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Method for synthesizing zeolite molecular sieve via solid phase method without organic template

A technology for synthesizing zeolites without organic templates, applied in the direction of molecular sieve catalysts, molecular sieves and base exchange compounds, inorganic chemistry, etc., to achieve the effects of increasing single-pot yield, avoiding loss, good crystallinity and purity

Inactive Publication Date: 2013-03-27
BASF AG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, these two methods have their own shortcomings. The method for synthesizing zeolite molecular sieves without organic templates is hydrothermal synthesis, which uses a large amount of solvent water; while in the solid phase method, organic templates are used.

Method used

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  • Method for synthesizing zeolite molecular sieve via solid phase method without organic template
  • Method for synthesizing zeolite molecular sieve via solid phase method without organic template
  • Method for synthesizing zeolite molecular sieve via solid phase method without organic template

Examples

Experimental program
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Effect test

Embodiment 1

[0034] Example 1: Synthesis of ZSM-5 zeolite molecular sieve with relatively low silicon-aluminum ratio by solid-phase method without organic template

[0035] First, weigh the solid raw material 2gNa 2 SiO 3 9H 2 O,0.92gAl 2 (SO 4 ) 3 18H 2 O, 1.3g of solid silica gel and 0.17g of ZSM-5 seed crystals (the amount of seed crystals is based on the input SiO 2 Calculated by mass percentage), pour it into a mortar, grind and mix, grind for 10 minutes, add the reaction raw materials into a polytetrafluoroethylene stainless steel reactor, crystallize at 180°C for 15 hours to complete crystallization, and filter the product. The product is obtained after drying. The proportioning of reaction raw material is as follows:

[0036] SiO 2 : 0.05Al 2 o 3 :0.25Na 2 O : 3H 2 O. The mass ratio of seed crystal to silicon source is 10%.

[0037] According to X-ray diffraction analysis, its structure is ZSM-5 zeolite molecular sieve. attached figure 1 The XRD patterns and scann...

Embodiment 2

[0038] Example 2: The secondary utilization of the product prepared by the solid-phase synthesis of ZSM-5 zeolite molecular sieve without organic template

[0039] First, weigh the solid raw material 2gNa 2 SiO 3 9H 2 O,0.92gAl 2 (SO 4 ) 3 18H 2 O, 1.3g of solid silica gel and 0.17g of ZSM-5 seed crystals (the amount of seed crystals is based on the input SiO 2 The mass percentage is calculated based on the mass percentage, the seed crystal is the product synthesized in Example 1), it is poured into a mortar, and then ground and mixed, ground for 10 minutes, the reaction raw materials are added in a polytetrafluoroethylene stainless steel reaction kettle, crystallized at 180 ° C After 15 hours of complete crystallization, the product was filtered with suction and dried to obtain the product. The proportioning of reaction raw material is as follows:

[0040] SiO 2 : 0.05Al 2 o 3 :0.25Na 2 O : 3H 2 O. The mass ratio of seed crystal to silicon source is 10%.

[00...

Embodiment 3

[0042] Example 3: Synthesis of ZSM-5 zeolite molecular sieve with relatively high silicon-aluminum ratio by solid-phase method without organic template

[0043] First, weigh the solid raw material 1.1gNa 2 SiO 3 9H 2 O,0.3gAl 2 (SO 4 ) 3 18H 2 O, 1.4g solid silica gel and 0.17g ZSM-5 seed crystals (the amount of seed crystals is based on the input SiO 2 Calculated by mass percentage), pour it into a mortar, grind and mix, grind for 10 minutes, add the reaction raw materials into a polytetrafluoroethylene stainless steel reactor, crystallize at 180°C for 15 hours to complete crystallization, and filter the product. The product is obtained after drying. The proportioning of reaction raw material is as follows:

[0044] SiO 2 : 0.016Al 2 o 3 :0.14Na 2 O : 1.5H 2 O. The mass ratio of seed crystal to silicon source is 10%. The obtained product is analyzed by X-ray diffraction and its composition is ZSM-5 zeolite molecular sieve.

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Abstract

The invention relates to a preparation method for a molecular sieve, and aims to provide a method for synthesizing a zeolite molecular sieve via a solid phase method without an organic template. The method comprises the steps of grinding and mixing weighed solid raw materials of silicon source, aluminium source and alkali source; putting the above mixture in a reaction kettle; performing a crystallization reaction for 5 h-20 d at a temperature of 50-200 DEG C; suction-filtering a product, and drying the product to obtain various molecular sieve raw powder. A ZSM-5 zeolite molecular sieve, a Beta zeolite molecular sieve, an FAU zeolite molecular sieve, an MOR zeolite molecular sieve, an LTA zeolite molecular sieve an a GIS zeolite molecular sieve which have relatively good crystallinity and controllable silica-alumina ratio in a certain range can be obtained through the method. The product has good crystallinity and purity; no organic template and solvent is used in the whole production process; so that unnecessary loss in the production process can be prevented greatly. Besides, a conventional method is simplified greatly; and single-kettle yield is increased greatly.

Description

technical field [0001] The invention belongs to a molecular sieve preparation method, in particular to a method for synthesizing a zeolite molecular sieve by combining an organic template-free method and a solid-phase method. Background technique [0002] Molecular sieves are widely used in catalysis, ion exchange, adsorption and separation due to their open structure and large surface area. Research on molecular sieves is closely related to industry, and the exploration of new synthetic routes for molecular sieves is one of the hotspots of researchers. Molecular sieves were first synthesized by hydrothermal method, but only A, X, Y, L and other molecular sieves could be synthesized. After the 1960s, with the use of organic templates, all kinds of molecular sieves were synthesized, which is more important in industry. Such as ZSM-5, Beta and other molecular sieves. [0003] In recent years, the synthesis of zeolite molecular sieves without organic templates has become a ho...

Claims

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Application Information

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IPC IPC(8): C01B39/02C01B39/38
CPCC01B39/02B01J29/06C01B39/38C01B39/20C01B39/26B01J29/08B01J29/18B01J29/70C01B39/14C01B39/46B01J35/30B01J35/617B01J35/633B01J29/40B01J37/009B01J37/04
Inventor 孟祥举吴勤明肖丰收
Owner BASF AG
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