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Method for measuring mass fraction of imine-methyl ether hydrochloride
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A technology of iminomethyl ether hydrochloride and mass fraction, which is applied in the direction of chemical analysis by titration, can solve the problem of inability to accurately determine the mass fraction of iminomethyl ether hydrochloride, unstable iminomethyl ether hydrochloride, and inaccurate Determination of mass fraction and other issues to achieve the effect of simple operation, improved yield and quality, and high precision
Inactive Publication Date: 2014-07-16
CHONGQING UNISPLENDOUR CHEM
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[0003] Iminomethyl ether hydrochloride is unstable at room temperature, and it is easy to decompose when it sees water, so it is difficult to analyze and detect it
There is a method for determining the mass fraction of iminomethyl ether by measuring the total chlorine in the iminomethyl ether hydrochloride sample, but because iminomethyl ether hydrochloride is synthesized with excess hydrogen chloride, the isolated Hydrogen chloride is attached to the sample, and the chlorine in hydrogen chloride is also measured at the same time, which makes the measurement result higher. Therefore, this method cannot accurately determine the mass fraction of iminomethyl ether hydrochloride in the sample, and the measurement result is also unstable.
Another method is to determine the iminomethyl ether mass fraction by measuring the total nitrogen content in the iminomethyl ether hydrochloride sample, but because there is an excessive amount of methyl alcohol in the iminomethyl ether hydrochloride synthesis, it will inevitably occur A small amount of alcoholysis reaction occurs to generate ammonium chloride by-product, and the nitrogen in ammonium chloride is measured at the same time, which makes the measurement result higher and cannot accurately determine the mass fraction of iminomethyl ether hydrochloride in the sample.
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Embodiment 1
[0033] Embodiment 1, a kind of method for measuring iminomethyl ether hydrochloride mass fraction comprises the following steps,
[0034] 1) Prepare anhydrous mercury acetate solution, perchloric acid standard titration solution and crystal violet indicator solution;
[0035] Mercury acetate solution: take 5g of mercury acetate, add glacial acetic acid to dissolve and dilute to 100mL;
[0036] Perchloric acid standard titration solution: Take 750mL of anhydrous glacial acetic acid, add 8.5mL of perchloric acid, shake well, add 23mL of acetic anhydride dropwise while stirring, shake while adding, shake evenly after adding, let cool , add anhydrous glacial acetic acid to 1000mL;
[0037] Crystal violet indicator solution: Weigh 0.50 g of crystal violet, dissolve in glacial acetic acid, and dilute to 100 mL with glacial acetic acid.
[0038] 2) Calibrate perchloric acid standard titration solution: take standard potassium hydrogen phthalate dried at 105°C to constant weight, we...
Embodiment 2
[0062] Example 2, a method for measuring the mass fraction of iminomethyl ether hydrochloride, the batch number is 2009016, see Example 1 for the experimental procedure, the amount of anhydrous formic acid is 5mL, the amount of glacial acetic acid is 30mL, the amount of mercuric acetate solution is 7mL, repeat The experiment was performed 5 times, and the experimental data are shown in Table 3.
[0063] Table 3 Experimental data of embodiment 2 of the present invention
[0064]
Embodiment 3
[0065] Example 3, a method for determining the mass fraction of iminomethyl ether hydrochloride, the batch number is 2009020, see Example 1 for the experimental procedure, the sample size is 0.1654g, the amount of anhydrous formic acid is 4mL, the amount of glacial acetic acid is 30mL, mercury acetate The solution volume was 6 mL. The actual concentration of perchloric acid standard titration solution is 0.1024mol / L, the volume of perchloric acid standard titration solution consumed by titration sample is 15.55mL, and the volume of perchloric acid standard titration solution consumed by blank test is 0.10mL.
[0066] Calculation result: w=91.35%
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Abstract
The invention relates to a method for measuring the mass fraction of imine-methyl ether hydrochloride, which is characterized in that firstly, dissolving an imine-methyl ether hydrochloride sample into anhydrous formic acid, adding glacial acetic acid, and then adding mercuric acetate to perform a reaction with the imine-methyl ether hydrochloride so as to ensure hydrochloric acid in the imine-methyl ether hydrochloride to generate mercuric chloride difficult to ionize; then titrating imine-methyl ether hydrochloride solution by using perchloric acid standard titration solution as titrant; and according to the concentration and the using amount of the perchloric acid standard titration solution and the using amount of the imine-methyl ether hydrochloride sample, calculating the mass fraction of the imine-methyl ether hydrochloride in the sample, wherein the reaction is performed in anhydrous solution. According to the method, not only is the interference of the hydrochloric acid and ammonium chloride removed and are the accuracy and the stability of a measuring result improved, but also the method has high precision and is simple, convenient and rapid to operate, the working efficiency is improved and the method has important significance for optimizing the trimethyl orthoformate synthesis conditions and improving the yield and the quality of trimethyl orthoformate.
Description
technical field [0001] The invention relates to a method for measuring the mass fraction of iminomethyl ether hydrochloride. Background technique [0002] Iminomethyl ether hydrochloride is an intermediate in the synthesis of trimethyl orthoformate by hydrocyanic acid method, which is produced by the reaction of hydrocyanic acid with excess hydrogen chloride and methanol. Trimethyl orthoformate is an important intermediate in organic synthesis, widely used in the synthesis of medicines, pesticides and spices. The quality of imidomethyl ether hydrochloride directly affects the yield and the quality of trimethyl orthoformate, therefore, the mensuration of imidomethyl ether hydrochloride massfraction, to optimizing trimethyl orthoformate synthesis condition, improves yield and quality has important meaning. [0003] Iminomethyl ether hydrochloride is unstable at room temperature and easily decomposes in water, so it is difficult to analyze and detect it. There is a method fo...
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