Nanometer needle-shaped SAPO-34 molecular sieve, as well as preparation and application thereof

A SAPO-34, nanoneedle technology, applied in molecular sieve and alkali exchange phosphate, molecular sieve characteristic silicoaluminophosphate, nanotechnology and other directions, can solve problems such as difficult application, reporting, environmental pollution, etc., and achieve large specific surface area, operation Easy, step-by-step effects

Active Publication Date: 2017-08-18
SHANTOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The structure-directing agent introduced is a long-chain alkyltrimethylammonium halide. Since the structure-directing agent contains halogen and ammonia, it is easy to pollute the environment during sample processing.
[0005] Patent CN102616810A introduces a SAPO-34 molecular sieve with a crystal size of 20~300nm and a cubic or sheet shape. This patent uses a microwave-assisted synthesis method, but this synthesis method limits large-scale production and is difficult to apply in industrial production.
[0006] At present, the morphology of synthesized SAPO-34 molecular sieves is mostly cubic, and there are also reports of special shapes such as flakes, but there are no reports of nano needle-shaped SAPO-34 molecular sieves.

Method used

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  • Nanometer needle-shaped SAPO-34 molecular sieve, as well as preparation and application thereof
  • Nanometer needle-shaped SAPO-34 molecular sieve, as well as preparation and application thereof
  • Nanometer needle-shaped SAPO-34 molecular sieve, as well as preparation and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Weigh 2.04g of aluminum isopropoxide into the beaker, then add 7.2ml of deionized water into the beaker, then add 0.615ml of phosphoric acid solution, stir for 20 minutes under the condition of heating in a water bath at 35°C, then add 1.32ml of morpholine solution, After continuing to stir for 1 hour, add 0.677ml of tetraethyl orthosilicate dropwise, continue heating and stirring in a water bath for 2 hours to obtain gel A, then add 5.45ml of 40% HF acid solution dropwise, at this time, gel A decondenses into solution B, and then Stirring was continued for 2h. After the solution B obtained above was stirred, it was transferred to a reaction kettle lined with polytetrafluoroethylene. After the kettle was filled, the reaction kettle was moved into an oven for crystallization at 170° C. for 60 hours. Immediately after the crystallization was completed, the reaction kettle was taken out, and the outer wall of the reaction kettle was rinsed with tap water to make it cool ra...

Embodiment 2

[0032] Weigh 2.04g of aluminum isopropoxide into the beaker, then add 7.2ml of deionized water into the beaker, then add 0.615ml of phosphoric acid solution, stir for 20 minutes under the condition of heating in a water bath at 35°C, then add 1.32ml of morpholine solution, After continuing to stir for 2 hours, add 0.677ml of tetraethyl orthosilicate dropwise, continue heating and stirring in a water bath for 3 hours to obtain gel A, then add 5.45ml of 40% HF acid solution dropwise, at this time, gel A decondenses into solution B, and then Stirring was continued for 3h. After the solution B obtained above was stirred, it was transferred to a reaction kettle with a polytetrafluoroethylene lining. After the kettle was filled, the reaction kettle was moved into an oven, and crystallized at 200° C. for 36 hours. Immediately after the crystallization was completed, the reaction kettle was taken out, and the outer wall of the reaction kettle was rinsed with tap water to make it cool ...

Embodiment 3

[0034] The steps in this embodiment are exactly the same as those in Embodiment 1. The difference is: the HF solution taken changed from 5.45ml to 4.35ml. The prepared samples are also nano-acicular SAPO-34 molecular sieves.

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Abstract

The invention relates to a nanometer needle-shaped SAPO-34 molecular sieve, as well as preparation and application thereof. A gel decondensation hydrothermal synthesis method is adopted and particularly comprises the following steps: (1) mixing an aluminum source, a phosphorus source, a silicon source, deionized water and a template agent, heating and stirring to obtain gel A; (2) adding excessive HF solution into the gel A, wherein the gel is decondensed into a solution at this moment; (3) performing hydrothermal crystallization: transferring the solution obtained in the step (2) into a polytetrafluoroethylene reaction kettle, performing high-temperature crystallization, rapidly cooling after the crystallization is completed, filtering and washing the obtained solid, drying and roasting to obtain the nanometer needle-shaped SAPO-34 molecular sieve. The preparation process is simple and easy to operate, and the molecular sieve has important application in methanol to olefin reaction; meanwhile, due to the special shape, the molecular sieve can serve as a carrier of catalyst active components and has potential industrial application prospect.

Description

technical field [0001] The invention belongs to the technical field of zeolite molecular sieve synthesis, and in particular relates to a method for synthesizing nano needle-like SAPO-34 molecular sieves. Background technique [0002] The silicoaluminophosphate molecular sieve SAPO-34 with CHA topology was designed and synthesized by Union Carbide Corporation in 1984. SAPO-34 molecular sieve belongs to the trigonal crystal system, R-3m space group, has an 8-membered ring channel structure, high specific surface area, suitable acidity and good hydrothermal stability, and has excellent performance in the catalytic reaction of methanol to olefins (MTO). It has excellent catalytic performance and high selectivity to low-carbon olefins, so it has attracted extensive attention from researchers. [0003] At present, there are many reports on SAPO-34 molecular sieves. Studies have shown that the preparation of SAPO-34 molecular sieves with smaller grain size can not only increase th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B37/08C01B39/54B82Y30/00B82Y40/00
CPCB82Y30/00B82Y40/00C01B37/08C01B39/54C01P2002/72C01P2004/03C01P2004/10C01P2004/64
Inventor 方奕文张世超熊卫赵汝路旭朋陈文斌杨玲宋一兵
Owner SHANTOU UNIV
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