Preparation method and application of hierarchical pore SSZ-13 molecular sieve and method for preparing olefin from methanol

A technology of methanol to olefins and molecular sieves, which is applied in the direction of molecular sieve catalysts, including molecular sieve catalysts, molecular sieves and base exchange compounds, etc. It can solve the difficult control of molecular sieve desilication and dealumination processes, high synthesis cost of hierarchical porous materials, and expensive templates problems such as solvents, to achieve the effects of easy industrial application, high selectivity, and reduced over-etching

Active Publication Date: 2021-06-18
PETROCHINA CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

According to the existing research results, the soft template method and the hard template method require expensive template agents, and it is difficult to realize their industrial production.
The post-treatment method is simple to operate and easy to apply industrially, but the process of desilication and dealumination of molecular sieves is difficult to control, and some post-treatment methods have not yet got rid of the dependence on organic templates, which makes the synthesis cost of hierarchical porous materials higher.

Method used

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  • Preparation method and application of hierarchical pore SSZ-13 molecular sieve and method for preparing olefin from methanol
  • Preparation method and application of hierarchical pore SSZ-13 molecular sieve and method for preparing olefin from methanol
  • Preparation method and application of hierarchical pore SSZ-13 molecular sieve and method for preparing olefin from methanol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Weigh 8.4g to remove the hydrogen-type microporous SSZ-13 molecular sieve of the organic template (SiO in the molecular sieve gel 2 / Al 2 o 3 molar ratio 80) was added to 336ml of copper nitrate solution with a concentration of 0.1mol / L, and stirred in a water bath at 70°C for 2h to obtain Cu 2+ protected by SSZ-13 molecular sieves. The molecular sieve solid product after framework protection was centrifuged and added to 336ml of 0.2mol / L sodium hydroxide aqueous solution, and stirred in a water bath at 70°C for 2h. After alkali treatment, the solid product was centrifuged and added to 168 ml of aqueous hydrogen chloride solution with a hydrogen ion concentration of 0.3 mol / L, and stirred at room temperature for 2 hours. After the acid treatment, the solid product was centrifuged and washed, then added to 336ml of ammonium chloride solution with a concentration of 1mol / L, and exchanged ammonium ions in a water bath at 70°C for 2 hours, and exchanged 3 times. The sol...

Embodiment 2

[0050] Weigh 7.2g to remove the hydrogen-type microporous SSZ-13 molecular sieve of the organic template (SiO in the molecular sieve gel 2 / Al 2 o 3 molar ratio 80) was added to 288ml of zinc nitrate solution with a concentration of 0.1ml / L, and stirred in a water bath at 70°C for 2h to obtain Zn 2+ protected by SSZ-13 molecular sieves. The molecular sieve solid product after framework protection was centrifuged and added to 288ml of 0.2mol / L sodium hydroxide aqueous solution, and stirred in a water bath at 70°C for 2h. After alkali treatment, the solid product was centrifuged and added to 144 ml of aqueous hydrogen chloride solution with a hydrogen ion concentration of 0.3 mol / L, and stirred at room temperature for 2 hours. After the acid treatment, the solid product was centrifuged and washed, then added to 288ml of ammonium chloride solution with a concentration of 1mol / L, and exchanged ammonium ions in a water bath at 70°C for 2 hours, and exchanged 3 times. The solid ...

Embodiment 3

[0053] Evaluation of Catalytic Performance of Sample Molecular Sieve MTO Reaction Application.

[0054] The MTO reaction performance of the microporous SSZ-13 molecular sieve (SZ-0) before treatment, the molecular sieve catalyst obtained in Comparative Example 1 and Examples 1 and 2 was investigated by using a fixed bed micro-reactor device. The evaluation method is as follows: use a mold to press the hydrogen-type molecular sieve sample into tablets, crush it and pass it through a 60-80 mesh sieve, collect 1 g of the sieved molecular sieve sample and put it into a fixed-bed reactor, and fill the upper and lower ends of the molecular sieve with quartz sand. Before the reaction, the catalyst needs to be pretreated, and the flow rate is 60ml / min nitrogen carrier gas, the reactor is raised from normal temperature to 500°C for 1h and kept for 0.5h, then lowered to the reaction temperature of 350°C, and the reaction material methanol is introduced , its mass concentration is 60%, a...

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Abstract

The invention provides a preparation method of a hierarchical porous SSZ-13 molecular sieve. The method comprises the following steps: mixing a microporous SSZ-13 molecular sieve, a molecular sieve skeleton protective agent and water to obtain a skeleton-protected SSZ-13 molecular sieve; sequentially carrying out alkali treatment, acid treatment, ammonium ion exchange and roasting treatment on the skeleton-protected SSZ-13 molecular sieve, so as to obtain the hydrogen type hierarchical pore SSZ-13 molecular sieve. Compared with the conventional preparation method of the hierarchical porous SSZ-13 molecular sieve, the preparation method has the advantages of simplicity in operation, low cost and no need of an organic template agent. The obtained hierarchical pore SSZ-13 molecular sieve shows more excellent performance in the methanol-to-olefin process, the selectivity of ethylene and propylene is high, and the reaction life is long.

Description

technical field [0001] The present invention relates to a molecular sieve preparation method and its application, in particular to a preparation method and application of a hierarchically porous SSZ-13 molecular sieve, and a methanol-to-olefin method using the hierarchically porous SSZ-13 molecular sieve as a catalyst. Background technique [0002] SSZ-13 molecular sieve is made of AlO 4 and SiO 4 Tetrahedral microporous zeolite molecular sieve with chabazite (CHA) structure. The molecular sieve contains an ellipsoidal cage with an eight-membered ring structure and three-dimensional intersecting channel structure (channel size ), its special ordered framework makes it have good thermal stability and suitable acidity. In recent years, SSZ-13 molecular sieve has been widely concerned and reported as a new type of efficient adsorption, separation and catalytic materials. The limited pore size of SSZ-13 molecular sieve endows it with excellent shape-selective catalytic pe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/02C01B39/46B01J29/70B01J29/72C07C1/20C07C11/04C07C11/06
CPCC01B39/026C01B39/46B01J29/7065B01J29/723C07C1/20C07C2529/70C07C2529/72C01P2002/72C01P2004/03C07C11/04C07C11/06Y02P20/52Y02P30/20Y02P30/40
Inventor 代跃利朱小春汲永刚刘剑孙恩浩万书宝孙淑坤杜海褚洪岭徐显明张永军于静邴淑秋
Owner PETROCHINA CO LTD
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