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Methanol indicator and preparation method thereof

An indicator, methanol technology, applied in material analysis by observing the influence of chemical indicators, analysis by making materials undergo chemical reactions, cobalt organic compounds, etc., can solve problems such as expensive, few, time-consuming and laborious , to achieve the effect of easy operation, wide application and simple synthesis

Inactive Publication Date: 2014-08-27
HUAZHONG NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the appearance, smell, taste, density, and combustion status of methanol are very similar to alcohol, and it is difficult to distinguish them by simple methods such as senses.
However, there are very few reports at home and abroad on how to detect methanol simply, effectively, conveniently and quickly.
Several methanol detection methods commonly used at present are either expensive, or time-consuming and labor-intensive, and cannot well meet the needs of cheap, convenient and fast in daily life.

Method used

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  • Methanol indicator and preparation method thereof
  • Methanol indicator and preparation method thereof
  • Methanol indicator and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Embodiment 1 (NBu 4 )[(Tp)Fe(CN) 3 ]Synthesis:

[0017] Weigh FeCl 2 . 2H 2 O 1.2 g and KTp 4 g, add 30 ml of methanol, stir for 2 h and then filter, discard the filtrate and then add 30 ml of methanol, add 1.36 g of NaCN aqueous solution, and stir overnight at 60 °C. Remove the solvent, dissolve the solid in hot water (70-80°C), filter while it is hot, add NBu after the filtrate is cooled 4 Br (tetrabutylammonium bromide) 7 g, add 30% H 2 o 2 20 ml, after stirring for 10 h, an orange-red solid was produced, which was collected, washed with ether, dried in the air, mixed in methanol solution or diffused with ether for recrystallization to obtain orange-red crystals.

Embodiment 2

[0018] The synthesis of embodiment 2 DCEB

[0019] Weigh 4 g of 2,2'-bipyridine-4,4'-dicarboxylic acid in 30 ml of ethanol, then drop into 4 ml of concentrated sulfuric acid, stir, and heat to reflux for 120 h. The ethanol was removed, and 5 ml of water was added to the residue. After neutralization by sodium carbonate, a white solid was produced. The solid was collected, washed with water, and dried in vacuum to obtain a white powder. Yield: 68%.

Embodiment 3

[0020] Synthesis and characterization of the methanol indicator complex of embodiment 3

[0021] (1) Synthesis: Add Co(ClO 4 ) 2 . 6H 2 O 46 mg and 75 mg of DCEB synthesized above, then add 20 ml of anhydrous methanol, stir until completely dissolved, add (NBu 4 )[(Tp)Fe(CN) 3 ] 70 mg, continued to stir for 2 h, filtered, and the red powder after rotary evaporation to remove the volatile solvent was the target compound. In addition, if the filtrate is allowed to stand for a week, green crystals can be obtained with a yield of 60% (171 mg), which is the methanol adduct of the target product.

[0022] (2) Crystal structure determination of methanol indicator complex methanol adduct

[0023] A green crystal with a size of about 0.08×0.12×0.35 mm was selected, and the Mo Kα ray (λ = 0.71703 ?) monochromated by graphite was used as the light source on the Bruker APEX-II CCD X-ray diffractometer, and the measurement temperature was At 100(2) K, the unit cell parameters were c...

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Abstract

The invention relates to a methanol indicator and a preparation method thereof. The methanol indicator of the present invention is a Fe2Co2 tetranuclear compound linked by cyano groups, and its chemical formula is: [Co2Fe2(CN)6(Tp)2(4,4'-DCEB)4](ClO4)2, wherein Tp is tripyrazole borate, DCEB is ethyl 2,2'-bipyridine-4,4'-dicarboxylate. The methanol indicator of the present invention is usually displayed as red, and only turns green immediately after contacting methanol solvent. The structure of the green compound after combining with methanol was determined by X-ray single crystal diffraction, and it was confirmed to be a planar tetragonal Fe2Co2 tetranuclear coordination compound bridged by cyano groups, and the molecular formula is [Co2Fe2(CN)6(Tp)2( 4,4'-DCEB)4] (ClO4)2.2MeOH, where MeOH is methanol. The methanol indicator of the present invention shows a highly selective response to methanol molecules, and has no response to other various alcohol solvents and other various non-alcohol solvents; it has the advantages of simple synthesis, easy operation, fast response, clear color change indication and The advantages of being reusable and recyclable.

Description

technical field [0001] The invention relates to a methanol indicator molecule and a preparation method thereof. Background technique [0002] Using counterfeit industrial alcohol with high concentration of methanol to make white wine, causing poisoning incidents, poisoning tens of thousands of people and killing hundreds of people, this is a well-known and feared acute methanol poisoning accident. What's more, some companies use methanol to fake alcohol (ethanol) and mix it into gasoline in order to make more profits. The reason is that the price of methanol is about half that of alcohol, which is the source of the proliferation of counterfeit industrial alcohol. However, the appearance, smell, taste, density, and combustion status of methanol are very similar to alcohol, and it is difficult to distinguish them by simple methods such as senses. However, there are very few reports at home and abroad on how to detect methanol simply, effectively, conveniently and quickly. ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F15/06G01N21/78
Inventor 李东风曹莉王锋王成刚宋学刚
Owner HUAZHONG NORMAL UNIV
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