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Preparation method of rare earth metal Nd doped H-ZSM-34 molecular sieve

A technology of rare earth metals and molecular sieves, applied in molecular sieve catalysts, including molecular sieve catalysts, chemical instruments and methods, etc., can solve the problems of easy deactivation, short supply, low propylene efficiency, etc., and achieve suitable acidity, long service life and high production efficiency Effect

Inactive Publication Date: 2019-07-23
HENAN NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Propylene can be used to produce important chemical products such as polypropylene, propylene oxide, acetone, isopropanol, phenol, glycerin, etc. It is an indispensable chemical production raw material for the development of modern society and economy. Therefore, there is a need to develop efficient methods for the production of propylene
[0003] At present, the production route of producing propylene from methyl halide is mature, and the reaction of preparing propylene from methyl halide requires a molecular sieve catalyst. Although this method improves the yield of propylene, it is prone to loss due to the pore structure and acidity of the molecular sieve catalyst. Therefore, it is particularly important to prepare molecular sieve catalysts with long catalytic life, good stability and high catalytic performance.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] 3.5g NaAlO 2 , 7g NaOH, 22g KOH and 67.5g water-soluble silica gel were added to 100mL water in sequence, and after stirring for 0.5h, the mixture was aged for 3 days to obtain a clear seed solution, that is, mixture A; 5.54g NaOH and 28.85g water-soluble silica gel were added to 83mL water, stirred for 5h, and then added 2.71g crystal Al 2 (SO4) 3 18H 2 0 and 10mL mixture A obtain precursor solution;

[0025] Step S2: Stir the precursor solution for 0.5h, add Nd(NO 3 ) 3 ·6H 2 O solid, stirred at room temperature for 13h, put into the kettle, crystallized at 120°C for 7d, left the kettle, filtered and washed, dried at 100°C, and then calcined at 550°C in air atmosphere for 6h to obtain Nd-doped Na-ZSM- 34;

[0026] Step S3: Add 2g of Nd-doped Na-ZSM-34 into 40mL of 1mol / L ammonium nitrate solution, stir at 80°C for 3h, filter and wash with suction, and dry the obtained solid at 100°C for 5h;

[0027] Step S4: Repeat operation step S3 four times to obtain Nd-dop...

Embodiment 2

[0031] 3.5g NaAlO 2 , 7g NaOH, 22g KOH and 67.5g water-soluble silica gel were added to 100mL water in sequence, and after stirring for 0.5h, the mixture was aged for 3 days to obtain a clear seed solution, that is, mixture A; 5.54g NaOH and 28.85g water-soluble silica gel were added to 83mL water, stirred for 5h, and then added 2.71g crystal Al 2 (SO4) 3 18H 2 0 and 10mL mixture A obtain precursor solution;

[0032] Step S2: Stir the precursor solution for 0.5h, add Nd(NO 3 ) 3 ·6H 2 O solid, stirred at room temperature for 13h, put into the pot, crystallized at 120°C for 7d, left the pot, filtered and washed, dried at 100°C, and then calcined at 550°C in air atmosphere for 6h to obtain Nd-doped Na-ZSM- 34;

[0033] Step S3: Add 2g of Nd-doped Na-ZSM-34 into 40mL of 1mol / L ammonium nitrate solution, stir at 80°C for 3h, filter and wash with suction, and dry the obtained solid at 100°C for 5h;

[0034] Step S4: Repeat operation step S3 four times to obtain Nd-doped NH ...

Embodiment 3

[0038] 3.5g NaAlO 2 , 7g NaOH, 22g KOH and 67.5g water-soluble silica gel were added to 100mL water in sequence, and after stirring for 0.5h, the mixture was aged for 3 days to obtain a clear seed solution, that is, mixture A; 5.54g NaOH and 28.85g water-soluble silica gel were added to 83mL water, stirred for 5h, and then added 2.71g Al 2 (SO4) 3 18H 2 0 and 10mL mixture A obtain precursor solution;

[0039] Step S2: Stir the precursor solution for 0.5h, add Nd(NO 3 ) 3 ·6H 2 O solid, stirred at room temperature for 13h, put into the pot, crystallized at 120°C for 7d, left the pot, filtered and washed, dried at 100°C, and then calcined at 550°C in air atmosphere for 6h to obtain Nd-doped Na-ZSM- 34;

[0040] Step S3: Add 2g of Nd-doped Na-ZSM-34 into 40mL of 1mol / L ammonium nitrate solution, stir at 80°C for 3h, filter and wash with suction, and dry the obtained solid at 100°C for 5h;

[0041] Step S4: Repeat operation step S3 four times to obtain Nd-doped NH 4 - ZSM...

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Abstract

The invention discloses a preparation method of a rare earth metal Nd doped H-ZSM-34 molecular sieve, the preparation method comprises the following steps of: adding an aluminum source into water, continuously adding an alkali source and a silicon source, stirring and aging to obtain a clear seed crystal solution; sequentially adding sodium hydroxide and water-soluble silica gel into an aqueous solution, stirring, then sequentially adding aluminum sulfate crystals and the seed solution to obtain a precursor solution; adding a Nd(NO3)3.6H2O solid in the precursor solution, stirring at room temperature, putting the mixture into a kettle, crystallizing, taking out of the kettle, filtering by suction, washing, drying and roasting in air to obtain Nd-doped Na-ZSM-34; adding the Nd-doped Na-ZSM-34into an ammonium nitrate solution, stirring, filtering by suction, washing and drying; and repeating ammonium exchange four times to obtain NH4-ZSM-34, and roasting the NH4-ZSM-34 in the air to obtain the rare earth metal Nd doped H-ZSM-34 molecular sieve. The rare earth metal Nd doped H-ZSM-34 molecular sieve prepared by the method has the advantages of unique pore structure, suitable acidity,good stability, larger specific surface area and the like.

Description

technical field [0001] The invention belongs to the technical field of synthesis of H-ZSM-34 molecular sieves, and in particular relates to a preparation method of rare-earth metal Nd-doped H-ZSM-34 molecular sieves. Background technique [0002] Propylene can be used to produce important chemical products such as polypropylene, propylene oxide, acetone, isopropanol, phenol, glycerin, etc. It is an indispensable chemical production raw material for the development of modern society and economy. Therefore, there is a need to develop an efficient method for producing propylene. [0003] At present, the production route of preparing propylene from methyl halide is mature, and the reaction of preparing propylene from methyl halide requires a molecular sieve catalyst. Although this method improves the yield of propylene, it is prone to loss due to the pore structure and acidity of the molecular sieve catalyst. Therefore, it is particularly important to prepare molecular sieve ca...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/50C07C1/26C07C11/06
CPCB01J29/505B01J2229/18C07C1/26C07C2529/50C07C11/06Y02P20/52
Inventor 徐霆岑诗雨杜立方
Owner HENAN NORMAL UNIV
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