Method for synthesizing nano-Beta molecular sieve

A molecular sieve and nanotechnology, applied in nanotechnology, nanotechnology, nanotechnology for materials and surface science, etc., can solve the problems of excessive amount of template agent and difficult collection of products, and achieve strong guiding effect and high crystallinity. Effect

Active Publication Date: 2017-05-24
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
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Problems solved by technology

[0013] Aiming at the deficiencies of the existing nano-molecular sieve technology, especially the problem that the amount of template agent is too much and the product is difficult to collect, the present invention provides a method for synthesizing nano-Beta molecular sieve, which can synthesize molecular sieve without organic template agent, and collect the product by traditional filtration method. Greatly reduce the synthesis cost of nano molecular sieves

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  • Method for synthesizing nano-Beta molecular sieve
  • Method for synthesizing nano-Beta molecular sieve
  • Method for synthesizing nano-Beta molecular sieve

Examples

Experimental program
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Effect test

Embodiment 1

[0050] Preparation of macroporous carbon materials:

[0051] (a) Mix 150g of calcium carbonate with 5000mL of 0.05mol / L sodium hydroxide solution, stir at 70°C for 2h; then filter, and dry the obtained solid sample at 500°C for 2.5h;

[0052] (b) Add 7000 mL of distilled water and 300 g of sucrose to the calcium carbonate obtained in step (a), stir for 30 min and then ultrasonicate for 5 h.

[0053] (c) The solution prepared in step (b) was placed in a 70°C water bath and stirred to make the water evaporate until the solution became viscous; then dried at 70°C; finally, the sample was placed in a tube furnace and passed through Inject nitrogen gas at a flow rate of 20mL / min; raise the temperature from room temperature to 900°C at 11°C / min, and keep the temperature constant for 5h;

[0054] (d) Mix the substance obtained in step (c) with 5000mL of 50% hydrochloric acid solution evenly, treat at 140°C for 6h, finally wash with water until neutral, and dry at 100°C for 10h,

[...

Embodiment 2

[0057] (1) Take 4g of Beta molecular sieve and 100mL of 1mol / L NaOH solution in a beaker, stir at room temperature for 30min, transfer to a closed reaction kettle, and treat in an oven at 120°C for 4h. The resulting suspension is the structure-directing agent and is ready for use.

[0058] (2) Take 2.5 g of sodium hydroxide and 0.5 g of sodium aluminate in 50 mL of distilled water and stir vigorously until they are completely dissolved. Add 7 g of white carbon black slowly and stir vigorously for 30 min. Then add 2.5mL of the structure directing agent prepared in the previous step and stir vigorously for 30 min.

[0059] (3) Mix the synthetic gel obtained in step (2) with 8 g of the macroporous carbon prepared in Example 1, and ultrasonically treat it for 30 minutes; then stir it at 60°C until it becomes viscous; then dry it at 110°C until the water evaporates completely.

[0060] (4) Then put the mixture obtained in step (3) into the reactor, and then add 5 mL of water. T...

Embodiment 3

[0062](1) Take 4g of Beta molecular sieve and 80mL of 1mol / L NaOH solution in a beaker, stir at room temperature for 30min, transfer to a closed reaction kettle, and treat in an oven at 125°C for 4h. The resulting suspension is the structure-directing agent and is ready for use.

[0063] (2) Put 2 g of sodium hydroxide and 0.6 g of sodium aluminate in 50 mL of distilled water and stir vigorously until they are completely dissolved. Add 5.7 g of white carbon black slowly and stir vigorously for 30 min. Then add 2.5mL of the structure directing agent prepared in the previous step and stir vigorously for 30 min.

[0064] (3) Mix the synthetic gel obtained in step (2) with 8 g of the macroporous carbon prepared in Example 1, and ultrasonically treat it for 30 minutes; then stir it at 70°C until it becomes viscous; then dry it at 120°C until the water evaporates completely.

[0065] (4) Then put the mixture obtained in step (3) into the reactor, and then add 20 mL of water. The...

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Abstract

The invention discloses a method for synthesizing a nano-Beta molecular sieve. The method comprises the following steps: firstly, preparing a structure-directing agent; then mixing inorganic base, water, an aluminum source and a silicon source to obtain a gel; mixing the gel with macroporous carbon and then carrying out ultrasonic treatment; stirring at a temperature of 50-100 DEG C to be in a viscous state; drying until the water is completely evaporated; charging into a reactor and adding to a quantitative water-tight reactor for crystallization; filtering, washing and drying an obtained solid product, and then calcinating in oxygen or air atmosphere to obtain the nano-Beta molecular sieve. The method provided by the invention can synthesize the nano-Beta molecular sieve without template agent, so that the nano-Beta molecular sieve not only has high crystallinity, but also does not contain other crystal impurities.

Description

technical field [0001] The invention relates to a method for synthesizing nanometer Beta molecular sieves, in particular to a method for synthesizing nanoscale Beta molecular sieves with high efficiency and low cost, and belongs to the field of synthesis of molecular sieve catalytic materials. Background technique [0002] Zeolite molecular sieves are widely used as catalysts, adsorbents, ion exchangers and new functional Material. At present, the grain size of molecular sieves used in industry is generally in the micron order. With the upgrading of oil quality and the increasingly inferior quality of crude oil, the shortcomings of micron molecular sieves are also gradually enlarged, such as excessive internal diffusion resistance of substances and insufficient catalytic activity. Small grains, especially nano molecular sieves can just solve these problems. Generally, the crystal size of nano molecular sieves is limited within 100nm. Due to the extremely small crystal gra...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/02B82Y30/00
Inventor 范峰凌凤香王少军张会成杨春雁
Owner CHINA PETROLEUM & CHEM CORP
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