Nanometer EU-1 molecular sieve synthesizing method

An EU-1, synthesis method technology, applied in molecular sieve catalyst, nanotechnology, nanotechnology and other directions, can solve the problems of difficult collection of products, excessive amount of template agent, etc., and achieve the effect of high crystallinity

Active Publication Date: 2017-05-24
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0012] 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 synthesis method of nano-EU-1 molecular sieve, which can effectively reduce the amount of organic template agent. The product is collected by the method, which greatly reduces the synthesis cost of nano molecular sieves

Method used

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  • Nanometer EU-1 molecular sieve synthesizing method
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  • Nanometer EU-1 molecular sieve synthesizing method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Preparation of macroporous carbon materials:

[0046] (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;

[0047] (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.

[0048] (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;

[0049] (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

[0052] (1) Dissolve 0.85 g of sodium hydroxide in 30 mL of distilled water and stir for 30 min. Then add 0.6 g of sodium aluminate and stir for 30 min. Then add 2g of hexamethyldiammonium bromide and stir for 30 min. Add 6.5 g of white carbon black slowly and stir for 30 min.

[0053] (2) Mix the synthetic gel obtained in step (1) with 7.5 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; Dry until the water evaporates completely.

[0054] (3) Then put the mixture obtained in step (2) into the reactor, and then add 7 mL of water. Then the reactor was sealed, and the reactor was placed in an oven for crystallization at 190° C. for 60 h. Then the solid product was filtered and washed to neutrality, dried at 100°C for 10 hours, and finally calcined at 500°C for 3 hours in an air atmosphere. The obtained sample number was CL1. figure 1 and figure 2 As shown, it is a pure nano EU-1 mo...

Embodiment 3

[0056] (1) Dissolve 0.65 g of sodium hydroxide in 30 mL of distilled water and stir for 30 min. Then add 0.3 g of sodium aluminate and stir for 30 min. Then add 1.5g of hexamethyldiammonium bromide and stir for 30 min. Add 6.5 g of white carbon black slowly and stir for 30 min.

[0057] (2) Mix the synthetic gel obtained in step (1) with 10 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.

[0058] (3) Then put the mixture obtained in step (2) into the reactor, and then add 10 mL of water. Then the reactor was sealed, and the reactor was placed in an oven for crystallization at 210° C. for 55 h. Then filter and wash the solid product to neutrality, dry at 100°C for 10h, and finally roast at 500°C for 3h in the air atmosphere. The obtained sample number is CL2, which is a pure nano-EU-1 molecular sieve without other impuriti...

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Abstract

The invention discloses a nanometer EU-1 molecular sieve synthesizing method. The synthesizing method comprises the following steps: firstly, mixing inorganic base, water, a template agent, an aluminum source and a silicon source to obtain gel; mixing the gel with macroporous carbon and performing ultrasonic treatment; then stirring and treating under the condition of 50 to 100 DEG C until a thick state is formed; then drying until moisture is completely evaporated; then filling a reactor, adding a quantitative amount of water to seal the reactor for performing crystallization; filtering, washing and drying an obtained solid product and roasting the obtained solid product in an oxygen or air atmosphere to obtain the nanometer EU-1 molecular sieve. The synthesizing method disclosed by the invention can be used to synthesize the nanometer EU-1 molecular sieve under the situation of a low organic template agent using amount, crystalline degree is high, and other crystal impurities are avoided.

Description

technical field [0001] The invention relates to a method for synthesizing nanometer EU-1 molecular sieves, in particular to a method for synthesizing nanoscale EU-1 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): C01B39/04B82Y30/00B01J29/00
Inventor 范峰凌凤香王少军张会成杨春雁
Owner CHINA PETROLEUM & CHEM CORP
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