Safe stable type Karl Fischer reagent and preparation method thereof

A Karl Fischer reagent, safe and stable technology, applied in the field of chemistry, can solve problems such as poor storage stability, unfavorable environmental protection, health hazards of users, etc., and achieve the effect of stable quality

Inactive Publication Date: 2012-07-18
JIANGSU YONGHUA FINE CHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Existing Karl Fischer reagent is a mixed reagent of pyridine, methanol, iodine and sulfur dioxide, wherein because pyridine has a foul smell, it pollutes the operating environment; methanol is highly toxic, endangers human health, has poor storage stability, short

Method used

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  • Safe stable type Karl Fischer reagent and preparation method thereof
  • Safe stable type Karl Fischer reagent and preparation method thereof

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Embodiment Construction

[0016] The preferred embodiments of the present invention will be described in detail below in conjunction with the accompanying drawings, so that the advantages and features of the present invention can be more easily understood by those skilled in the art, so as to define the protection scope of the present invention more clearly.

[0017] combine figure 1 Shown, safe and stable type Karl Fischer reagent preparation method of the present invention a preferred embodiment technological process is as follows:

[0018] 1. Mixed reaction

[0019] In a 100L reactor, add 65kg of diethylene glycol methyl ether, add 10kg of diethanolamine and 5kg of pyridine under stirring, and stir and mix for 10 minutes.

[0020] 2. Slowly feed 14kg of sulfur dioxide into the mixed solution while cooling. At the end of the ventilation, the pH of the central control test was 4-7.

[0021] 3. Cool the semi-finished product that has passed the inspection of the central control to 10-15°C, and slowl...

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Abstract

The invention discloses a safe stable type Karl Fischer reagent which comprises the following components in percentage by mass: 60-64 percent of diethylene glycol monomethyl ether, 8-12 percent of diethanol amine, 3.5-5.5 percent of pyridine, 12-15 percent of sulfur dioxide and 8-12 percent of iodine. The preparation method of the safe stable type Karl Fischer reagent comprises the following steps of: adding the diethylene glycol monomethyl ether, the diethanol amine and the pyridine in a reaction kettle and mixing; introducing the sulfur dioxide; after the gas is introduced, cooling the mixed solution below 25DEG C; and adding the iodine and stirring the mixed solution until the iodine is completely dissolved and obtaining a target product. According to the safe stable type Karl Fischer reagent and the preparation method thereof disclosed by the invention, original poisonous dangerous solvent is replaced by a safety type solvent, so that the safe stable type Karl Fischer reagent is non-poisonous, safe, environment-friendly and stable in quality; and after the safe stable type Karl Fischer reagent is stored for a long time, the titer is still within a usable range.

Description

Technical field [0001] The invention involves chemical fields, especially a safe and stable Kar Fei test agent and their preparation methods. Background technique [0002] Karl-Fischer Reagent, also known as the Casa reagent, is a commonly used reagent that analyzes water content. It has a wide range of applications in neighborhoods such as medicine, chemical industry, and oil processing.Moisture is a recognized general method internationally and domestic. [0003] The existing Carbayo reagents are hybrid reagents for pyridine, methanol, iodine, and sulfur dioxide. Among them, due to pyridine have a bad odor and pollution operation environment; methanol is high toxic, endangers human health, has poor storage stability, short placed time, and flammable.Therefore, the existing type of Carl Fei test agent is a first -class flammable liquid, which has strict requirements for procurement, transportation, and storage, and is harmful to the health of users, which is not conducive to env...

Claims

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Application Information

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IPC IPC(8): G01N31/16
Inventor 顾学峰戴惠明
Owner JIANGSU YONGHUA FINE CHEM
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