Method for stably detecting moisture in chloroalkene

A chlorinated olefin, stable detection technology, applied in the field of chemical analysis and detection, can solve the problems of electrolyte failure and small value of analysis results, and achieve the effect of improving stability

Inactive Publication Date: 2020-08-25
常州新东化工发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The Karl Fischer method calculates the water content based on the electricity consumed by the quantitative redox reaction between iodine and water, so a small amount of oxidizing substances in chlorinated olefins will oxidize iodide ions in the Karl Fischer reagent, resulting in "overheating" of the analytical instrument. Iodine phenomenon", resulting in smaller and smaller analysis results, and eventually the electrolyte will fail

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Add p-methoxyphenol stabilizer to the 1,1,2,3-tetrachloropropene material sample to be tested, and store in a nitrogen seal at low temperature; After adding the p-methoxyphenol stabilizer, the concentration of the stabilizer is 500ppm; the Karl Fischer moisture analyzer is placed in a glove box, and the glove box is filled with nitrogen for circulation treatment; the nitrogen is dehydrated through 4A molecular sieve desiccant , and carry out deoxidation treatment, the water content is 5ppm, and the oxygen content is 8ppm; after adding pure water for electrolysis, the weight loss method is sampled three times, and the moisture detection values ​​are 144.9μg, 146.2μg, and 145.8μg, respectively. The relative error between the measured values 0.9%.

Embodiment 2

[0032] Add p-methoxyphenol and p-tert-amylphenol mixed stabilizer to the 1,1,2,3-tetrachloropropene material sample to be tested, and store at low temperature in a nitrogen seal; -After adding the mixed stabilizer of p-methoxyphenol and p-tert-amylphenol to the tetrachloropropene material sample, the concentration of the stabilizer is 400ppm; the ratio of p-methoxyphenol and p-tert-amylphenol is 3:1; The Fischer moisture analyzer was placed in a glove box, which was filled with nitrogen for circulation treatment; the nitrogen was dehydrated by 4A molecular sieve desiccant, and deoxygenated, with a water content of 2ppm and an oxygen content of 10ppm; After the water electrolysis was balanced, the weight loss method was sampled three times, and the moisture detection values ​​were 256.3 μg, 253.7 μg, and 258.1 μg, respectively, and the relative error between the measured values ​​was 1.7%.

Embodiment 3

[0034] Add p-methoxyphenol stabilizer to the 1,1,3-trichloropropene material sample to be tested, and store it under a nitrogen seal at low temperature; add p-methoxyl After the base phenol stabilizer, the concentration of the stabilizer was 600 ppm; the Karl Fischer moisture analyzer was placed in a glove box, and the glove box was filled with nitrogen for circulation treatment; the nitrogen was dehydrated by 4A molecular sieve desiccant, and removed Oxygen treatment, the water content is 2ppm, and the oxygen content is 10ppm; after adding pure water for electrolysis, the weight loss method is sampled three times, and the moisture detection values ​​are 89.3μg, 90.2μg, and 89.8μg, respectively. The relative error between the measured values ​​is 1.0%.

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Abstract

The invention provides a method for stably detecting moisture in chloroalkene, which comprises the following steps: a stabilizer is added into a chloroalkene sample to be detected, and low-temperaturelightproof nitrogen sealing preservation is carried out; the moisture meter is placed in a glove operation box, and inert gas circulation treatment is adopted in the glove operation box; after electrolytic equilibrium of the moisture meter, the water content in the chlorinated olefin sample is measured; preferably, the stabilizing agent is p-methoxyphenol; inert gas in the glove operation box issubjected to drying dehydration and deoxygenation treatment. According to the present invention, the anti-oxidative decomposition stabilizer is added to the chloroalkene sample to be detected, and thelow-temperature light-shielding nitrogen sealing storage is performed, such that the stability of the chloroalkene sample to be detected can be improved so as to accurately analyze the moisture in the chloroalkene; through verification, the method for stably detecting the moisture in the chloroalkene is accurate in moisture content determination, small in relative error, simple to operate and good in repeatability, and can be widely applied to determination of the moisture in the chloroalkene.

Description

technical field [0001] The invention belongs to the technical field of chemical analysis and detection, and in particular relates to a method for the stability detection of moisture in chlorinated olefins. Background technique [0002] Chlorinated olefins include chloroethylene, chloropropene, etc. Among them, 1,1,3-trichloropropene and 1,1,2,3-tetrachloropropene in chloropropene are synthetic new environmentally friendly refrigerants 2,3, An important intermediate of 3,3-tetrafluoropropene (HFO-1234yf), with the emergence of ozone depletion and global warming, HFO-1234yf as a new environmentally friendly refrigerant will gradually replace chlorofluorocarbons CFCs and hydrochlorofluorocarbons Hydrocarbon HCFC. [0003] Moisture content is an important indicator in the finished product of chlorinated propylene, but α chlorine in chlorinated propylene is relatively active due to p-π conjugation, and usually does not contain stabilizer 1,1,2,3-tetrachloropropene, 1 ,1,3-Trich...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N31/16
CPCG01N31/168
Inventor 吴发明姚迪张驰孙运林马凯刘向超朱成明董亮陶文平王顺利
Owner 常州新东化工发展有限公司
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