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Method for synthesizing laminar ZSM-5 zeolite molecular sieve with single micro-molecule organic template

An organic template agent, zeolite molecular sieve technology, applied in the direction of crystalline aluminosilicate zeolite, borocarbonane silicone crystalline aluminosilicate zeolite, etc., can solve the complex steps of synthesizing the template agent, the aluminum atom is difficult to enter, and the synthesis cost is increased. and other problems, to achieve the effect of good crystallinity and purity, good catalytic activity and low price

Active Publication Date: 2017-04-26
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

These two methods require the presence of two templates to achieve synthesis, and the synthesis cost is relatively high
In 2009, Ryoo et al. designed a long-chain organic template and successfully synthesized a nano-flake ZSM-5 zeolite with a large number of mesoporous pores. However, the steps for synthesizing the template are extremely complicated, which greatly increases the synthesis cost.
It is worth pointing out that this template is a cheap and easy-to-obtain template that has been commercialized. However, the phosphine species will remain in the pores during the calcination process of the phosphine-containing organic template, which will affect its catalytic performance.
Okubo et al. designed a tetrapropylammonium dimer as a small molecule organic template, synthesized a ZSM-5 zeolite with a 90-degree flaky intersection, and pointed out that the existence of dimer tetrapropylammonium is the key to synthesis. The key to this type of ZSM-5 zeolite is that in this synthesis, it is difficult for aluminum atoms to enter the zeolite framework, which greatly affects its further application

Method used

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  • Method for synthesizing laminar ZSM-5 zeolite molecular sieve with single micro-molecule organic template
  • Method for synthesizing laminar ZSM-5 zeolite molecular sieve with single micro-molecule organic template
  • Method for synthesizing laminar ZSM-5 zeolite molecular sieve with single micro-molecule organic template

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Example 1: Synthesis of all-silicon ZSM-5 zeolite with a new and cheap single small molecule organic template

[0022] 5g H 2 O, 0.28g NaOH, 1.0g organic template (T, structure such as figure 1 ) and 3.9 g of silica sol with a silicon dioxide content of 30% were placed in a beaker and stirred evenly, and then the gel was added to a polytetrafluoroethylene stainless steel reaction kettle, crystallized at 140 ° C for 3 days, and then completely crystallized, and the product was suction filtered. The product is obtained after drying. The proportioning of reaction raw material is as follows:

[0023] 22H 2 O:SiO 2 :0.18Na 2 O:0.18T

[0024] Through X-ray diffraction analysis, its structure is ZSM-5 zeolite molecular sieve belonging to MFI ( figure 2 ), and it can be seen from the scanning electron microscope that the synthesized product presents a sheet-like appearance (low magnification), and the sheet-like appearance of the product is intersecting with each other,...

Embodiment 2

[0025] Example 2: Synthesis of aluminum-rich ZSM-5 zeolite with a new and cheap single small molecule organic template

[0026] 5g H 2 O, 0.32g Al 2 (SO 4 ) 3 18H 2 O, 0.77g NaOH, 2.8g organic template (T, structure such as figure 1 ) and 3.9g of silica sol with a silicon dioxide content of 30% were placed in a beaker and stirred evenly, and then the gel was added into a polytetrafluoroethylene stainless steel reaction kettle, crystallized at 100°C for 10 days, and then completely crystallized, and the product was suction filtered. The product is obtained after drying. The proportioning of reaction raw material is as follows:

[0027] 22H 2 O:SiO 2 :0.025Al 2 o 3 :0.5Na 2 O:0.5T

Embodiment 3

[0028] Example 3: Synthesis of high-silicon ZSM-5 zeolite with a new and cheap single small molecule organic template

[0029] 5g H 2 O, 0.023g NaAlO 2 , 0.32g NaOH, 1.0g organic template (T, structure such as figure 1 ) and 3.9g of silica sol with a silicon dioxide content of 30% were placed in a beaker and stirred evenly, and then the gel was added into a polytetrafluoroethylene stainless steel reaction kettle, crystallized at 100°C for 10 days, and then completely crystallized, and the product was suction filtered. The product is obtained after drying. The proportioning of reaction raw material is as follows:

[0030] 22H 2 O:SiO 2 :0.005Al 2 o 3 :0.21Na 2 O:0.18T

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Abstract

The invention relates to a morphological control preparation method for a molecular sieve, and aims to provide a method for synthesizing a laminar ZSM-5 zeolite molecular sieve with a single micro-molecule organic template. The method comprises the following steps: mixing water, a silicon source, an alkali source and a template, or adding an aluminum source and then continuously mixing to be uniform; then, performing crystallization reaction in a reaction kettle to obtain a product, and performing suction filtration and drying on the product to obtain raw powder of the ZSM-5 zeolite molecular sieve. According to the method, a high-cost organic template is eliminated, and the synthesis cost is greatly reduced; the synthesized product has a special laminar morphology, the thickness is 20-30nm, and cross growth between sheets is realized. The product not only maintains good crystallinity and purity, but also has good catalytic reaction activity. Inorganic raw materials and the organic template adopted in the whole production process are environmentally friendly, and low in cost, and therefore the method plays an important role in the field of actual chemical industry production.

Description

technical field [0001] The invention belongs to a method for preparing molecular sieve morphology control, in particular to a method for synthesizing thin-sheet ZSM-5 zeolite molecular sieves with a novel low-cost single small molecule organic template. Background technique [0002] ZSM-5 zeolite is a high-silica zeolite with a three-dimensional ten-membered ring pore structure widely used in industry at the present stage. It has a wide range of applications in catalytic processes such as alkylation reaction, heavy oil cracking dewaxing, and methanol conversion to gasoline. Therefore, it is of great significance to study the synthesis of ZSM-5 zeolite. In the synthesis process, the regulation of its morphology and pore structure can improve its catalytic performance. Therefore, researchers have done a lot of research work in this area. In 2000, Jacobsen et al. synthesized mesoporous ZSM-5 zeolite for the first time by hard template method; in 2006, Xiao et al. synthesized Z...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/40
CPCC01B39/40C01P2002/72C01P2004/03C01P2004/20
Inventor 吴勤明孟祥举肖丰收
Owner ZHEJIANG UNIV