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Cubic aluminum formate, gallium formate and preparing method

A technology of aluminum formate and formic acid, applied in the preparation of carboxylate, etc.

Inactive Publication Date: 2007-09-12
LIAONING NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

There is no report on cubic gallium formate, and its crystal parameters are: a=b=c=11.540 Ȧ, space group: Im-3, which has the same structure as cubic aluminum formate

Method used

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  • Cubic aluminum formate, gallium formate and preparing method
  • Cubic aluminum formate, gallium formate and preparing method
  • Cubic aluminum formate, gallium formate and preparing method

Examples

Experimental program
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Effect test

example 1

[0009] Example 1 Aluminum nitrate and formic acid redox reaction to remove nitrate preparation method

[0010] Weigh 1.0g Al(NO 3 ) 3 9H 2 O, first add 1 / 10 of it to about 40mL of formic acid (88%) or anhydrous formic acid. After about 5 minutes, formic acid and nitrate undergo a redox reaction to generate CO2 and NO, and then add the remaining Al(NO 3 ) 3 9H 2 O (in order to control the reaction rate, the reaction can be placed in a condensed water bath). During the reaction process, a large amount of formed [Al(HCOO) 3 3 / 4 CO 2 1 / 4H 2 O·1 / 4 HCOOH] cubic aluminum formate crystals produced. After filtering, place it in a desiccator with Na(OH) as desiccant and dry it. Yield is more than 70% (as Al(NO 3 ) 3 9H 2 O meter).

example 2

[0011] Example 2 Acid-base neutralization method of Al(OH)3 and formic acid in CO2 atmosphere

[0012] Add 2.0g of Al(OH)3 solid to a 250mL three-necked bottle filled with 80mL formic acid (88%) or anhydrous formic acid. Heating to reflux and feeding CO2 gas to react for 3 days. XRD shows that Al(OH)3 has all produced cubic aluminum formate. After filtering, the product is dried in a desiccator using Na(OH) as desiccant. The yield is over 90% (calculated as Al(OH)3). For mass production of cubic aluminum formate, the reaction temperature should be above 100°C, and the CO2 atmosphere pressure should be carried out in a reactor above 1 bar, which will greatly shorten the reaction time.

[0013] There are two specific preparation methods for cubic gallium formate:

example 3

[0014] Example 3 Preparation method of gallium nitrate and formic acid redox reaction to remove nitrate

[0015] Weigh 1.0g Ga(NO 3 ) 3 ·xH 2 O, first add 1 / 10 of it to about 40mL of formic acid (88%) or anhydrous formic acid. After about 5 minutes, formic acid and nitrate undergo a redox reaction to generate CO2 and NO, and then add the remaining Ga(NO 3 ) 3 ·xH 2 O (in order to control the reaction rate, the reaction can be placed in a condensed water bath). During the reaction process, a large amount of generated composition is [Ga(HCOO) 3 3 / 4 CO 2 1 / 4H 2 O · 1 / 4 HCOOH] cubic indium formate (space group: Im-3) crystals produced. After filtering, the product is dried in a desiccator using Na(OH) as desiccant. The yield is above 80% (with Ga(NO 3 ) 3 ·xH 2 O meter).

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Abstract

This invention relates to anhydrous cubic Al formate and Ga formate and their preparation method aiming at providing a compound of organic Al and Ga in a pure sinlge object phase to be the precursor of advanced ceramic material Al2O3 and semiconductor material Ga2O3 nm particles, in which, the structure of the cubic Al formate includes: a=b=c=11.448 and the space group: Im-3, the cubic Ga formate: a=b=c=11.540 and the space group: Im-3. The product is affirmed to be a 3-D coordinated polymer tested by an X-ray monocrystal diffractor, the chemical formula is [M(HCOO)3.3 / 4CO2.1 / 4 H2O.1 / 4HCOOH], the framework structure of M(HCOO)3 is shown in the ReO3 topology, and CO2, H2O and HCOOH are object molecules, and the test result of X-ray powder diffraction is the same to the analog result of its monocrystal diffraction and the product is shown to be a sinlge pure phase, and experiment shows that AlO2 and Ga2O3 particles can be got by thermo-analysis of cubic Al formate and In formate.

Description

technical field [0001] The invention relates to cubic aluminum formate and gallium formate and a preparation method thereof. The general chemical formula of cubic aluminum formate and gallium formate is [M(HCOO) 3 3 / 4 CO 2 1 / 4H 2 O·1 / 4 HCOOH], M(HCOO) 3 The skeleton structure is in ReO3 topology, where CO 2 、H 2 O and HCOOH are guest molecules. A literature search shows that the chemical formula of cubic aluminum formate has been mistaken for [Al(HCOO) 3 ·xH 2 O]; Cubic gallium formate is a new compound, and they are all precursors for the preparation of oxide nanoparticles by thermal decomposition. The preparation methods of cubic aluminum formate include: (1) under CO2 atmosphere, use Al(OH)3 and formic acid reaction preparation method, including normal pressure and non-pressure reaction preparation; (2) aluminum nitrate and formic acid reaction preparation method, this method is in The CO2 produced during the redox reaction between nitrate and formic acid provides ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C53/06C07C51/41
Inventor 田运齐
Owner LIAONING NORMAL UNIVERSITY
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