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Organogel for testing trace water content in organic solvent, preparation method and application thereof

An organic solvent and organogel technology, applied in the direction of chemical analysis by micro-analysis, can solve the problems of not suitable for fast and low-cost analysis, not suitable for liquid sample analysis, expensive equipment and instruments, etc. Fast water splitting, simple and convenient application method, and simple and quick effect

Inactive Publication Date: 2021-06-25
邹沐华
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

As early as 1935, Fischer and Karl et al. proposed a method for determining water content. This method is usually called the Karl Fischer method. This method can accurately and quantitatively determine the trace moisture in the solvent. This method Although accurate and quantitative, the equipment and instruments required are expensive and the operation is complicated, which is not suitable for fast and low-cost analysis
Gas chromatography also has the above-mentioned disadvantages, that is, expensive equipment needs to be purchased
The dry weighing method is easy to operate and the equipment is cheap, but it is not suitable for the analysis of liquid samples

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Under nitrogen protection, dissolve 1 g of hydroxyl-terminated polybutadiene with a number average molecular weight of 2000 in 10 ml of n-hexane, add 0.08 g of triisobutylaluminum (dissolved in 0.5 ml of n-hexane in advance for easy addition), and shake well , standing at room temperature for 5 minutes to obtain the product gel.

[0027] After testing, when the gel is put into an organic solvent to be tested containing a small amount of water (0.1%-5%wt), the gel decomposes rapidly, but no obvious decomposition is seen in anhydrous solvent.

[0028] The above test method is as follows: in a closed container, put 1 g of the organogel prepared in Example 1 into 100 mL of tetrahydrofuran, shake it for 3 minutes, and observe whether the gel is decomposed. The water content of tetrahydrofuran was 0, 0.1%, 0.2%, 0.3%, 0.4%, 0.5% in sequence, and was determined by gas chromatography in advance.

Embodiment 2

[0030] Under nitrogen protection, dissolve 10 g of hydroxyl-terminated polybutadiene with a number average molecular weight of 1000 in 200 ml of n-hexane, add 1 g of triisobutylaluminum (dissolved in 10 ml of n-hexane in advance for easy addition), shake well, and Let it stand for 5 minutes to obtain the product gel.

[0031] After testing, when the gel is put into an organic solvent containing a small amount of water (0.1%-5%wt), the gel decomposes rapidly, but there is no obvious decomposition in an anhydrous solvent.

[0032] The test method is the same as in Example 1, except that the organic solvent to be tested is toluene.

Embodiment 3

[0034] Under nitrogen protection, dissolve 10 g of hydroxyl-terminated polybutadiene with a number-average molecular weight of 200 in 200 ml of n-hexane, add 1 g of triisobutylaluminum (dissolved in 10 ml of n-hexane in advance for easy addition), shake well, and Let it stand for 5 minutes to obtain the product gel.

[0035] After testing, when the gel is put into an organic solvent containing a small amount of water (0.1%-5%wt), the gel decomposes rapidly, but there is no obvious decomposition in an anhydrous solvent.

[0036] The test method is the same as in Example 1, except that the organic solvent to be tested is carbon tetrachloride.

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Abstract

The invention relates to gel, in particular to organogel for testing trace water content in an organic solvent, a preparation method and application thereof. The gel is prepared from a hydroxyl-terminated polymer, trialkyl aluminum and an aprotic organic solvent, wherein the mass ratio of the hydroxyl-terminated polymer to the trialkyl aluminum is (10:1)-(1000:1), the mass ratio of the hydroxyl-terminated polymer to the aprotic organic solvent is (1:100)-(30:100), the hydroxyl-terminated polymer is one or two of hydroxyl-terminated polybutadiene or hydroxyl-terminated polyisoprene, the trialkyl aluminum is one or more of trimethylaluminum, triethyl aluminum or triisobutyl aluminum, and the aprotic organic solvent is one or more of normal hexane, methylbenzene or tetrahydrofuran. According to the invention, the gel can react with trace water in an organic solvent (namely, the gel is decomposed when meeting water); and when the gel is used, the prepared gel is put into the to-be-detected solvent, and whether the water content in the solvent exceeds the standard or not can be judged by observing whether the gel is decomposed or not, so that the cost is low.

Description

technical field [0001] The invention relates to a gel, in particular to an organogel for testing trace water content in an organic solvent, a preparation method and application thereof. Background technique [0002] Trace water tests usually have drying weighing method, gas chromatography and Karl Fischer method. As early as 1935, Fischer and Karl et al. proposed a method for determining water content. This method is usually called the Karl Fischer method. This method can accurately and quantitatively determine the trace moisture in the solvent. This method Although accurate and quantitative, the equipment and instruments required are expensive and the operation is complicated, which is not suitable for fast and low-cost analysis. Gas chromatography also has the above-mentioned disadvantages, that is, expensive equipment needs to be purchased. The dry weighing method is easy to operate and the equipment is cheap, but it is not suitable for the analysis of liquid samples. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N31/20
CPCG01N31/20
Inventor 邹沐华
Owner 邹沐华
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