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Method for detecting functional monomers in solvent type acrylic resin

An acrylic resin and functional monomer technology, applied in the field of chemical analysis, can solve the problems of not easy to produce peaks, cover, and add less amount, and achieve the effect of less sample dosage, good repeatability and small relative standard deviation

Active Publication Date: 2020-04-21
上海微谱检测科技集团股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the functional monomers are mainly characterized by PGC, but because most of the functional monomers are polar monomers, the peaks are not easy to appear on PGC, and the addition amount is small, which is easily covered by other peaks, and often the functional monomers cannot be detected In some cases, some customers even reported that they added 5% hydroxyl monomers to the resin, but the PGC failed to detect them.
Quantitative results are mainly calculated by titration, such as hydroxyl value, acid value and other test results. At present, the titration results are very unstable, and the accuracy of titration has not been verified.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0062] The preparation step of standard sample in step (1) of the present invention is: in the four-neck flask that condenser, agitator, thermometer and constant pressure funnel are housed, add 1 / 2 basic monomer, functional monomer and 1 / 2 3 solvent, then add 1 / 3 initiator, stir evenly, heat up to 80-85°C, react for 0.5-1h, titrate the mixed solution of remaining basic monomer, initiator and remaining solvent, keep warm for 3-5h after dropping, cool down To 50 ~ 60 ℃, discharge the standard sample.

[0063] During the preparation of the standard sample, the applicant found that when the concentration of basic monomers was too high at the initial stage, the internal solution would boil and reflux violently, and the solid content test of the synthesized resin would meet the standard, but the viscosity was too high, which was not conducive to the next step of detection and analysis. . When controlling to add 1 / 2 basic monomer, functional monomer, 1 / 3 solvent and 1 / 3 initiator at...

Embodiment 1

[0082] Embodiment 1 of the present invention provides the detection method of functional monomer in solvent type acrylic resin, comprises the following steps:

[0083] (1) Add the main monomer and functional monomer into the solvent, then add the initiator, heat up to 85°C, react for 0.5h, keep warm, cool down and discharge to obtain a standard sample;

[0084] (2) Place the standard sample in an oven at 160°C for 4 hours, and then send it to a pyrolysis gas chromatography / mass spectrometer for data determination;

[0085] (3) Calculate the relative correction factor of the functional monomer by the peak area of ​​the main monomer and the functional monomer measured;

[0086] (4) According to the peak area of ​​the functional monomer to be tested, the content of the functional monomer to be tested is calculated by the average relative correction factor.

[0087] The basic monomers include methyl methacrylate and butyl acrylate; the mass ratio of methyl methacrylate and butyl ...

Embodiment 2

[0106] Embodiment 2 of the present invention provides the detection method of functional monomer in solvent type acrylic resin, comprises the following steps:

[0107] (1) Add the main monomer and functional monomer into the solvent, then add the initiator, heat up to 85°C, react for 0.5h, keep warm, cool down and discharge to obtain a standard sample;

[0108] (2) Place the standard sample in an oven at 160°C for 4 hours, and then send it to a pyrolysis gas chromatography / mass spectrometer for data determination;

[0109] (3) Calculate the relative correction factor of the functional monomer by the peak area of ​​the main monomer and the functional monomer measured;

[0110] (4) According to the peak area of ​​the functional monomer to be tested, the content of the functional monomer to be tested is calculated by the average relative correction factor.

[0111] The basic monomers include methyl methacrylate and butyl acrylate; the mass ratio of methyl methacrylate and butyl ...

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Abstract

The invention relates to the field of chemical analysis, and particularly provides a method for detecting functional monomers in solvent type acrylic resin. The method is characterized by comprising the following steps: (1) adding a basic monomer and a functional monomer into a solvent, adding an initiator, making reaction, keeping the temperature, and carrying out cooling and discharging to obtain a standard sample; (2) drying a standard sample, sending the standard sample into a pyrolysis gas chromatograph / mass spectrometer, and carrying out data determination; (3) calculating a relative correction factor of the functional monomer according to the measured peak areas of the main monomer and the functional monomer; and (4) according to the peak area of the functional monomer to be detected, calculating the content of the functional monomer to be detected by the average relative correction factor.

Description

technical field [0001] The invention relates to the field of chemical analysis, and more specifically, the invention provides a detection method for functional monomers in solvent-type acrylic resins. Background technique [0002] According to different application fields, solvent-based acrylic resins often add various functional monomers to modify the resin. Usually, the amount of functional monomers added is less than 2%, but it will have a great impact on the performance of the resin. The main function is to introduce special functional groups. The common modified functional groups are: carboxyl group, which can significantly improve the cohesive strength of the resin, hydroxyl group, which can improve the adhesion to polar substrates, introduce post-curing crosslinking points, etc., and ring Oxygen, amides, etc., are key components for resin synthesis and performance adjustment. Many large synthetic companies with rich product experience often focus on modified function...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
CPCG01N30/88G01N2030/025G01N2030/884
Inventor 胡亚吴杰贾梦虹覃国飞
Owner 上海微谱检测科技集团股份有限公司
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