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Method for synthesizing P-Al molecular sieve by microwave heating

A technology of phosphorus-aluminum molecular sieve and microwave heating, which is applied in molecular sieve catalysts, molecular sieves and alkali-exchanged phosphates, chemical instruments and methods, etc., can solve problems such as long crystallization time of molecular sieves, expensive organic template agents, acid-base waste liquid discharge, etc. , achieving the effects of low synthesis cost, environmental friendliness, and fast crystallization rate

Inactive Publication Date: 2008-08-13
PETROCHINA CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The purpose of the present invention is to provide a method for synthesizing aluminum-phosphorus molecular sieves to overcome the disadvantages of hydrothermal high-pressure process in conventional hydrothermal synthesis of aluminum-phosphorus molecular sieves, long crystallization time of molecular sieves, use of expensive organic templates, and discharge of acid-base waste liquid

Method used

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  • Method for synthesizing P-Al molecular sieve by microwave heating
  • Method for synthesizing P-Al molecular sieve by microwave heating
  • Method for synthesizing P-Al molecular sieve by microwave heating

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[0017] The synthetic method of aluminum phosphorus molecular sieve of the present invention comprises: phosphorus source, aluminum source, ionic liquid and mineralization agent make uniform reaction mixture aP 2 o 5 :Al 2 o 3 : b ionic liquid: c mineralizer (a, b, c are molar ratios in the formula) is heated up gradually under microwave radiation heating, and the reaction mixture is carried out ion thermal crystallization under a certain temperature and pressure for a certain period of time, and then filtered, washed, Drying, the specific conditions are: (1) The mixing temperature of the reaction raw materials is: 10-150°C; (2) The crystallization conditions are: at the crystallization temperature of 100-300°C, under normal pressure or autogenous pressure, the crystallization time is 1-200 Minutes; (3) in the composition of the reaction mixture, a is 0.5-10, b is 0.1-100, and c is 0.01-2.

[0018] The crystallization process of the molecular sieve in the above synthesis met...

Embodiment 1

[0033]Add 1-ethyl-3-methylimidazolium bromide ionic liquid into a three-necked flask and heat up to 100°C, then add phosphoric acid and aluminum isopropoxide and mix well, then add mineralizer HF and mix well, the resulting mixture is aP 2 o 5 :Al 2 o 3 : b ionic liquid: cHF, where in molar ratio, a=3, b=40, c=0.6; the above mixture is heated to 150° C. under microwave radiation, and crystallized for 60 minutes under normal pressure or autogenous pressure; the above reaction mixture is cooled to room temperature, filter, wash the filtrate with water or an organic solvent, and dry at 100°C to obtain a powder product of aluminum phosphorus molecular sieve, which is AlPO-11 molecular sieve by XRD test.

Embodiment 2

[0035] Add 1-butyl-3-methylimidazolium bromide ionic liquid into a three-necked flask and heat up to 100°C, add phosphoric acid and aluminum isopropoxide and mix well, then add mineralizer HF and mix well, the resulting mixture is aP 2 o 5 :Al 2 o 3 : b ionic liquid: cHF, where in molar ratio, a=3, b=40, c=0.6; the above mixture is heated to 150° C. under microwave radiation, and crystallized for 60 minutes under normal pressure or autogenous pressure; the above reaction mixture is cooled to room temperature, filter, wash the filtrate with water or an organic solvent, and dry at 100°C to obtain a powder product of aluminum phosphorus molecular sieve, which is AlPO-5 molecular sieve by XRD test.

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Abstract

The invention discloses a synthesizing method of amblygonite molecular sieve, which comprises the following steps: A) heating ionic liquid to 10-150 deg.c; adding phosphor source and aluminum source to blend evenly; adding mineralizer to mix evenly; producing molar proportion at 0.5-1.0 a, 0.1-100 b and 0.01-2 c for aP2O5:Al2O3:b ionic liquid : c mineralizer; B) heating step A compositions to 100-300 deg.c through microwave irradiation; crystallizing for 1-200 min under normal pressure or self-pressure; C) cooling step B composition to indoor temperature; filtering; washing filtrate through water or organic solvent; drying at 80-110 deg.c to produce powder-shaped product. The invention is rapid to synthesize the molecular sieve, which saves cost effectively.

Description

technical field [0001] The invention relates to a method for synthesizing molecular sieve materials, in particular to a method for synthesizing phosphorus-aluminum molecular sieves by microwave heating. Background technique [0002] Aluminum phosphorus molecular sieve is an important porous material, which is widely used in catalytic reaction and adsorption separation process. At present, the main methods for the synthesis of aluminum phosphorus molecular sieves are: hydrothermal synthesis, solvothermal synthesis, gas phase transfer and microwave synthesis using special heating methods (CN03155999.9, CN03150739.5, CN87104924, CN02130787.3, CN03121112.7 , CN02129306.6, CN99112754.4, CN99112751.X, US7014827, US6620983, US4440871, US5096684, US6111037, US5296208, US5126308, US6160191). The common features of these methods are: at high temperature, due to the volatile solvent medium will generate a certain autogenous pressure, the synthesis reaction is generally carried out in ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/54B01J29/83
Inventor 徐云鹏田志坚王炳春王磊魏莹马怀军李鹏
Owner PETROCHINA CO LTD
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