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Method for preparing aluminum phosphate molecular screen in eutectic mixture

A eutectic mixture, aluminum phosphate molecular sieve technology, applied in the direction of molecular sieve characteristic aluminum phosphate, molecular sieve and alkali-exchanged phosphate, phosphorus compounds, etc., can solve the problem that the template effect of quaternary ammonium salt component cannot be exerted, and limit the aluminum phosphate molecular sieve and other problems, to achieve the effect of not easy to deliquescence and easy to use

Inactive Publication Date: 2009-12-16
TAIYUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, for aluminum phosphate molecular sieves, low-melting mixtures of urea (or urea derivatives) can decompose ammonia or organic amines at high temperatures; while low-soluble mixtures of carboxylic acids have strong acidity, often need to add organic amines to Adjust the acidity and alkalinity of the system, this "extra" organic amine has a strong template effect, so that the template effect of the quaternary ammonium salt component in the system cannot be exerted, which limits the possible formation of aluminum phosphate molecular sieves

Method used

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  • Method for preparing aluminum phosphate molecular screen in eutectic mixture
  • Method for preparing aluminum phosphate molecular screen in eutectic mixture
  • Method for preparing aluminum phosphate molecular screen in eutectic mixture

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Embodiment approach 1

[0024] 2.7g of pentaerythritol and 1.5g of tetramethylammonium bromide (molar ratio is 2.0) are thoroughly ground in a mortar, and then the mixture of the two is placed in a beaker and heated at 130°C until it becomes transparent liquid, a eutectic mixture (DES) was obtained, which turned into a white solid after cooling to room temperature. At room temperature, the prepared 4.2g DES, 0.20gAl[OCH(CH 3 ) 2 ] 3 , 0.23 g H 3 PO 4 , 20μl HF was sequentially added to a 20ml polytetrafluoroethylene-lined stainless steel reactor, and the molar ratio of the final reactant was 0.5HF:1.0Al[OCH(CH 3 ) 2 ] 3 : 2.0H 3 PO 4 : 30DES, after sealing, the crystallization temperature is 180°C for 3 days, after the reaction, take out the reactor and cool to room temperature. The obtained crystallized product was taken out, washed with ethanol, filtered and dried. The final product is a ZON type aluminum phosphate molecular sieve, and its XRD spectrum is shown in the appendix figure 1 ...

Embodiment approach 2

[0026] 2.0g of pentaerythritol and 2.2g of mepizom (molar ratio is 1.0) are thoroughly ground in a mortar, then the mixture of the two is placed in a beaker and heated at 130°C until it becomes a transparent liquid, then A eutectic mixture (DES) was obtained which became a white solid upon cooling to room temperature. At room temperature, the prepared 4.2g DES, 0.21g Al[OCH(CH 3 ) 2 ] 3 , 0.23 g H 3 PO 4 , 20μl HF was added to a 20ml polytetrafluoroethylene-lined stainless steel reaction kettle in turn, and the molar ratio of the final reactant was 0.5HF:1.0Al[OCH(CH 3 ) 2 ] 3 : 2.0H 3 PO 4 : 29DES, after sealing, the crystallization temperature was 180°C for 3 days, and after the reaction was completed, the reactor was taken out and cooled to room temperature. The obtained crystallized product was taken out, washed with ethanol, filtered and dried. The final product is an ERI aluminum phosphate molecular sieve, and its XRD spectrum is shown in the appendix of the sp...

Embodiment approach 3

[0028] No HF was added to the initial reaction system, and the molar ratio of the final reactant was 1.0Al[OCH(CH 3 ) 2 ] 3 : 2.0H 3 PO 4 : 29DES, others are the same as embodiment 2, and the final product is an AWW type aluminum phosphate molecular sieve, and its XRD spectrogram is shown in the attached description image 3 .

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Abstract

The invention provides a method for preparing an aluminum phosphate molecular screen in a eutectic mixture, and belongs to the field of inorganic chemical synthesis. In particular, the invention relates to a method for an aluminum phosphate molecular screen by the eutectic mixture as a reaction solvent and a template. The method is characterized by using the eutectic mixture prepared by combining alcohol and quaternary ammonium salt as the reaction solvent and the template to prepare the aluminum phosphate molecular screen. In the ion thermal reaction, the eutectic mixture has proper acidity and alkaline, the alcohol organic matters are not decomposed to release extra organic amine in the crystallization reaction process when being heated, and the quaternary ammonium salt in the system can fully complete the structure guide action. Compared with the imidazole ionic liquid, the used eutectic mixture material has the advantages of low price, easy purchase and preparation, hard deliquescence and convenient use.

Description

technical field [0001] The invention discloses a method for preparing aluminum phosphate molecular sieves in a eutectic mixture, belonging to the field of inorganic chemical synthesis. Specifically, it relates to a method for preparing aluminum phosphate molecular sieves by using a eutectic mixture as a reaction solvent and a template agent. Background technique [0002] Thermal synthesis of ionic liquids is a new synthesis method of inorganic crystal materials reported by the research group of Professor Russell Morris of St Andrews University in the UK in 2004. This method is different from the traditional solvothermal method, and its characteristic is that in the synthesis system, ionic liquids not only It is not only a solvent, but also a solvent and a template. The thermal synthesis of ionic liquids has brought the synthesis of inorganic crystal materials to a completely new field, so it has been highly valued by people. [0003] Metallophosphate molecular sieves have t...

Claims

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Application Information

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IPC IPC(8): C01B39/54C01B37/04
Inventor 刘雷李西平徐红李晋平董晋湘
Owner TAIYUAN UNIV OF TECH
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