O3 is 2.5-9.2, H2O: Al2O3 is 300-2000, RE2O3: Al2O3 is 0.01-0.56, the addition of the seed accounts for 0.1-10.0% of total mass of raw material silicon aluminum oxide, a reaction initial raw material mixture is crystallized for 20-72 hours under the authigenic pressure and crystallization temperature of 150-200 DEG C, the rare earth-containing ZSM-35 molecular sieve is prepared by hydrothermal synthesis, and the invention has the advantages of simple process, friend environment, low cost and good products crystallization quality, the rare earth element is directly introduced in a molecular sieve frame during the synthesis process, so that the stability of the molecular sieve is enhanced.

Description

technical field [0001] The invention relates to the technical fields of material chemistry and catalytic chemistry, and in particular provides a green synthesis method of rare earth-containing ZSM-35 molecular sieves. Background technique [0002] ZSM-35 molecular sieve is a layered molecular sieve material with Ferrierite (FER) topology developed by Mobil Corporation of the United States in 1977 (USP4,016,245). ZSM-35 belongs to the orthorhombic crystal system and has a vertically intersecting two-dimensional channel system. The size of the ten-membered ring channel parallel to the [001] plane is 0.42×0.54nm, and the size of the eight-membered ring channel parallel to the [010] plane is 0.35×0.48nm. Due to its suitable pore channels, excellent thermal / hydrothermal stability and acidity, ZSM-35 molecular sieve is widely used in hydrocarbon conversion processes such as isomerization, polymerization and cracking. [0003] At present, the templates used in the synthesis of ZS...

Claims

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Application Information

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IPC IPC(8): C01B39/44
Inventor 徐龙伢张玲刘盛林谢素娟王清遐
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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