Inorganic synthesis method for regulating morphology of ZSM-5 molecular sieve

An inorganic synthesis, ZSM-5 technology, applied in the direction of crystalline aluminosilicate zeolite, borocarbane silicone crystalline aluminosilicate zeolite, etc., can solve the problems of irreversible agglomeration of nano ZSM-5 molecular sieve, increased cost, environmental pollution, etc. , to achieve good economic and social benefits, reduce pollution, and avoid waste gas

Active Publication Date: 2017-01-25
SHANGHAI ADVANCED RES INST CHINESE ACADEMY OF SCI
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Problems solved by technology

[0003] In view of the shortcomings of the prior art described above, the object of the present invention is to provide an inorganic synthesis method for regulating the morphology of ZSM-5 molecular sieves, which is used to solve the problem of the need to add an organic template as a directing agent or add organic ma

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  • Inorganic synthesis method for regulating morphology of ZSM-5 molecular sieve
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  • Inorganic synthesis method for regulating morphology of ZSM-5 molecular sieve

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[0032] like figure 1 As shown, the present invention relates to a kind of inorganic synthesis method of regulating and controlling ZSM-5 molecular sieve morphology, and it at least comprises the following steps:

[0033] Step (1): Add silicon source, alkali source, and aluminum source into pure water respectively, and stir evenly to obtain silica-alumina gel.

[0034] Step (2): adding molecular sieve shape-adjusting inorganic additives and zeolite seed crystals to the silica-alumina gel, and stirring evenly to obtain a gel mixture.

[0035] Step (3): transfer the gel mixture to a sealed reaction kettle for crystallization, and then separate and dry the crystallized product to obtain ZSM-5 molecular sieve.

[0036] Among them, the morphology of the ZSM-5 molecular sieve is suitable for regulation by adjusting the morphology of the molecular sieve and adjusting the addition amount of inorganic additives.

[0037]In step (2), the molecular sieve morphology adjustment inorganic ...

Embodiment 1

[0049] Take by weighing 113g silica sol (SiO 2 Content is 30%) and 77g pure water are mixed, then add 1.51g sodium hydroxide, after stirring evenly, then add 3.1g sodium aluminate (Al 2 o 3 content is 75%), continue to stir until a uniform silica-alumina gel is formed, and the molar ratio of each component in the silica-alumina gel is SiO 2 :Al 2 o 3 : Na 2 O: H 2 O=30:1:2:460. After that, add SiO 2 :Al 2 o 3 =25 MFI type molecular sieve seed crystal 1.7g stirred evenly, finally added 2.6g hydrogen peroxide solution (H 2 o 2 content is 30%), after stirring evenly, the mixture was transferred to a stainless steel sealed reaction kettle with polytetrafluoroethylene lining, placed in an oven at 170°C, and crystallized for 48 hours. The crystallized product was cooled, separated (including filtering and washing) and then dried at 120°C for 8 hours to obtain ZSM-5 molecular sieve.

[0050] figure 2 It is the XRD spectrogram of the ZSM-5 molecular sieve sample obtained...

Embodiment 2

[0053] Take by weighing 184g silica sol (SiO 2 content is 30%) and 101g water are mixed, then add 10.3g sodium hydroxide, after stirring evenly, then add 2.5g pseudo-boehmite (Al 2 o 3 Content is 75%) and 1.2g zinc nitrate, continue to stir until forming uniform silica-alumina gel, the molar ratio of each composition in this silica-alumina gel is SiO 2 :Al 2 o 3 : Na 2 O: H 2 O=50:1:7:700. After that, add SiO 2 :Al 2 o 3 =400 MFI type molecular sieve seed crystal 4.5g stir evenly, finally add 1.5g hydrogen peroxide solution (H 2 o 2 content 30%), after stirring evenly, the mixture was transferred to a stainless steel sealed reaction kettle with polytetrafluoroethylene lining, placed in an oven at 155° C., and crystallized for 60 hours. The crystallized product was cooled, separated (including filtering and washing), and then dried at 120°C for 8 hours to obtain Zn-ZSM-5 molecular sieve.

[0054] Figure 4 It is the scanning electron microscope picture of the ZSM-5...

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Abstract

The invention provides an inorganic synthesis method for regulating the morphology of a ZSM-5 molecular sieve. The method at least comprises the following steps: (1) adding a silicon source, an alkali source and an aluminum source into pure water respectively, and stirring uniformly to obtain silica-alumina gel; (2) adding a molecular sieve morphology regulation inorganic additive and a zeolite seed crystal into the silica-alumina gel, and stirring uniformly to obtain a gel mixture; and (3) transferring the gel mixture into a sealed reaction kettle for crystallization, and then separating and drying the crystallized product to obtain a ZSM-5 molecular sieve, wherein the morphology of the ZSM-5 molecular sieve is suitable to be controlled by regulating the addition amount of the molecular sieve morphology regulation inorganic additive. Through the method provided by the invention, a low-silicon ZSM-5 molecular sieve with a regulatable morphology and a silica-alumina ratio controllable in a certain range can be obtained, and the low-silicon ZSM-5 molecular sieve has relatively high crystallinity and purity and good aromatization reaction performance; and moreover, a roasting step is saved in the production process, and environmental pollution is reduced.

Description

technical field [0001] The invention belongs to the field of inorganic chemistry and relates to the technical field of molecular sieve preparation, in particular to an inorganic synthesis method for regulating the morphology of ZSM-5 molecular sieve. Background technique [0002] The ZSM-5 molecular sieve with MFI structure and its heteroatom-substituted molecular sieves are widely used in aromatization and other reactions due to their strong acidity. At present, the development of aromatization catalysts mainly focuses on the 2 / Al 2 o 3 Relative, strongly acidic, small-grain ZSM-5 molecular sieves are synthesized and modified, among which, the morphology regulation of ZSM-5 molecular sieves also has an important influence on the catalyst activity and selectivity. For example, the straight channels parallel to the b-axis in ZSM-5 molecular sieve crystals are more conducive to the transport and diffusion of molecules in it, while the zigzag-type channels parallel to the a...

Claims

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Application Information

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IPC IPC(8): C01B39/38
CPCC01B39/38C01P2002/72C01P2004/03C01P2004/20C01P2004/32
Inventor 杨承广吴晛刘子玉丘明煌陈新庆曾高峰孙予罕
Owner SHANGHAI ADVANCED RES INST CHINESE ACADEMY OF SCI
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