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Method for preparing zeolite molecular sieve catalyst through circulating gas phase method

A zeolite molecular sieve and circulating gas technology, applied in molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problem of difficulty in regulating the relative humidity of water vapor, unfavorable industrialization, silica-alumina dry glue and template agent or water vapor problems such as poor mass transfer effect, to achieve the effect of shortening synthesis time, conducive to industrial production, reducing environmental pollution and production costs

Active Publication Date: 2012-09-19
BEIJING UNIV OF CHEM TECH
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

Compared with the traditional hydrothermal method, the method uses a gas-phase synthesis kettle. Compared with the traditional hydrothermal method, the amount of organic template agent is reduced, the post-treatment process is simple, and the discharge of amine-containing organic matter is reduced at the same time, and the environmental pollution in the production process is reduced; The mass transfer effect of aluminum dry glue and template agent or water vapor is poor, and the operation is batch operation, which is not conducive to industrialization
[0005] Naik et al. used a new type of gas-phase reactor to synthesize zeolite molecular sieves (The Journal of Physical Chemistry B.2003, 107, 29: 7006-7014.), which can control the relative water vapor in the gas-phase synthesis of zeolite molecular sieves. Humidity, to overcome the shortcomings of traditional gas-phase synthesis kettles that are difficult to control the relative humidity of water vapor, and to explore a new route to synthesize zeolite molecular sieves at a specific relative humidity of water vapor

Method used

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  • Method for preparing zeolite molecular sieve catalyst through circulating gas phase method
  • Method for preparing zeolite molecular sieve catalyst through circulating gas phase method
  • Method for preparing zeolite molecular sieve catalyst through circulating gas phase method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] Fully mix 50 grams of silica gel, 3.7 grams of SB powder and 4.3 grams of sodium hydroxide, and the material ratio (molar ratio) of the reactants is: SiO 2 :Al 2 o 3 :OH - =30:1:3.9, after fully mixing, add 5 grams of nitric acid, 3.3 grams of pore-enlarging agent PEG-20000 and 70 grams of deionized water to the mixture to obtain silica-alumina dry glue, and then extrude the silica-alumina dry glue into strips, Dry at 60°C to obtain cylindrical particles. Take 12 grams of formed cylindrical particles, put them into the partition plate in the autoclave in 3 layers, the height of each layer is about 0.03 meters, there are 40 grams of HMI and 160 grams of deionized water in the liquid storage tank, and the preheating temperature is 80 ℃, the temperature of the high-pressure reactor is 150 ℃, the pressure is 0.36MPa, and the organic template agent steam and water vapor are circulated by a double plunger pump, and the space velocity is 0.5h -1 , in situ crystallization f...

Embodiment 2

[0052] Get 12 grams of formed cylindrical granules in Example 1, put them on the dividing plate in the autoclave in 3 layers, each layer has a height of about 0.03 meters, and the residual liquid in Example 1 is in the liquid storage tank, preheating The temperature is 80°C, the temperature of the autoclave is 150°C, and the pressure is 0.36MPa. The steam of the organic template agent and the water vapor are circulated by a double plunger pump, and the space velocity is 0.5h -1 , in situ crystallization for 6 days. Take it out, wash it, filter it, dry it at 90°C, exchange it with ammonium, and roast it at 540°C for 6 hours to get the product. The obtained zeolite molecular sieve catalyst was determined by XRD to be an MCM-22 zeolite molecular sieve catalyst with a crystallinity of 94.6% (compared with the crystallinity in Example 1).

Embodiment 3

[0054] 50 grams of white carbon black, 18.3 grams of aluminum sulfate, 3.3 grams of sodium hydroxide and 152 grams of mass fraction 35% tetraethylammonium hydroxide are fully mixed, and the material ratio (molar ratio) of the reactant is: SiO 2 :Al 2 o 3 :OH - :TEAOH=30:1:3:13, evaporate water at 60°C to obtain silica-alumina dry glue. Take 12 grams of powdery silica-alumina dry glue, put it into the partition plate in the high-pressure reactor in 3 layers, the height of each layer is about 0.03 meters, there is 120 grams of deionized water in the liquid storage tank, and the preheating temperature is 80 ° C. The temperature of the high-pressure reactor is 140°C, the pressure is 0.26MPa (at this time, the water vapor is in a saturated state), and the double plunger pump is used to circulate the water vapor, and the space velocity is 0.5h -1 , in situ crystallization for 24h. Take it out, wash it, filter it, dry it at 90°C, exchange it with ammonium, and roast it at 540°C f...

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Abstract

The invention relates to a method for preparing a zeolite molecular sieve catalyst through a circulating gas phase method. The method belongs to the field of catalysts. Water vapor or an organic template agent and water mixed steam are in the continuous circulating state to enable silicon-aluminum dry glue to be completely contacted with the water vapor or the organic template agent and the watermixed steam to improve mass transfer effect between the silicon-aluminum dry glue and the water vapor or the organic template agent and the water mixed steam, increase mass transfer rate and shorten combining time. A high pressure reaction kettle adopts a multi-layer structure and greatly improves single-kettle yield. Pressure of the high pressure reaction kettle can be regulated according to reaction conditions to enable the water vapor or the organic template agent and the water mixed steam to be in saturation, supercooling or superheat states and enable the organic template agent to be recycled repeatedly most importantly. The method reduces discharge of organics containing amine, further reduces consumption of raw materials especially the organic template agent, reduces environment pollution and production cost in the production process, enables the production process to be continuous, and facilitates industrial production.

Description

technical field [0001] The invention relates to a method for preparing a zeolite molecular sieve catalyst by a circulating gas phase method, that is, a method for preparing a zeolite molecular sieve catalyst in continuously circulating steam. Specifically, it refers to the in-situ preparation of zeolite molecular sieve catalysts such as Beta and MCM-22 in continuously circulating water vapor or mixed steam of an organic template agent and water. Background technique [0002] Zeolite molecular sieve has a unique regular crystal structure, and microporous molecular sieve has strong acid center and regular pore structure. These characteristics make it a catalyst with excellent performance. It is widely used in petroleum refining, petrochemical, fine chemical industry and special chemical industry. Synthesis of products and other fields. [0003] The main method for the synthesis of industrial zeolite molecular sieves is the hydrothermal method. The hydrothermal method is curre...

Claims

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Application Information

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IPC IPC(8): C01B39/04B01J29/06
Inventor 李英霞王煊陈标华
Owner BEIJING UNIV OF CHEM TECH
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