Method for preparing silicon-aluminum-phosphorus molecular sieve from montmorillonite, product obtained by method and application thereof

A montmorillonite and molecular sieve technology is applied in the field of molecular sieves to achieve the effect of reducing costs, wide distribution and low price

Active Publication Date: 2010-11-24
CHNA ENERGY INVESTMENT CORP LTD +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] Although montmorillonite has been used as a silicon source in the synthesis of other molecular sieves, there has b

Method used

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  • Method for preparing silicon-aluminum-phosphorus molecular sieve from montmorillonite, product obtained by method and application thereof
  • Method for preparing silicon-aluminum-phosphorus molecular sieve from montmorillonite, product obtained by method and application thereof
  • Method for preparing silicon-aluminum-phosphorus molecular sieve from montmorillonite, product obtained by method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0079] Add 4.23g of montmorillonite to 25ml of 0.2M NaOH solution. The montmorillonite was activated in alkaline solution for 4h. Add 5ml of 0.2M NH 4 NO 3 aqueous solution, so that the pH of the activated montmorillonite solution is 8.5. Weigh 30 g of triethylamine, add it into the above solution, and react the triethylamine with the silicon in the activated solution or the silicon source on the surface of the activated montmorillonite. Dissolve 9g of pseudo-boehmite in 18g of water, add the pseudo-boehmite slurry into the mixed solution of montmorillonite and triethylamine, and stir for 30 minutes. Take 14.61g of 85% phosphoric acid, add it to the above solution, and stir for 2h. After the crystallization stock solution was aged for 2 hours, it was hydrothermally crystallized at 200°C for 72 hours. After chilling, filter, wash, dry, and activate by roasting at 600°C for 4h.

[0080] figure 2 It is the XRD spectrum of the SAPO-34 molecular sieve synthesized in situ fr...

Embodiment 2

[0084] Add 4.23g of montmorillonite to 25ml of 0.2M NaOH solution. The montmorillonite was activated in alkaline solution for 4h. Add 5ml of 0.2M NH 4 NO 3 aqueous solution, so that the pH of the activated montmorillonite solution is 8.5. Weigh 20 g of triethylamine, add it into the above solution, and react the triethylamine with the activated solution silicon or surface silicon. Dissolve 9 g of pseudo-boehmite in 18 g of water, add the slurry of pseudo-boehmite into the activated montmorillonite solution, and stir for 30 minutes. Weigh 14.61 g of 85% phosphoric acid, add to the above solution, and stir for 2 h. After the crystallization stock solution was aged for 2 hours, it was poured into a hydrothermal crystallization kettle, and hydrothermally crystallized at 200° C. for 48 hours. After chilling, filter, wash, dry, and activate by roasting at 600°C for 4h. XRD spectrum as image 3 As shown, the XRD characterization results show that the obtained product is a SAPO...

Embodiment 3

[0086] Add 4.23g of montmorillonite to 25ml of 0.2M NaOH solution. The montmorillonite was activated in alkaline solution for 4h. Add 5ml of 0.2M NH 4 NO 3 aqueous solution, so that the pH of the activated montmorillonite solution is 8.5. Weigh 30 g of triethylamine, add it into the above solution, and react the triethylamine with the activated solution silicon or surface silicon. Dissolve 9 g of pseudo-boehmite in 18 g of water, add the slurry of pseudo-boehmite into the activated montmorillonite solution, and stir for 30 minutes. Weigh 14.61 g of 85% phosphoric acid, add to the above solution, and stir for 2 h. After the crystallization stock solution was aged for 2 hours, it was poured into a hydrothermal crystallization kettle, and hydrothermally crystallized at 200° C. for 48 hours. After chilling, it was filtered, washed, dried, and activated by calcination at 600°C for 4 hours. XRD characterization results showed that the obtained product was SAPO-34 molecular siev...

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Abstract

The invention relates to a method for preparing a silicon-aluminum-phosphorus molecular sieve from montmorillonite, a molecular sieve product obtained by the method and application thereof. The method comprises the following steps of: activating the montmorillonite with alkaline solution; mixing the activated montmorillonite, an aluminum source, a phosphorus source, a template and de-ionized water; and performing hydrothermal crystallization reaction on the mixture, wherein the product after the crystallization comprises a small-sized silicon-aluminum-phosphorus molecular sieve grown on a laminar structure and free silicon-aluminum-phosphorus molecular sieve. The silicon-aluminum-phosphorus molecular sieve prepared from the montmorillonite serving as a raw material is partially the small-sized silicon-aluminum-phosphorus molecular sieve grown on the laminar structure, so the influence of internal diffusion of reactant molecules and product molecules can be effectively reduced; and the silicon-aluminum-phosphorus molecular sieve is partially the free silicon-aluminum-phosphorus molecular sieve. An active skeletal silicon source formed by activating the montmorillonite with the alkaline solution contributes to forming a small-grain silicon-aluminum-phosphorus molecular sieve on the surface of the montmorillonite laminar structure and diffusing the reactant molecules and the product molecules; and the montmorillonite is widely distributed in China and has low cost, so the cost for synthesizing the silicon-aluminum-phosphorus molecular sieve is reduced.

Description

technical field [0001] The present invention relates to molecular sieves, more particularly to silicon aluminum phosphorus molecular sieves. Background technique [0002] The US patent USP4440871 in 1984 disclosed that a certain proportion of silicon source, aluminum source, phosphorus source and template were mixed, and hydrothermal crystallization at 100-250 ° C was used to synthesize a variety of new silicon aluminum phosphate series (SAPO-n) molecular sieves . [0003] Since the grain size has a great influence on the product selectivity of the MTO reaction, many scholars have devoted themselves to the development of small particle size molecular sieve catalysts. EP-A-541915 describes in specification that small particle size catalyst is beneficial to low carbon olefins (C 2 ~C 4 ), and disclosed that the small-grain SAPO-34 was obtained by stirring the crystallization mixture to reduce the intramolecular diffusion resistance. Exxon Mobil Chemical Patent Company disc...

Claims

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Application Information

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IPC IPC(8): C01B39/54C01B37/08
Inventor 邢爱华蒋立翔李艺朱伟平岳国
Owner CHNA ENERGY INVESTMENT CORP LTD
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