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Preparation method of A type molecular sieve with hierarchical duct

A technology of molecular sieves and channels, which is applied in the field of preparation of multi-channel A-type molecular sieves, can solve the problems of single channels and poor separation effects, and achieve the effects of shortening the cycle, increasing the force, and large specific surface area

Inactive Publication Date: 2015-01-14
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The object of the present invention is to solve the problem of single channel and poor separation effect of microporous type A molecular sieve, and provide a preparation method of multistage channel type A molecular sieve, which specifically includes the following steps:

Method used

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  • Preparation method of A type molecular sieve with hierarchical duct
  • Preparation method of A type molecular sieve with hierarchical duct
  • Preparation method of A type molecular sieve with hierarchical duct

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Weigh 2.40g of sodium hydroxide solid and 1.64g of sodium metaaluminate and dissolve them in 14.13mL of deionized water, stir and dissolve until clear; add 4.80g of silica sol and 0.12g of TPOAC to the above solution while stirring, and stir and age for 1h; Then transfer the mixture to a stainless steel kettle lined with polytetrafluoroethylene, put it in an oven at 80°C for crystallization for 4 hours; filter and separate, wash the filter residue with deionized water until the pH is lower than 9, and place the washed filter residue in the oven Dry at 90°C overnight, then put it in a muffle furnace, and bake at 500°C for 3 hours to remove the organosilane template, and then obtain a type A molecular sieve with hierarchical channels.

[0025] The specific surface area of ​​the multi-stage channel type A molecular sieve described in this embodiment is 589m 2 / g, the channels are evenly distributed between mesopores and micropores.

Embodiment 2

[0027] Weigh 1.60g of sodium hydroxide solid and 3.28g of sodium metaaluminate and dissolve in 17.64mL of deionized water, stir and dissolve until clear; add 12.00g of silica sol and 2.36g of TPOAC to the above solution while stirring, and stir and age for 5h; Then transfer the mixture to a stainless steel kettle lined with polytetrafluoroethylene, put it in an oven at 110°C for crystallization for 9 hours; filter and separate, wash the filter residue with deionized water until the pH is lower than 9, and place the washed filter residue in the oven Dry at 90°C overnight, then place it in a muffle furnace, and bake at 600°C for 6 hours to remove the organosilane template to obtain a molecular sieve with hierarchical channels A.

[0028] The specific surface area of ​​the multi-stage channel type A molecular sieve prepared in this example is 621m 2 / g, the channels are evenly distributed between mesopores and micropores.

Embodiment 3

[0030] Weigh 1.76g of sodium hydroxide solid, 1.31g of sodium metaaluminate and dissolve in 18.50mL of deionized water, stir and dissolve until clear; add 3.60g of silica sol and 1.18g of TPOAC to the above solution while stirring, and stir and age for 4h; Then transfer the mixture to a stainless steel kettle lined with polytetrafluoroethylene, put it in a 90°C oven for crystallization for 7 hours; filter and separate, wash the filter residue with deionized water until the pH is lower than 9, and place the washed filter residue in the oven Dry at 90°C overnight, then place in a muffle furnace, and bake at 550°C for 4 hours to remove the organosilane template to obtain a molecular sieve with hierarchical channels A.

[0031] The XRD spectrogram of the multi-stage channel type A molecular sieve prepared in this embodiment is as follows Figure 2~3 shown, where figure 2 The XRD spectrum of the multi-stage channel A molecular sieve, image 3 It is the small-angle diffraction sp...

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Abstract

The invention discloses a preparation method of an A type molecular sieve with a hierarchical duct, belonging to the preparation field of a zeolite molecular sieve. The preparation method comprises the following steps: adding a certain amount of sodium hydroxide and sodium metaaluminate into deionized water, adding silica sol and trimethoxysilylpropyl dimethyl octadecyl ammonium chloride (TPOAC) under stirring, ageing the liquid for 1-5 hours; then, filling the aged liquid into a hydrothermal synthesis kettle for crystallizing for 4-9 hours at 80-110 DEG C; and obtaining the A type molecular sieve with the hierarchical duct by virtue of steps such as filtering, washing, drying and roasting, wherein a molar ratio of reactants is that Na2O / SiO2 / Al2O3 / H2O / TPOAC is (2-4) / (1-5) / (0.5-2) / (90-150) / (0.01-0.2). The preparation method disclosed by the invention is simple, capable of introducing a mesoporous material into a microporous A type molecular sieve, so that the A type molecular sieve has a structure of the hierarchical duct.

Description

technical field [0001] The invention relates to a method for preparing a multi-channel A-type molecular sieve, which belongs to the field of preparation of zeolite molecular sieves. technical background [0002] The hierarchical pore structure zeolite molecular sieve material refers to that this type of zeolite material has pore structures of other sizes, such as mesopore and macropore structures, in addition to the micropores of the zeolite itself. Although the particle size of this type of material itself may be on the micron scale, the secondary or even tertiary pores in the material can make it easier for guest molecules to enter the interior of the material for adsorption and catalysis, and the main structure of the microporous zeolite overcomes the pure mesoporous material water. The disadvantage of poor thermal stability. Therefore, compared with conventional molecular sieves, multi-level pore zeolite molecular sieves have the following advantages as adsorbents: (1) ...

Claims

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Application Information

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IPC IPC(8): C01B39/14
CPCC01B39/145C01P2006/17C01P2006/12C01P2002/72
Inventor 刘艳娜肖松龙代奎唐晓宁祝琳华孙彦琳
Owner KUNMING UNIV OF SCI & TECH
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