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-CLO structural aluminum phosphate molecular sieve and preparation method thereof

A technology of aluminum phosphate molecular sieve and molecular sieve, applied in the field of molecular sieve, can solve the problem of long crystallization time of molecular sieve, and achieve the effects of low synthesis cost, no acid and alkali discharge, safe and convenient operation

Inactive Publication Date: 2011-08-03
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Xu Yunpeng and others disclosed a method for synthesizing aluminum phosphate molecular sieves by microwave heating in the Chinese patent document CN100410172C. This method adopts the synthesis method of ion heat, and uses microwave radiation as the heating method at the same time, which overcomes the problem of water in the conventional aluminum phosphate molecular sieve hydrothermal synthesis process. Disadvantages such as hot high pressure process and long crystallization time of molecular sieves

Method used

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  • -CLO structural aluminum phosphate molecular sieve and preparation method thereof
  • -CLO structural aluminum phosphate molecular sieve and preparation method thereof
  • -CLO structural aluminum phosphate molecular sieve and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0033] Add 52.8g of 1-ethyl-3-methylimidazolium bromide ionic liquid (EMIMBr) into a 100ml beaker, heat up to 100°C, add 0.8g of phosphoric acid with a concentration of 85wt%, 1.4g of aluminum isopropoxide, and mix evenly Add 0.41g concentration of 40% hydrofluoric acid dropwise, stir until uniform, then add 0.64g hexamethylenediamine (HDA), continue stirring until uniform to obtain the reaction precursor mixture, the mixture of Al 2 o 3 :P 2 o 5 :F - The ratio of :EMIMBr:HDA (phosphorus and aluminum are expressed in the form of their oxides) is (molar ratio) 1:1:2.4:80:1.6. Transfer the mixture to a 100ml stainless steel reaction kettle with a Teflon liner, put it in an oven at 230°C, and keep it for 1 hour, then cool the reaction mixture to room temperature, add 150ml of deionized water, stir, and wash it ultrasonically. The thing was filtered to obtain a white solid powder, which was washed three times, and the white powder was washed with 50ml of acetone. The final wh...

Embodiment 2

[0035] Add 52.8g of 1-ethyl-3-methylimidazolium bromide ionic liquid (EMIMBr) into a 100ml beaker, heat up to 100°C, add 0.8g of phosphoric acid with a concentration of 85wt%, 1.4g of aluminum isopropoxide, and mix evenly Add 0.34g concentration of 40% hydrofluoric acid dropwise, stir until uniform, then add 0.40g hexamethylenediamine (HDA), continue stirring until uniform to obtain the reaction precursor mixture, the mixture of Al 2 o 3 :P 2 o 5 :F - The ratio of :EMIMBr:HDA (phosphorus and aluminum expressed in the form of their oxides) is (molar ratio) 1:1:2:80:1. Transfer the mixture to a 100ml stainless steel reaction kettle with a polytetrafluoroethylene liner, put it in an oven at 190°C, and keep it for 6 hours, then cool the reaction mixture to room temperature, add 150ml of deionized water, stir, and wash it ultrasonically. The thing was filtered to obtain a white solid powder, which was washed three times, and the white powder was washed with 50ml of acetone. Th...

Embodiment 3

[0037] Add 52.8g of 1-ethyl-3-methylimidazolium bromide ionic liquid (EMIMBr) into a 100ml beaker, heat up to 100°C, add 0.8g of phosphoric acid with a concentration of 85wt%, 1.4g of aluminum isopropoxide, and mix evenly Add 0.16g concentration of 40% hydrofluoric acid dropwise, stir until uniform, then add 0.12g hexamethylenediamine (HDA), continue stirring until uniform to obtain the reaction precursor mixture, the mixture of Al 2 o 3 :P 2 o 5 :F - The ratio of :EMIMBr:HDA (phosphorus and aluminum are expressed in the form of their oxides) is (molar ratio) 1:1:0.8:80:0.3. Transfer the mixture to a 100ml stainless steel reaction kettle with a polytetrafluoroethylene liner, put it in an oven at 150°C, and keep it for 12 hours, then cool the reaction mixture to room temperature, add 150ml of deionized water, stir, and wash it ultrasonically. The thing was filtered to obtain a white solid powder, which was washed three times, and the white powder was washed with 50ml of ace...

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Abstract

The invention relates to a -cloverite (-CLO) structural aluminum phosphate molecular sieve Dalian national laboratory number 1 (DNL-1) and a preparation method thereof. The -CLO structural aluminum phosphate molecular sieve DNL-1 confirmed by International Zeolite Association is synthesized by an ionothermal method, wherein ionic liquid serves as a reaction medium. The molecular sieve has high stability, extremely low skeletal density and a wide application prospect in aspects of catalysis, gas adsorption and separation and the like. The preparation method is high in economy, is safe in operation, is convenient to operate and is environment-friendly.

Description

technical field [0001] The invention relates to a molecular sieve, in particular to an aluminum phosphate molecular sieve with a -CLO structure and a preparation method thereof. Background technique [0002] Molecular sieves, as the name implies, refer to substances with sieving ability in molecular size. Due to its regular pore structure and unique surface properties, it has been widely used in catalysis, ion exchange, adsorption and separation and other fields. The earliest molecular sieve material recognized by human beings is natural zeolite. In the 1940s, Barrer R M and others realized the artificial synthesis of molecular sieves for the first time. Afterwards, a large number of molecular sieve materials were artificially synthesized one after another. However, with the development of industry, many fields require The performance and structure of molecular sieves put forward higher requirements, so the development of new molecular sieve materials is of great significan...

Claims

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Application Information

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IPC IPC(8): C01B37/04C01B39/54
CPCC01B39/54B01J29/83C01B37/04B01J20/18B01J20/08
Inventor 田志坚魏莹裴仁彦马怀军李科达徐云鹏
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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