Fluorine-containing high-silicon Y molecular sieve and preparation method thereof

A molecular sieve and high silicon technology, applied in molecular sieve catalysts, molecular sieves and alkali exchange compounds, chemical instruments and methods, etc., can solve the problems of expensive crown ethers, high toxicity, and limited industrial applications.

Active Publication Date: 2020-10-27
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In 1990, French Delprato et al. (Zeolites, 1990,10(6):546-552) synthesized FAU molecular sieves with a cubic structure for the first time using crown ethers as templates. The highest value that can be achieved by the method, but the expensive and highly toxic crown ether limits its industrial application

Method used

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  • Fluorine-containing high-silicon Y molecular sieve and preparation method thereof
  • Fluorine-containing high-silicon Y molecular sieve and preparation method thereof
  • Fluorine-containing high-silicon Y molecular sieve and preparation method thereof

Examples

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Effect test

Embodiment 1

[0128] The preparation of embodiment 1 sample S1

[0129]Preparation of guiding agent A: 0.23g sodium hydroxide (analytically pure, Tianjin Kemiou Chemical Reagent Co., Ltd.), 0.35g sodium aluminate (chemically pure, China Pharmaceutical (Group) Shanghai Chemical Reagent Company) were dissolved in 19.06g IV Methylammonium hydroxide (25% aqueous solution, Aladdin Reagent (Shanghai) Co., Ltd.) was stirred until clarification, and then 14.00 g of ethyl orthosilicate (chemically pure, China Pharmaceutical (Group) Shanghai Chemical Reagent Company) was added dropwise and cooled at room temperature. Stir for 2h. The above solution was left to stand at 25°C for 12h and then transferred to 80°C for 48h of rotational aging.

[0130] Prepare synthetic gel C: join 0.13g sodium aluminate, 0.07g sodium hydroxide in 10.84g tetrapropyl ammonium hydroxide (25wt%) solution and stir until clear, and dropwise add 13.33g silica sol (SiO 2 : 30wt%, Shenyang Chemical Co., Ltd.) stirred for 0.5h, ...

Embodiment 2

[0134] The preparation of embodiment 2 sample S2

[0135] Preparation of directing agent A: Dissolve 1.03g of alumina (China Pharmaceutical (Group) Shanghai Chemical Reagent Company, 65wt%) in 19.24g of tetraethylammonium hydroxide (25% aqueous solution, Aladdin Reagent (Shanghai) Co., Ltd.) and stir Until clarification, 14.00 g of ethyl orthosilicate (chemically pure, China Pharmaceutical (Group) Shanghai Chemical Reagent Company) was added dropwise and stirred at room temperature for 2 h. The above solution was rotatably aged at 75°C for 36h.

[0136] Preparation of synthetic gel C: 0.08g of sodium aluminate (Al 2 o 3 : 51wt%, Na 2 (2:41wt%, Tianjin Guangfu Chemical Co., Ltd.) was added to 4.71g tetraethylammonium hydroxide (25wt%) solution and stirred until clarification, and 13.33g silica sol (SiO 2 : 30wt%, Shenyang Chemical Co., Ltd.) stirred for 0.5h, then added 0.80g hydrofluoric acid (40wt%), then added 2.46g of the above-mentioned directing agent and stirred for ...

Embodiment 3

[0140] The preparation of embodiment 3 sample S3-S30

[0141] See Table 1 for the raw material types, molar ratio, crystallization conditions, water-to-silicon ratio, and product crystal structure and composition of samples S3-S30. See Table 2 for the aging temperature, time, aging method and amount of the directing agent. The batching process Same as the preparation of sample S1 in Example 1.

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Abstract

The invention discloses a fluorine-containing high-silicon Y molecular sieve and a preparation method thereof, and belongs to the field of molecular sieve synthesis. The anhydrous chemical compositionof the fluorine-containing high-silicon Y molecular sieve is hF.kM.mR1. NR2. (SixAly) O2, and the silica-alumina ratio of the fluorine-containing high-silicon Y molecular sieve is 25-100. The methodcomprises the following steps: a) mixing raw materials containing an aluminum source, a silicon source, an alkali metal source, a fluorine source, an organic template agent R2 and water to obtain initial gel, then adding a guiding agent or a silicon-aluminum molecular sieve seed crystal, and stirring to obtain synthetic gel; b) dewatering the synthetic gel to obtain a dry powder mixture; and c) crystallizing the dry powder mixture. According to the method disclosed by the invention, the fluorine-containing high silicon Y molecular sieve has characteristics of high silica-alumina ratio, low alkali metal content and easy ion exchange, and the preparation method has characteristics of rapid crystallization rate, simple process, and easy large-scale industrial production.

Description

technical field [0001] This application relates to a fluorine-containing high-silicon Y molecular sieve and its preparation method, and in particular to a synthesis of fluorine-containing high-silicon Y molecular sieve under ultra-low water by introducing an organic template into the synthetic gel system and adding a directing agent or seed crystal. The method for Y molecular sieve belongs to the field of molecular sieve synthesis. Background technique [0002] Y molecular sieve is a silica-alumina molecular sieve with FAU topology, which is mainly used in fluid catalytic cracking (FCC), and is currently the most used molecular sieve material. The silicon-aluminum ratio of Y molecular sieve plays a decisive role in its catalytic performance, and the higher the silicon-aluminum ratio, the better the catalytic activity and stability. At present, the high-silicon Y molecular sieves used in industry are mainly obtained through chemical / physical dealumination, etc. This post-tre...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/24B01J32/00B01J29/08
CPCC01B39/205B01J29/084B01J2229/16B01J2229/18
Inventor 王林英田鹏朱大丽刘中民李冰张建明
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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