Beta type molecular sieve and method of manufacturing the same

A technology of molecular sieves and natural minerals, applied in the direction of crystalline aluminosilicate zeolites, etc., can solve problems such as filtration difficulties, achieve the effects of saving time, improving work efficiency, and improving synthesis efficiency

Active Publication Date: 2011-08-24
CHINA UNIV OF PETROLEUM (BEIJING)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0014] The object of the present invention is not only to prepare β molecular sieve materials with higher thermal and hydrothermal stability, but also to solve the problem of difficult filtration of such materials and improve production efficiency; at the same time, to expand the source of raw materials for preparing β molecular sieves and reduce manufacturing costs It is also an object of the present invention

Method used

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  • Beta type molecular sieve and method of manufacturing the same
  • Beta type molecular sieve and method of manufacturing the same

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0062] Using commercially available bentonite (see attached table 1 for the composition) as raw material, 5 g was roasted in a muffle furnace at 850° C. for 5 hours. Silica sol (containing SiO 2 30wt%) 25g, tetraethylammonium hydroxide solution 18.54g (TEAOH, percentage by weight: 18%), sodium hydroxide 0.51g and the bentonite after roasting treatment drop in the stainless steel reactor, stir 40 minutes and be mixed with the mixture solidified glue. The molar ratio of each component in the gel according to its oxide is: SiO 2 / Al 2 o 3 =24; (Na 2 O+K 2 O) / SiO 2 =0.04;H 2 O / SiO 2 =10; TEAOH / SiO 2 = 0.12. After sealing, heat up to 150°C and crystallize at a constant temperature for 4 days under stirring. After the crystallization is completed, cool and filter to remove the mother liquor, wash and dry the filter cake to obtain a crystallized product.

[0063] As determined by X-ray diffraction (XRD), its phase belongs to β molecular sieve, and the relative crystallini...

Embodiment 2

[0067] Commercially available kaolin with fine grains is used as raw material (50% of the particle size is not greater than 3.1 μm, see attached table 2 for the composition), and 3 g is roasted in a muffle furnace at 850° C. for 6 hours. Silica sol (containing SiO 2 30wt%) 25g, sodium hydroxide 0.51g, tetraethylammonium hydroxide 18.54g (18wt% aqueous solution), and the kaolin after the above-mentioned roasting treatment drop into the stainless steel reactor, stir 30 minutes and be mixed with mixture gel. The molar ratio of each component in the gel according to its oxide is: SiO 2 / Al 2 o 3 =11; (Na 2 O+K 2 O) / SiO 2 =0.04;H 2 O / SiO 2 =12; TEAOH / SiO 2 = 0.15. After the stainless steel reactor was sealed, the temperature was raised to 150°C for crystallization for 4 days. After the crystallization is completed, it only takes 2 minutes to cool down and filter to remove the mother liquor, then wash and dry the filter cake to obtain the crystallized product.

[0068] As...

Embodiment 3

[0072] Kaolin raw material is with example 2, successively silica sol (containing SiO 2 30wt%) 35g, sodium hydroxide 0.67g, tetraethylammonium hydroxide 48g (18wt% aqueous solution), kaolin 2.5g after deionized water 4g and roasting process drop in stainless steel reactor, stir 30 minutes and be mixed with mixture gel . The molar ratio of oxides in the gel is: SiO 2 / Al 2 o 3 =17; (Na 2 O+K 2 O) / SiO 2 =0.04;H 2 O / SiO 2 =19; TEAOH / SiO 2 = 0.3. After the stainless steel reactor was sealed, the temperature was raised to 150°C for crystallization for 6 days. After the crystallization was completed, the mother liquor was removed by filtration (2.5 minutes), and the filter cake was washed and dried to obtain a crystallized product. As determined by X-ray diffraction, the phase is β molecular sieve. The relative crystallinity of the β molecular sieve in the crystallized product is 95%.

[0073] Variation of this method: Add about 0.5g β molecular sieve seed crystals (usi...

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Abstract

The invention provides a method for preparing Beta molecular sieve. The whole or parts of the aluminum sources are provided with the natural minerals such as kaolin and bentonite as raw materials and organic ammonium template is added to carry out crystallization reaction under hydrothermal condition to gain the crystallization product containing Beta molecular sieve. The gained crystallization product can use different post-processing method to prepare modification Beta molecular sieve and can be used as active constituent or carrier of the catalyst. The Beta molecular sieve prepared by the method of the invention has higher heat and hydrothermal stability, solves the problem of difficult filtering of Beta molecular sieve preparation and post-processing and can increase the production efficiency. The invention extends the range of raw materials of the compound Beta molecular sieve, finds novel purpose for more natural minerals and further lowers the cost of preparing Beta molecular sieve.

Description

technical field [0001] The invention belongs to the technical field of molecular sieves and their preparation. Specifically, it relates to using natural minerals to provide all or part of the aluminum source required for synthesizing β-type molecular sieves, using a template method to synthesize β-zeolite and the method thereof. Background technique [0002] Beta molecular sieve (also known as beta zeolite) was first synthesized by Mobil Corporation of the United States in 1967 by the classic hydrothermal crystallization method (US3,308,069), and many synthetic methods have been reported so far. In the structure of β zeolite, there are both large channels of 12-membered rings and medium-sized channels of 10-membered rings. It is a high-silica zeolite with a three-dimensional structure of large pores. The silicon-aluminum molar ratio of the beta zeolite framework is generally between 10 and 200. This structural and compositional feature makes β zeolite have acid catalytic p...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/04
Inventor 申宝剑王萍郭巧霞凌聪高金森张美英
Owner CHINA UNIV OF PETROLEUM (BEIJING)
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