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A technology of diaminotoluene and a detection method is applied in the detection field of diaminotoluene isomers, which can solve the problems of inability to detect the isomer ratio, inability to meet product detection and separation requirements, and not representing the true quality of products.
Inactive Publication Date: 2015-12-02
四川北方红光特种化工有限公司
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[0002] Diaminotoluene, referred to as TDA, is currently used to detect its isomers by gas chromatography. There is only one main peak in the detection, and the six isomers of TDA cannot be completely separated. For 80 / 20TDA and 20 / 80TDA The isomer ratio cannot be detected, that is to say, 2,6-TDA and 2,4-TDA cannot be completely separated, only the total mass fraction can be detected, and the isomer ratio cannot be calculated, and the isomer ratio cannot be accurately detected. Whether the composition ratio meets the requirements of process control and customers
At the same time, for a single product 2,6-TDA or 2,4-TDA, because the two cannot be separated, then our analysis result can only be the sum of the two, and the mass fraction of each component cannot be detected, then our analysis result is not Does not represent the true quality of the product
The previous analytical method can only detect the total amount of 2,6-TDA and 2,4-TDA, and cannot separate 2,3-TDA from 3,4-TDA, which cannot meet the detection and separation requirements of high-standard enterprises for products
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Embodiment 1 2
[0022] The detection method of embodiment 1 diaminotoluene isomer
[0023] The detection method of diaminotoluene isomers is determined by gas chromatography, comprising the following steps:
[0024] (1) get the diaminotoluene isomers to be tested;
[0025] (2) Inject the test sample into the gas chromatograph, wherein the chromatographic conditions are as follows:
[0026] Chromatographic column: polyethylene glycol (PEG) gas-phase capillary column, a CAM column produced by Agilent, with a specification of 15m*0.25mm*0.25um;
[0027] Carrier gas: N 2 , the front pressure of the column is 0.1MPa;
[0028] Column temperature conditions: initial temperature 130°C, keep for 5 minutes, heating rate 10°C / min, final temperature 200°C, keep for 20 minutes;
[0031] According to the detection conditions of this example, for the analysis of...
Embodiment 2
[0038] According to the detection conditions of Example 1, for the analysis of 20 / 80TDA (i.e. the diaminotoluene isomer mixture of 20% 2,4-TDA and 80% TDA), its separation spectrum is shown in figure 2 , and the analysis results are shown in Table 3 and Table 4.
[0039] table 3
[0040]
[0041] Table 420 / 80TDA Analysis Results
[0042]
Embodiment 3
[0044] According to the detection conditions of Example 1, the 2,4-TDA product is analyzed, and its separation spectrum is shown in image 3 , the analysis results are shown in Table 5 and Table 6.
[0045] table 5
[0046]
[0047] Table 62,4-TDA Analysis Results
[0048]
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Abstract
The invention discloses a detection method of a diaminotoluene (TDA) isomer. The diaminotoluene isomer is determined by adopting a gas chromatographic method. The detection method comprises the following operation steps: (1), obtaining a to-be-detected diaminotoluene isomer test product; and (2), injecting the test product in a gas chromatograph, wherein chromatographic conditions are as follows: a chromatographic column is a polyethylene glycol (PEG) gas-phase capillary-column chromatographic column, a carrier gas is N2, and the starting column pressure is 0.1MPa, column temperature conditions are as follows: the initial temperature is 130 DEG C, and is kept for 5min, the temperature rise rate is 10 DEG C / min, the final temperature is 200 DEG C and is kept for 20min, the temperature of a vaporizing chamber is 250-280 DEG C, an adopted detector is a flame ionization detector (FID), and the detection temperature is 250-280 DEG C. The detection method disclosed by the invention relates to purities of six isomer monomers of TDA and content analysis of all components of a mixture of the six isomer monomers of the TDA, and the minimum detectable quantity reaches 0.001 percent; meanwhile, six isomers of the TDA can be effectively separated and detected, and thus a TDA production device can continuously and stably run for a long time.
Description
technical field [0001] The invention relates to a method for detecting isomers, in particular to a method for detecting diaminotoluene isomers. Background technique [0002] Diaminotoluene, referred to as TDA, is currently used to detect its isomers by gas chromatography. There is only one main peak in the detection, and the six isomers of TDA cannot be completely separated. For 80 / 20TDA and 20 / 80TDA The isomer ratio cannot be detected, that is to say, 2,6-TDA and 2,4-TDA cannot be completely separated, only the total mass fraction can be detected, and the isomer ratio cannot be calculated, and the isomer ratio cannot be accurately detected. Whether the composition ratio meets the process control and customer requirements. At the same time, for a single product 2,6-TDA or 2,4-TDA, because the two cannot be separated, then our analysis result can only be the sum of the two, and the mass fraction of each component cannot be detected, then our analysis result is not Does not ...
Claims
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