A kind of determination method of p-hydroxyanisole in acrylate reactive diluent

A technology of p-hydroxyanisole and active diluent, which is applied in the field of printed matter, can solve problems such as odor stimulation, no visible measurement, influence of chromatographic column and gas path, etc., and achieve good repeatability

Active Publication Date: 2018-03-20
LUCKY HUAGUANG GRAPHICS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The detection method of polymerization inhibitor MEHQ has a lot, such as gas chromatography, liquid chromatography, ultraviolet spectrometry etc., has document disclosed to use capillary gas chromatography, analyzes polymerization inhibitor (MEHQ) content method in acrylonitrile, this The sample described in the literature is MEHQ in acrylonitrile, and the sample described in this patent is an acrylate reactive diluent. The active components in the sample are likely to affect the chromatographic column and the gas path, so this method cannot be directly used; The content of MEHQ was determined by ultraviolet spectrometry, using NaNO 2 , carried out in an acidic environment, but for the acrylate reactive diluent system, MEHQ cannot produce color reaction; the national standard GB / T17530.5-1998 stipulates the determination of the inhibitor p-hydroxyanisole in industrial acrylic acid and propylene ester method, using NaNO 2 As a color developer, glacial acetic acid is used as a solvent. Because glacial acetic acid has strong volatility, strong corrosiveness, and irritating odor, it has a great impact on the environment, has certain harm to the worker's body, and causes certain corrosion to the instrument. The target samples analyzed are different, and this standard is also not suitable for the determination of acrylate reactive diluent systems; NaNO 2 -Al(NO 3 ) 3 The system is often used to determine the total phenolic acid content in Chinese herbal medicines, but it has not been used for the determination of MEHQ in diluents

Method used

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  • A kind of determination method of p-hydroxyanisole in acrylate reactive diluent
  • A kind of determination method of p-hydroxyanisole in acrylate reactive diluent
  • A kind of determination method of p-hydroxyanisole in acrylate reactive diluent

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Embodiment 1

[0031] A kind of assay method of p-hydroxyanisole in acrylate reactive diluent, comprises the following steps:

[0032] (1) Drawing of standard curve

[0033] A. take p-hydroxyanisole standard substance and be dissolved in volume percent concentration and be 70% ethanol aqueous solution, be diluted into the standard solution that concentration is 40ppm;

[0034] B. Sequentially draw 0.5mL, 1.0mL, 1.5mL, 2.0mL and 2.5mL of the above-mentioned standard solution with a concentration of 40ppm, place them in a 25mL volumetric flask respectively, first add 1.2mL of 10wt% sodium nitrite aqueous solution, and shake well; then Add 2mL of 10wt% aluminum nitrate aqueous solution, shake well, and stand in the dark for 5min at room temperature; finally add 7.5mL of 2.0mol / L sodium hydroxide solution, dilute with 70% ethanol aqueous solution to the mark and shake well. Stand in the dark for 10 minutes at room temperature;

[0035] C. Blank control sample solution: sequentially add 1.2mL o...

Embodiment 2

[0040]The similarities between this example and Example 1 will not be repeated, the difference lies in the determination of the sample in step (2):

[0041] Use a pipette to measure 1.0 mL of diethylene glycol diacrylate sample and place it in a 25 mL volumetric flask, first add 1.2 mL of 10 wt % sodium nitrite aqueous solution, and shake well; then add 2 mL of 10 wt % aluminum nitrate aqueous solution, shake well, Stand at room temperature in the dark for 5 minutes; finally add 7.5 mL of 2.0 mol / L alkaline solution, dilute with 70% ethanol aqueous solution to the scale and shake well, and keep in the dark for 10 minutes at room temperature; , measure the absorbance of the solution at a wavelength of 463nm, and figure 1 Compared with the standard curve, the content of p-hydroxyanisole in the diethylene glycol diacrylate reactive diluent is 448.3ppm.

Embodiment 3

[0043] The similarities between this example and Example 1 will not be repeated, the difference lies in the determination of the sample in step (2):

[0044] Use a pipette to measure 1.0 mL of benzyl glycidyl ether acrylate sample and place it in a 25 mL volumetric flask, first add 1.2 mL of 10 wt % sodium nitrite aqueous solution, and shake well; then add 2 mL of 10 wt % aluminum nitrate aqueous solution, shake well, Stand at room temperature in the dark for 5 minutes; finally add 7.5 mL of 2.0 mol / L alkaline solution, dilute with 70% ethanol aqueous solution to the scale and shake well, and keep in the dark for 10 minutes at room temperature; , measure the absorbance of the solution at a wavelength of 463nm, and figure 1 Compared with the standard curve, the content of p-hydroxyanisole in the benzyl glycidyl ether acrylate reactive diluent was 384.2ppm.

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Abstract

The invention relates to a method for measuring p-hydroxyanisole in acrylate reactive diluents. It draws a certain amount into a standard volumetric flask, and first adds a certain amount of 5-15wt% sodium nitrite aqueous solution, shakes well; then adds a certain amount 5-15wt% aluminum nitrate aqueous solution, shake well, and stand in the dark for 3-6 minutes at room temperature; finally add a certain amount of 1.5-2.5mol / L alkaline solution, dilute to the mark with a volume percentage concentration of 70% ethanol solution, and shake well. Stand at room temperature in the dark for 5-10 minutes; select the following blank control sample solution for comparison, use a 1cm cuvette, measure the absorbance of the standard solution at a wavelength of 463nm, draw a standard curve, and calculate the p-hydroxybenzoic acid in the acrylate reactive diluent ether content. The method of the invention has the advantages of low cost, rapidity, accuracy and the like.

Description

technical field [0001] The invention belongs to the technical field of printed matters, and in particular relates to a method for determining p-hydroxyanisole in acrylate reactive diluents. Background technique [0002] Reactive diluent, also known as functional monomer, is a small organic molecule containing polymerizable functional groups. It is an important component in the formulation of photocurable coatings, photoresists, and paints. It not only has the function of dissolving and diluting oligomers and adjusting the viscosity of the system, but also participates in photosensitive polymerization, affecting the photocuring speed and various properties of the cured film, such as hardness, wear resistance, adhesion, flexibility and other physical and mechanical properties. performance etc. [0003] From the perspective of reactive diluent structure, free radical reactive diluents are all monomers with C=C unsaturated double bonds, such as acryloyloxy, methacryloyloxy, vin...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N21/31
Inventor 王凤兰晓丽王怀功王盼马晓丽张玉娜黄剑莉陆金荣
Owner LUCKY HUAGUANG GRAPHICS
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