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Establishment of QC for Systhetic Process of Ethyl Difluoroacetoacetate (DFAAE)

Author: FangFang
Tutor: WangLiMin；ZhangTao
School: East China University of Science and Technology
Course: Industry Technology and Engineering
Keywords: Chlorodifluoroacetic acid Ethyl difluoroacetate Ethyl Difluoroacetoacetate Pesticides Quality control system
CLC: TQ225.241
Type: Master's thesis
Year: 2011
Downloads: 183
Quote: 0
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Abstract


Ethyl Difluoroacetoacetate is an important material to synthetise 3-difluoromethyl-4-pyrazole carboxylic acid esters---an important intermediate for the manufacture of pyrazole carboxanilide pesticides. In order to obtain high-purity product, the raw material, intermediate product and final product should be well controlled during the synthetic process. After a series of experiments, synthetic process was established to produce Ethyl Difluoroacetoacetate, which employed industrial waste Chlorodifluoroacetic acid (C1DFA) as starting material. The lab achievement has been applied into the pilot plant, which confirmed that the process is not only economical but also environment-friendly.In order to well control the process, this paper set up a quality control (QC) system for the synthetic process of Ethyl Difluoroacetoacetate (DFAAE). According to this system, the chemical purity of raw material CDFA is analyzed by Ion Chromatography (IC). The purity of DFAE and DFAAE are analyzed by Gas Chromatography (GC). Through comparison of different testing conditions, the optimal analytical conditions were determined. The result also verified by NMR and GCMS. All the test methods are validated by linearity, repeatability, detection limit. Test method also assessment by six sigma methodology according to internationally accepted quality management. The practice of the pilot plant indicated that the QC system can accurately and efficiently control the production of Ethyl Difluoroacetoacetate (DFAAE).

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CLC: > Industrial Technology > Chemical Industry > Basic Organic Chemistry Industry > The production of aliphatic compounds ( acyclic compounds) > Aliphatic carboxylic acid and its derivatives > Carboxylic acid derivatives of the function > Ester > Yuan ester
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