Detection method of chlorine content in 2-ethylanthraquinone

Abstract

The invention discloses a detection method of the chlorine content in 2-ethylanthraquinone. The detection method comprises the following steps of 1) preparing an organic chlorine standard solution; 2)preparing a sample, and weighing about 4 micrograms of sample in a sample weighing cup with an analysis scale; 3) putting the sample on a micro-coulometry sulfur-chlorine determinator for detection,wherein integration resistance of a data workstation of the micro-coulometry sulfur-chlorine determinator is equal to 1 K, and the amplification factor is equal to 2000; 4) calculating an average conversion rate; and 5) sending the sample into the micro-coulometry titrator for determination by using a solid sample feeding boat. In the detection method, as the feeding quantity required for detection is small and is less than 4 micrograms, the detection cost can be reduced, and the detection speed is increased. The practical application discovers that the detection method is short in detection time, good in data stability and simpler in operation compared with the prior art and can lower the labor intensity of detecting personnel.

Description

Technical field: [0001] The invention relates to the technical field of detection methods for chemical reagents, in particular to a detection method for chlorine content in 2-ethylanthraquinone. Background technique: [0002] 2-Ethylanthraquinone is synthesized by acylation reaction using ethylbenzene and phthalic anhydride as raw materials, chlorobenzene as solvent, and catalyzed by anhydrous aluminum trichloride. Due to the use of chlorobenzene and anhydrous aluminum trichloride in the reaction raw materials, the finished product inevitably contains chloride ions. Although it has been purified through multiple processes, the finished product still contains trace amounts of chloride ions. 2-Ethylanthraquinone products are mainly produced with hydrogen peroxide. The hydrogenation catalyst palladium catalyst produced by hydrogen peroxide is very sensitive to chloride ions. Trace amounts of chloride ions can easily cause the hydrogenation catalyst palladium catalyst to lose it...

AI Technical Summary

Problems solved by technology

Since chlorobenzene and anhydrous aluminum trichloride are used in the reaction raw materials, the finished product inevitably contains chloride ions. Although it has been purified through multiple processes, the finished product still contains trace amounts of chloride ions

2-Ethylanthraquinone products are mainly produced with hydrogen peroxide. The hydrogenation catalyst palladium catalyst produced by hydrogen peroxide is very sensitive to chloride ions. Trace amounts of chloride ions can easily cause the hydrogenation catalyst palladium catalyst to lose its activity, seriously affecting the normal production of hydrogen peroxide.

[0003] 1. 2-Ethylanthraquinone is detected by the method stipulated in the national standard GB / T23672-2009, and an appropriate amount of sample is put into a porcelain crucible, and after being carbonized on a discharge furnace, it is then put into a high-temperature furnace for burning treatment, and then according to GB / T23672-2009 The specified colorimetric method in T9728 is used for detection. There are many deficiencies in this detection method. Because 2-ethylanthraquinone products contain two kinds of chloride ions in organic and inorganic states, carbonization and burning treatment will cause organic chloride ions Decomposition, affecting the accuracy of detection data

In addition, because the detection method is cumbersome to operate, the detection time is long, and the data stability is poor, it is not suitable for this detection

[0004] 2. The test method recommended by FMC Company of the United States is to put an appropriate amount of sample into a combustion cup, put it into a closed oxygen bomb, and ignite it in pure oxygen to convert chloride ions into hydrogen chloride. After absorption treatment, according to GB / T9728 There are many deficiencies in this detection method. Since the 2-ethylanthraquinone product is a solid sample, it must be ignited with an ignition wire. The oxygen bomb is a high-pressure container, and its equipment is cumbersome. During the process, the ignition wire is easy to loose, resulting in successful ignition or incomplete combustion, which affects the accuracy of detection data

This method also has poor repeatability of detection data, long detection time, and cumbersome detection process.