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Method for preparing nano molecular sieve microspherical catalyst

A nano-molecular sieve and catalyst technology, which is applied in the direction of molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the adverse catalytic performance of SAPO-34 molecular sieve, the influence of SAPO-34 molecular sieve utilization rate, and the performance of SAPO-34 molecular sieve Differences and other issues can be achieved to solve the size control problem, reduce the risk of damage, and improve the uniformity of growth

Active Publication Date: 2013-03-13
SHANGHAI LVQIANG NEW MATERIALS CO LTD +1
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Problems solved by technology

[0005] Chinese patent CN1557555A discloses a method for preparing a homogeneous nano-molecular sieve material with high catalytic activity. The patent uses 100-300 nanometer uniform polymer beads in the water phase to form a nano-molecular sieve confined reactor after stirring for a certain period of time. Nano-molecular sieves were synthesized. The molecular sieves prepared by this method are limited to the raw powder of molecular sieves and cannot be directly applied to industrial production.
[0010] There are many patents related to SAPO-34 molecular sieve molding technology, but less about nanometer SAPO-34 molecular sieve molding technology. For example, Chinese patent CN101284246B discloses a catalyst for converting oxygen-containing compounds into low-carbon olefins. The patent points out that in the catalyst The crystal size of 90% of the contained SAPO-34 molecular sieves is less than 0.5 microns, and the grain size of the SAPO-34 molecular sieves is still far behind that of nano-molecular sieves in the strict sense. At the same time, the molding technology adopted is traditional Hybrid bonding molding technology, due to the limitations of this method, the utilization rate of SAPO-34 molecular sieve is also affected to a certain extent, which is not conducive to fully exerting the catalytic performance of SAPO-34 molecular sieve
[0011] Chinese patent CN102219237A discloses a method for preparing a SAPO molecular sieve material with a hierarchical pore structure. The actually obtained monolithic SAPO molecular sieve material with a hierarchical pore structure cannot be directly applied to a fluidized bed process due to its shape and strength.
The reason is that during hydrothermal crystallization, the solid phase carrier in the crystallization mother liquor has uneven mass transfer due to natural settlement, because of the concentration gradient and the liquid-solid separation problem in the reaction process.
It will inevitably lead to performance differences in the synthesized SAPO-34 molecular sieve, and the prepared catalyst cannot achieve the best catalytic performance

Method used

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  • Method for preparing nano molecular sieve microspherical catalyst
  • Method for preparing nano molecular sieve microspherical catalyst
  • Method for preparing nano molecular sieve microspherical catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Nano molecular sieve preparation

[0041] 7.8g pseudo-boehmite (content 65%) was mixed with 110g tetraethylammonium hydroxide and stirred for 30 minutes, after stirring evenly, 3.6g silica sol (content 25%) was added thereto, then slowly added 11.5g phosphoric acid (content 85%), stirred at room temperature for 12 hours, under dynamic conditions, nucleated at 100-160°C for 2-4h, cooled naturally, added 260g deionized water, crystallized by microwave at 150-180°C for 40-80min, and the product was washed , dried at 110°C for 12 hours, and roasted at 600°C for 4 hours. XRD test showed that the molecular sieve was SAPO-34 molecular sieve ( figure 1 ), SEM test shows that gained molecular sieve is nano molecular sieve ( figure 2 ).

Embodiment 2

[0043] In situ synthesis of nanomolecular sieves

[0044] (1) Preparation of kaolin microspheres

[0045] First kaolin 3000g, silica sol 1000g (solid content 25%) and certain P 2 o 5 / Al 2 o 3 200g of phosphorus-aluminum sol in molar ratio and 1560g of deionized water were mixed to form a uniform slurry, and then 30g of polyethylene glycol was added through a rubber mill for rubber grinding, so that the particle size was less than 3 μm, and 90% of the particle size was less than 2 μm. 70% of the particle size is less than 1 μm; then the mixed slurry is spray-dried to obtain kaolin microspheres, the particle size is between 20-150 μm, the average particle size is 60 μm, and roasted at 950 ° C for 1-4 hours to obtain kaolin microspheres .

[0046] (2) Preparation of nano-molecular sieve microsphere catalyst

[0047] 7.8g pseudo-boehmite (content 65%) was mixed with 110g tetraethylammonium hydroxide and stirred for 30 minutes, after stirring evenly, 3.6g silica sol (content...

Embodiment 3

[0049] In situ synthesis of nanomolecular sieves

[0050] (1) Preparation of montmorillonite microspheres

[0051] First, the montmorillonite is rubber-milled by a rubber mill so that the particle size is less than 2 μm, wherein 90% of the particle size is less than 2 μm, and 70% of the particle size is less than 1 μm; then get 3000 g of gained kaolin and 1200 g of aluminum sol Content 25%) and deionized water 1560g are mixed into a uniform slurry, and the kaolin microspheres are prepared by spray drying method, the particle size is between 20-150 μm, the average particle size is 80 μm, and roasted at 1000 ° C for 1-4h to obtain Monto soil microspheres.

[0052] (2) Preparation of nano-molecular sieve microsphere catalyst

[0053] 7.8g pseudo-boehmite (content 65%) was mixed with 110g tetraethylammonium hydroxide and stirred for 30 minutes, after stirring evenly, 3.6g silica sol (content 25%) was added thereto, then slowly added 11.5g phosphoric acid (content 85%), after st...

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Abstract

The invention relates to a method for preparing a nano molecular sieve microspherical catalyst. The method comprises the following steps of: mixing pseudo-boehmite, silica solution, phosphoric acid and a template agent in a rotary reaction tank, rotating the rotary reaction tank around a horizontal central shaft, heating and nucleating at the temperature of 100 to 160 DEG C for 2 to 4 hours, adding an abrasion-resistant carrier and water, heating by microwave at the temperature of 150 to 180 DEG C, crystallizing for 40 to 80 minutes, and obtaining the nano molecular sieve microspherical catalyst. Compared with the prior art, the method has the advantages that the process is simple and is suitable for production. The prepared nano molecular sieve microspherical catalyst is high in uniformity and has the characteristics of high specific area and high catalyst activity. The nano molecular sieve microspherical catalyst is applied to reaction of methyl alcohol and dimethyl ether in preparing low-carbon olefin, has the characteristic of low abrasion consumption and is favorable for industrial production.

Description

technical field [0001] The invention relates to a molecular sieve catalyst, in particular to a preparation method of a nano molecular sieve microsphere catalyst. Background technique [0002] Nano-molecular sieves refer to molecular sieves with a particle size between 1-100nm. The ratio of the number of surface atoms to the number of bulk phase atoms increases sharply as the particle size decreases, making nano-molecular sieves a new material with unique catalytic properties. The characteristics of nano-molecular sieves are specifically manifested in: it has a larger outer surface, which exposes more active centers, effectively eliminates the diffusion effect, and enables the catalyst efficiency to be fully exerted; it has more pores exposed to the outside, and is not easy to be reacted Sediment clogging is beneficial to prolong the reaction operation cycle. [0003] The advantages of nano-SAPO-34 molecular sieve are obvious, such as (1) improved diffusion limitation, which...

Claims

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Application Information

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IPC IPC(8): B01J29/85B01J35/08C01B39/54C07C1/20C07C11/02
Inventor 徐华胜胡杰王鹏飞
Owner SHANGHAI LVQIANG NEW MATERIALS CO LTD
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