Method for determining polymerization inhibitor in acrylic acid and derivatives thereof
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A technology of polymerization inhibitors and derivatives, applied in the field of analysis of organic chemical products, can solve problems such as environmental impact, strong corrosion, and odor stimulation
Inactive Publication Date: 2017-08-18
JIANGSU CHINA RAILWAY ARIT NEW MATEIRALS CO LTD
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However, glacial acetic acid has strong volatility, strong corrosiveness, and irritating smell, which has a great impact on the environment, has certain harm to the body of workers, and causes certain corrosion to instruments.
[0004] Lu Junliang et al. used acidified ethanol instead of glacial acetic acid to measure the polymerization inhibitor p-hydroxyanisole (MEHQ) in industrial acrylic acid and acrylate esters, but ethanol also has strong volatility and strong deliquescence, so it can be quickly deliquescent. Moisture is absorbed in the air, which is easy to cause errors in the experiment
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Embodiment 1
[0016] 1) Prepare acidic isopropanol solution: the volume ratio of isopropanol (AR) to 6mol / L hydrochloric acid solution is 1:0.3.
[0017] 2) Preparation of standard solution: Weigh 0.1000g MEHQ into a 100mL volumetric flask filled with 50mL of acidic isopropanol. Mix well to dissolve it completely, and dilute to the mark with acidic isopropanol to prepare a standard solution.
[0018] 3) Preparation method of sodium nitrite solution: dissolve 2 g of sodium nitrite in water and dilute to 100 mL.
[0019] 4) Drawing of the working curve: Draw 1, 2, 4, 6 and 10mL of standard solutions, pour them into 50mL volumetric flasks respectively, dilute each to the mark with acidic isopropanol, and mix thoroughly. Take 10mL of standard solutions from each of these standard solutions in turn and place them in 50mL volumetric flasks filled with about 20mL of acidic isopropanol, add 2mL of sodium nitrite solution, and dilute to the mark with acidic isopropanol. Mix well and let stand for ...
Embodiment 2
[0024] 1) Prepare acidic isopropanol solution: the volume ratio of isopropanol (AR) to 6mol / L hydrochloric acid solution is 1:0.4.
[0025] 2) Preparation of standard solution: Weigh 0.1000g TBHQ into a 100mL volumetric flask filled with 50mL of acidic isopropanol. Mix well to dissolve it completely, and dilute to the mark with acidic isopropanol to prepare a standard solution.
[0026] 3) Preparation method of sodium nitrite solution: dissolve 2 g of sodium nitrite in water and dilute to 100 mL.
[0027] 4) Drawing of the working curve: Draw 1, 2, 4, 6 and 10mL of standard solutions, pour them into 50mL volumetric flasks respectively, dilute each to the mark with acidic isopropanol, and mix thoroughly. Take 10mL of standard solutions from these standard solutions in turn, place them in 50mL volumetric flasks filled with about 20mL of acidic isopropanol, add 2.5mL of sodium nitrite solution, and dilute to the mark with acidic isopropanol. Mix well and let stand for 10min. U...
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Abstract
The invention discloses a method for determining a polymerization inhibitor in acrylic acid and derivatives thereof. The method is mainly used for determining the polymerization inhibitor 4-metoxyphenol (MEHQ) or hydroquinone (TBHQ) in acrylic acid and derivatives thereof. The method comprises the following steps: firstly, weighting a certain amount of polymerization inhibitor, placing into an acidic isopropanol solution and preparing into a standard solution; then, drawing a working curve for the polymerization inhibitor content on the basis of the absorbance of the standard solution in a specific wavelength; adding a sodium nitrite solution into a sample, and diluting with acidic isopropanol till reaching a constant volume; taking acidic isopropanol as blank, and determining the solution at the specific wavelength; and finding the content of the polymerization inhibitor corresponding to the acquired absorbance from the working curve. The acidic isopropanol is used as the solvent according to the method; and the method has the characteristics of simplicity, convenience, accuracy, less environmental pollution, less pungent odor, and the like.
Description
technical field [0001] The invention relates to a method for measuring polymerization inhibitors in acrylic acid and its derivatives, belonging to the technical field of organic chemical product analysis. Background technique [0002] Polymerization inhibitor 4-methoxyphenol and hydroquinone are commonly used polymerization inhibitors in unsaturated monomer acrylic acid and its derivatives, which can prevent or slow down the polymerization of unsaturated monomers during storage. A small amount (mass ratio concentration < 0.03%) of this kind of polymerization inhibitor exists in acrylic acid and its derivatives, which generally does not affect the subsequent use of unsaturated monomers. Unsaturated monomers are unstable during storage and transportation, and are easily affected by storage and transportation conditions to cause quality changes, resulting in product quality reduction or unqualified, so polymerization inhibitors play a role in the storage of polymer monomers....
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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/31
CPCG01N21/31
Inventor 李梦婷朱桃姜海东郑春扬郭兆来
Owner JIANGSU CHINA RAILWAY ARIT NEW MATEIRALS CO LTD
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