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Synthetic method of nano SAPO-34 molecular sieve

A technology of SAPO-34, synthesis method, applied in molecular sieve and alkali-exchanged phosphate, molecular sieve characteristic silicoaluminophosphate, nanotechnology, etc., can solve the problems of difficult collection of products, excessive amount of template agent, etc., and achieve high crystallinity Effect

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

[0015] 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-SAPO-34 molecular sieve, which can effectively reduce the amount of organic template agent. The method of collecting products greatly reduces the synthesis cost of nano-molecular sieves

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0048] Preparation of macroporous carbon materials:

[0049] (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;

[0050] (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.

[0051] (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;

[0052] (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

[0055] (1) Dissolve 4.5mL of phosphoric acid in 50mL of distilled water, then add 7.5g of aluminum isopropoxide, after the dissolution is complete, add 5mL of ethyl orthosilicate, then add 3mL of diethylamine, and stir vigorously for 30 minutes.

[0056] (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 60°C until it becomes viscous; then dry it at 110°C until the water evaporates completely.

[0057] (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 200° 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-SAPO-34 molecular sieve,...

Embodiment 3

[0059] (1) Dissolve 4 mL of phosphoric acid in 50 mL of distilled water, then add 7 g of aluminum isopropoxide, after the dissolution is complete, add 4.5 mL of ethyl orthosilicate, then add 3.5 mL of diethylamine, and stir vigorously for 30 min.

[0060] (2) Mix the synthetic gel obtained in step (1) with 11 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.

[0061] (3) Then put the mixture obtained in step (2) into the reactor, and then add 13 mL of water. Then the reactor was sealed, and the reactor was placed in an oven for crystallization at 190° C. for 45 h. Then filter and wash the solid product to neutrality, dry at 100°C for 10 hours, and finally roast at 500°C for 3 hours in an air atmosphere. The obtained sample number is CL2, which is a pure nano-SAPO-34 molecular sieve without other impurities. The sample is speci...

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Abstract

The invention discloses a synthetic method of a nano SAPO-34 molecular sieve. The synthetic method comprises the steps as follows: firstly, mixing phosphoric acid, water, a template, an aluminum source and a silicon source to obtain gel, mixing the gel with macroporous carbon, conducting ultrasonic treatment, then, conducting stirring treatment at the temperature of 50-100 DEG C until the stirred material is in a viscous state, drying the viscous material until moisture is completely evaporated, placing the dried material in a reactor, adding a certain amount of water, sealing the reactor, carrying out a crystallization reaction, filtering the obtained solid product, conducting washing and drying, and conducting roasting in an oxygen or air atmosphere to obtain the nano SAPO-34 molecular sieve. With the adoption of the synthetic method, the nano SAPO-34 molecular sieve can be synthesized under the condition of low organic template dosage, the crystallinity is high, and other crystal impurities are not contained.

Description

technical field [0001] The invention relates to a method for synthesizing nanometer SAPO-34 molecular sieves, in particular to a method for synthesizing nanoscale SAPO-34 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 cryst...

Claims

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Application Information

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IPC IPC(8): C01B39/54C01B37/08B82Y40/00
Inventor 范峰凌凤香王少军张会成杨春雁
Owner CHINA PETROLEUM & CHEM CORP
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