Preparation method and application of stepped hole Beta molecular sieve

A molecular sieve and stepped pore technology, used in molecular sieve catalysts, preparation of organic compounds, molecular sieves and alkali exchange compounds, etc., can solve the problems of waste liquid discharge, destruction of molecular sieve crystal framework, and difficulty in controlling mesopore pore size, to avoid pollution, High BET specific surface area and improved selectivity

Inactive Publication Date: 2017-12-01
FUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The advantage of this post-treatment method is that it is convenient and simple, but it is difficult to control the formed mesopore diameter, and the post-treatment may cause damage to the molecular sieve crystal skeleton, and generate a large amount of waste liquid discharge, which is also a non-green process.

Method used

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  • Preparation method and application of stepped hole Beta molecular sieve
  • Preparation method and application of stepped hole Beta molecular sieve
  • Preparation method and application of stepped hole Beta molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Dissolve 0.8 g of NaOH solid in 16.6 g of deionized water and stir well. Then add 0.65 g of kaolin activated by sub-molten salt, and stir in a water bath at 70°C for 4 hours; then slowly add 3.3 g of white carbon black and 0.3 g of Beta molecular sieve seeds into the above solution, and stir for 30 minutes; the molar ratio in terms of oxide For: 40SiO 2 :Al 2 o 3 :10Na 2 O:660H 2 O. The above mixture was charged into a stainless steel reaction kettle lined with polytetrafluoroethylene, and statically crystallized at 140° C. for 18 hours. After cooling, the solid product was filtered, washed, and dried at 120°C for 12 hours to obtain the original Beta molecular sieve powder. After powder X-ray diffraction analysis, it is determined that the product is a pure-phase BEA molecular sieve with a relative crystallinity of 110%. The BET specific surface area of ​​the product is 666m 2 / g.

[0039] The Beta molecular sieve is used in the reaction of synthesizing ethyl ac...

Embodiment 2

[0041] Same as embodiment 1, only silicon source white carbon black is replaced by silica sol (SiO 2 Content is 30 wt%), keep the raw material molar ratio as 40SiO 2 :Al 2 o 3 :10Na 2 O:660H 2 O. After powder X-ray diffraction analysis, it is determined that the product is a pure-phase BEA molecular sieve with a relative crystallinity of 102%, and the BET specific surface area of ​​the product is 605 m 2 / g.

[0042] The Beta molecular sieve is used in the reaction of synthesizing ethyl acetate from acetic acid and ethanol, and the reaction is continuously reacted in a fixed-bed reactor.

Embodiment 3

[0044] Same as Example 1, only the ratio of water to silicon is changed to 20 (that is, the amount of water added becomes 20.2 g), and the molar ratio in terms of oxides is: 40SiO 2 :Al 2 o 3 :10Na 2 O:800H 2 O. Static crystallization at 140°C for 18 hours. After powder X-ray diffraction analysis, it is determined that the product is a pure-phase BEA molecular sieve with a relative crystallinity of 105%, and the BET specific surface area of ​​the product is 625 m 2 / g.

[0045] The Beta molecular sieve is used in the reaction of synthesizing ethyl acetate from acetic acid and ethanol, and the reaction is continuously reacted in a fixed-bed reactor.

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Abstract

The invention relates to a preparation method and application of a stepped hole Beta molecular sieve, and belongs to the field of preparation of molecular sieves. The method is characterized in that the macroporous-microporous composite stepped hole Beta molecular sieve is synthesized by taking sub-molten salt activated kaolin or rectorite as all of an aluminum source and part of a silicon source, uniformly mixing the activated minerals, an alkali source, an supplemented silicon source, crystal seeds and deionized water according to a certain ratio under the condition of adding no organic template agent and performing one-step hydrothermal crystallization. According to the method provided by the invention, the sub-molten salt activated natural minerals are used as all of the aluminum source and part of the silicon source, and no organic template agent is used in the synthesis process, thereby greatly lowering the synthesis cost of the Beta molecular sieve, and obviously improving the greenness in the production process of the molecular sieve material; and the synthesized Beta molecular sieve is a macroporous-microporous composite stepped hole material, and has high relative crystallinity and high BET specific surface area, thereby having favorable industrial application prospects.

Description

technical field [0001] The invention belongs to the field of molecular sieve preparation, and in particular relates to a method for preparing a stepped pore Beta molecular sieve. Background technique [0002] Beta molecular sieve was first synthesized by Wadlinger of Mobil Company in 1967, and its successful synthesis marked the beginning of the era of high silica zeolite. Beta molecular sieve has a unique pore structure, suitable acidity, and good thermal and hydrothermal stability. It is an important catalyst and adsorption material and is widely used in the fields of petroleum refining, petrochemical and fine chemical synthesis. As we all know, tetraethylammonium hydroxide (TEAOH) is currently the most widely used template for the synthesis of Beta molecular sieves. However, the use of organic templates also brings many negative problems. First, organic species used as templates are generally expensive, and their own synthesis process is complicated and cumbersome; seco...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/46B01J29/70C07C67/08C07C69/14
CPCC01B39/46B01J29/7007C01P2002/72C01P2006/12C01P2006/17C07C67/08C07C69/14
Inventor 岳源源刘涛李晓平鲍晓军袁珮白正帅朱海波
Owner FUZHOU UNIV
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