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A method for synthesizing all-silica beta zeolite molecular sieves by a sodium-free and solvent-free route

A beta zeolite, solvent-free technology, applied in the field of molecular sieve preparation, can solve the problems of large amount of template agent and increase the complexity of synthesis, and achieve the effect of improving yield, good crystallinity and purity, and environmental friendliness

Active Publication Date: 2020-08-14
ZHEJIANG JIRUITONG NEW MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, a certain amount of inorganic alkali sodium hydroxide is used in the synthesis process. In order to eliminate sodium ions, post-treatment (ion exchange) is required, which greatly increases the complexity of synthesis.
Previously, it has been reported that all-silicon Beta zeolite molecular sieves can be synthesized without using sodium hydroxide in hydrothermal synthesis (Micropor. Mesopor. Mater., 2010, 127, 104), but the synthesized products are in the state of nanoparticles, which need to be centrifuged. The corresponding product is obtained, and the amount of template agent used is extremely large

Method used

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  • A method for synthesizing all-silica beta zeolite molecular sieves by a sodium-free and solvent-free route
  • A method for synthesizing all-silica beta zeolite molecular sieves by a sodium-free and solvent-free route
  • A method for synthesizing all-silica beta zeolite molecular sieves by a sodium-free and solvent-free route

Examples

Experimental program
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Effect test

Embodiment 1

[0021] Example 1: Synthesis of all-silicon Beta zeolite molecular sieves by a sodium-free and solvent-free route

[0022] 1.6g of solid silica gel, 1.0g of tetraethylammonium hydroxide (T, mass fraction 50%) and 5% all-silicon Beta zeolite molecular sieve seed crystals were placed in a mortar and ground for 10min, and then the reaction materials were added to polytetrafluoroethylene stainless steel In the reaction kettle, crystallize at 140°C for 2 days to complete the crystallization, and the product is suction filtered and dried to obtain the product. The ratio of the reaction raw materials is as follows: SiO 2 :0.15T.

[0023] According to X-ray diffraction analysis, its structure is an all-silicon Beta zeolite molecular sieve such as figure 1 As shown, and through the scanning electron microscope photos, it can be seen that the synthesized product presents a sheet-like morphology, with a thickness of 100-150nm and a length of about 600nm. figure 2 shown.

Embodiment 2

[0024] Example 2: High-temperature synthesis of all-silicon Beta zeolite molecular sieve by a sodium-free and solvent-free route

[0025] 1.6g of solid silica gel, 1.67g of tetraethylammonium hydroxide (T, mass fraction 50%) and 10% all-silicon Beta zeolite molecular sieve seed crystals were placed in a mortar and ground for 10min, and then the reaction raw materials were added to polytetrafluoroethylene stainless steel In the reaction kettle, crystallize at 240°C for 1 hour to complete the crystallization, and the product is filtered with suction and dried to obtain the product. The ratio of the reaction raw materials is as follows: SiO 2 :0.25T.

Embodiment 3

[0026] Example 3: Low-temperature synthesis of all-silicon Beta zeolite molecular sieve by a sodium-free and solvent-free route

[0027] 1.6g of solid silica gel, 1.34g of tetraethylammonium hydroxide (T, mass fraction 50%) and 1% all-silicon Beta zeolite molecular sieve seed crystals were placed in a mortar and ground for 10min, and then the reaction materials were added to polytetrafluoroethylene stainless steel In the reaction kettle, crystallize at 100°C for 6 days to complete the crystallization, and the product is suction filtered and dried to obtain the product. The ratio of the reaction raw materials is as follows: SiO 2 :0.2T.

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Abstract

The invention relates to preparation of a molecular sieve, and aims at providing a method for synthesizing an all-silicon Beta zeolite molecular sieve by a sodium-free solvent-free route. The method for synthesizing the all-silicon Beta zeolite molecular sieve by the sodium-free solvent-free route is concretely characterized in that a silicon source, quaternary ammonium hydroxide and all-silicon seed crystals are put into a mortar; after the grinding is performed for 10 minutes, the materials are put into a reaction kettle; crystallization is performed for 1h to 6d at 100 to 240 DEG C; then, the obtained product is subjected to suction filtration and drying to prepare all-silicon Beta molecular sieve raw powder. The method for synthesizing the all-silicon Beta zeolite molecular sieve by the sodium-free solvent-free route has the advantages that the ion exchange process in the aftertreatment process is avoided; the prepared product does not need filtering or centrifugation; after the roasting, the prepared product can be directly used for performance research.

Description

technical field [0001] The invention relates to the field of molecular sieve preparation, in particular to a method for synthesizing all-silicon Beta zeolite molecular sieves through a sodium-free and solvent-free route. Background technique [0002] With the improvement of people's requirements for environmental protection and the emphasis on air quality, the reduction of PM2.5 emission has become an urgent and challenging issue. Nitrogen oxides (NO x ), volatile organic compounds (VOCs), SO 2 etc. are the main causes and sources of PM2.5, and its efficient elimination is urgent. [0003] VOCs are mainly divided into outdoor sources and indoor sources. Outdoor sources mainly include waste gas from chemical, printing, painting and other industries and automobile exhaust, while indoor sources mainly include harmful substances released from decoration materials, including benzene compounds and formaldehyde. Generally, benzene substances refer to toluene, xylene and styrene...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/04B01J20/18B01J20/30B01D53/02
CPCB01D53/02B01D2257/7027B01J20/186C01B39/04C01P2002/72C01P2004/03
Inventor 吴勤明孟祥举肖丰收
Owner ZHEJIANG JIRUITONG NEW MATERIAL CO LTD
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