Raman detection method of propylene glycol methyl ether acetate reaction liquid

Abstract

The invention relates to a Raman detection method for propylene glycol methyl ether acetate reaction liquid. The Raman detection method comprises the following steps: 1, sampling: extracting a propylene glycol methyl ether acetate reaction liquid sample with the volume of 1-3ml; and 2, Raman detection: carrying out ultrasonic mixing on the propylene glycol methyl ether acetate reaction liquid sample and the nanoparticle sol, and carrying out Raman spectrum detection after uniform mixing. The method has the advantages that 1, the operation is simple: the gas chromatography has strict operation standards and requirements, and the Raman spectrum detection only needs simple ultrasonic mixing in pretreatment; 2, rapidness and convenience: the gas chromatography generally needs 6-15 minutes, and the Raman spectrum detection and the pretreatment time of the method only need 2-3 minutes; 3, the accuracy is high: chromatographic peak trailing seriously affects content judgment, the Raman spectrum detects characteristic peaks, and the content can be intuitively and accurately calculated.

Description

Technical Field

[0001] The present invention relates to a detection method for propylene glycol methyl ether acetate reaction liquid, and particularly to a Raman detection method for propylene glycol methyl ether acetate reaction liquid. Background Art

[0002] Propylene glycol methyl ether acetate is a non-polluting solvent with multiple functional groups. It is mainly used as a solvent for inks, paints, ink, textile dyes, and textile oils, and can also be used as a cleaning agent in the production of liquid crystal displays; it is an excellent low-toxic high-grade industrial solvent with strong solubility for both polar and non-polar substances, and is suitable as a solvent for various polymers in high-grade coatings and inks, including amino methyl esters, vinyls, polyesters, cellulose acetates, alkyd resins, acrylic resins, epoxy resins, and nitrocelluloses, etc. Among them, propylene glycol methyl ether propionate is the best solvent in coatings and inks, and is suitable for unsaturated polyesters, polyurethane resins, acrylic resins, epoxy resins, etc.

[0003] Currently, the commonly used detection method is gas chromatography. The main components in the propylene glycol methyl ether acetate reaction liquid are propylene glycol methyl ether, propylene glycol methyl ether acetate, and acetic acid, as well as trace impurities and by-products. Due to the severe tailing of the acetic acid chromatographic peak, it is inaccurate to judge the content based on its peak area, resulting in a serious deviation in the composition of the overall reaction liquid. Summary of the Invention

[0004] In view of the above defects, the present invention provides a Raman detection method for propylene glycol methyl ether acetate reaction liquid, which meets the simple, rapid, border, and accurate detection requirements of propylene glycol methyl ether acetate reaction liquid through the surface enhancement effect of simply pretreating mixed nanoparticles.

[0005] Therefore, the technical solution adopted by the present invention is as follows: A Raman detection method for propylene glycol methyl ether acetate reaction liquid, comprising the following steps: The first step, sampling: extracting a sample of propylene glycol methyl ether acetate reaction liquid with a volume of 1 - 3 ml; The second step, Raman detection: ultrasonically mixing the above propylene glycol methyl ether acetate reaction liquid sample with nanoparticle sol, and performing Raman spectroscopy detection after mixing evenly.

[0006] As a further improvement of the above technical solution, the nanoparticle sol is one of gold, silver, copper, aluminum oxide, and silicon dioxide.

[0007] As a further improvement of the above technical solution, the volume ratio of the propylene glycol methyl ether acetate reaction liquid sample to the nanoparticle sol in the second step of Raman detection is 1:0.5 - 2.

[0008] The advantages of the present invention over the prior art are: 1. Simple operation: Gas chromatography has strict operation standards and requirements, while the Raman spectroscopy detection of the present invention only requires simple ultrasonic mixing for the pretreatment; 2. Fast and convenient: Gas chromatography usually takes 6 - 15 minutes, while the Raman spectroscopy detection of the present invention only takes 2 - 3 minutes including the pretreatment time; 3. High accuracy: Severe chromatographic peak tailing seriously affects the determination of content. The Raman spectroscopy detects characteristic peaks and can directly and accurately calculate the content. Specific embodiments

[0009] The technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without creative efforts shall fall within the protection scope of the present invention.

[0010] A Raman detection method for a propylene glycol methyl ether acetate reaction solution includes the following steps: The first step, sampling: Extract a sample of propylene glycol methyl ether acetate reaction solution with a volume of 1 - 3 ml; The second step, Raman detection: Ultrasonically mix the above propylene glycol methyl ether acetate reaction solution sample with a nanoparticle sol, and perform Raman spectroscopy detection after mixing evenly.

[0011] As a further improvement of the above technical solution, the nanoparticle sol is one of gold, silver, copper, alumina, and silica.

[0012] As a further improvement of the above technical solution, the volume ratio of the propylene glycol methyl ether acetate reaction solution sample to the nanoparticle sol in the second step of Raman detection is 1:0.5 - 2. Examples

[0013] Extract a sample of propylene glycol methyl ether acetate reaction solution with a volume of 1 - 3 ml; ultrasonically mix the propylene glycol methyl ether acetate reaction solution sample with a nanoparticle sol, and perform Raman spectroscopy detection after mixing evenly; prepare standard samples and calibration samples of propylene glycol methyl ether acetate reaction solution according to the mass ratios PM:PMA:HAC = 40:30:30, PM:PMA:HAC = 25:50:25, and PM:PMA:HAC = 60:0:40. Example 1

[0014] Take 1 mL of propylene glycol methyl ether acetate reaction solution and ultrasonically mix it evenly with 2 mL of gold nanoparticle sol, and perform Raman spectroscopy detection. The characteristic peaks are 638, 894, 1453, 1734 cm -1 .

[0015] After calculation, the mass ratios of the calibration samples are PM:PMA:HAC = 41:32:27, PM:PMA:HAC = 24:52:24, and PM:PMA:HAC = 61:0:39, respectively. Example 2

[0016] Take 1.5 mL of the propylene glycol methyl ether acetate reaction solution and ultrasonically mix it evenly with 1.5 mL of the gold nanoparticle sol, and perform Raman spectroscopy detection. The characteristic peaks are 638, 894, 1453, 1734 cm -1 .

[0017] After calculation, the mass ratios of the calibration samples are PM:PMA:HAC = 41:31:28, PM:PMA:HAC = 26:51:23, and PM:PMA:HAC = 60:0:40, respectively. Example 3

[0018] Take 1.5 mL of the propylene glycol methyl ether acetate reaction solution and ultrasonically mix it evenly with 1.5 mL of the silver nanoparticle sol, and perform Raman spectroscopy detection. The characteristic peaks are 638, 894, 1453, 1734 cm -1 .

[0019] After calculation, the mass ratios of the calibration samples are PM:PMA:HAC = 39:31:30, PM:PMA:HAC = 24:51:25, and PM:PMA:HAC = 60:0:40, respectively.

[0020] The above content is only an example and illustration of the concept of the present invention. Those skilled in the art of this technology can make various modifications or supplements to the described specific embodiments or use similar methods to replace them. As long as they do not deviate from the concept of the invention or exceed the scope defined by this claim book, they should all fall within the protection scope of the present invention.

Claims

1. A Raman detection method for propylene glycol methyl ether acetate reaction solution, characterized in that, It includes the following steps: The first step, sampling: extracting a propylene glycol methyl ether acetate reaction liquid sample with a volume of 1 - 3 ml; The second step, Raman detection: ultrasonically mixing the above propylene glycol methyl ether acetate reaction liquid sample with a nanoparticle sol, and performing Raman spectroscopy detection after mixing evenly.

2. The Raman detection method for the propylene glycol methyl ether acetate reaction solution according to claim 1, characterized in that, The nanoparticle sol is one of gold, silver, copper, alumina, and silica.

3. The Raman detection method for the propylene glycol methyl ether acetate reaction solution according to claim 1, characterized in that, In the second step, the volume ratio of the propylene glycol methyl ether acetate reaction liquid sample for Raman detection to the nanoparticle sol is 1:0.5 - 2.