Non-pyridine karl fischer agent as well as preparing method

A technology of pyridine Karl Fei and reagents, which is applied in the direction of chemical analysis by titration, can solve the problems of cumbersome operation process, high cost of raw materials, poor stability, etc., and achieve the effects of reducing environmental pollution, good stability, and stable storage

Inactive Publication Date: 2008-09-03
SHANGHAI CHEM REAGENT RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a kind of pyridine-free Karl Fischer reagent, to overcome the poor stability of imidazole in the prior art instead of pyridine products, high cost of raw materials, self-preparation when using two-component products, calibration titer, and cumbersome operation process insufficient

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Add 68 mol of ethanol to a reactor equipped with a stirrer and a temperature control device, add 15 mol of n-butylamine at room temperature, stir evenly, control the temperature at 18-23°C, feed 8.5 mol of sulfur dioxide, and slowly add a total of 3.2 mol in batches iodine, keep mixing evenly, continue stirring for more than 30 minutes, and leave overnight to obtain the product. Product testing: Sensitivity qualified, titer 3.6mgH 2 O / ml reagent, the stable time of the reaction end point is 2.8 minutes, and the application test is qualified. After 180 days of keeping the product sample, the titer is 3.4mgH 2 O / ml reagent.

Embodiment 2

[0022] Add 72 mol of ethanol to a reactor equipped with a stirrer and a temperature control device, add 21.5 mol of diethylamine at room temperature, stir evenly, control the temperature at 20-25°C, introduce 9.2 mol of sulfur dioxide, and slowly add a total of 3.5 mol in batches mol of iodine, keep mixing evenly, continue to stir for more than 30 minutes, and leave overnight to obtain the product. Product testing: Sensitivity qualified, titer 3.8mgH 2 O / ml reagent, the stable time of the reaction end point is 2.4 minutes, and the application test is qualified. After 180 days of keeping the product sample, the titer is 3.6mgH 2 O / ml reagent.

Embodiment 3

[0024] Add 66 mol of ethanol to a reactor equipped with a stirrer and a temperature control device, add 18.3 mol of triethylamine at room temperature, stir evenly, control the temperature at 30-35°C, introduce 8.8 mol of sulfur dioxide, and slowly add a total of 3.2 mol in batches. mol of iodine, keep mixing evenly, continue to stir for more than 30 minutes, and leave overnight to obtain the product. Product testing: Sensitivity qualified, titer 3.6mgH 2 O / ml reagent, the stable time of the reaction end point is 2.4 minutes, and the application test is qualified. After 180 days of keeping the product sample, the titer is 3.6mgH 2 O / ml reagent.

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PUM

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Abstract

The invention relates to a karl fischer reagent without pyridine and a preparing method. The specific composition and molar percentage provided by the invention include alcohol 60-75, aliphatic amine 14-25, sulfur dioxide 7.8-12, iodine 3.1-3.7, aliphatic amine, sulfur dioxide and iodine are added into the alcohol in sequence, the reagent is prepared at a certain temperature, and the target product is obtained. Compared with the prior art, cheap aliphatic amine is used to substitute pyridine, the methanol is not contained, which effectively reduces the product cost and the environment pollution and is helpful to the health of the operating staffs, the reagent provided by the invention has good storage stability and is easy to operate.

Description

technical field [0001] The invention relates to a pyridine-free Karl Fischer reagent and a preparation method. Background technique [0002] Karl Fischer Reagent (Karl-Fischer Reagent), also known as Karl Fischer Reagent, is a commonly used reagent for analyzing and determining water content. It is widely used in fields such as medicine, chemical industry, and petroleum processing. Internationally and domestically recognized common methods. [0003] Karl Fischer reagent is a mixed reagent containing pyridine, iodine, sulfur dioxide, and methanol. Because pyridine has a foul smell and pollutes the environment, methanol is highly toxic, endangers human health, has poor storage stability, and has poor use effects. People use no pyridine and no methanol For the goal, the Karl Fischer reagent has been continuously improved. Data show that there are many documents on pyridine-free Karl Fischer reagent and preparation methods, such as chemical reagents, 16 (4), 244-245; 254 (1994...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N31/16
Inventor 廖本仁安国成
Owner SHANGHAI CHEM REAGENT RES INST
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