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Separation and detection method of dipropylene glycol isomeride

A technology for reducing dipropylene glycol and isomers, which is applied in the field of analysis and detection, and can solve the problems of separate quantitative research and difficult separation of various isomers

Pending Publication Date: 2022-04-22
JIANGSU MAYSTA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The similarity of structures and physical and chemical properties of various isomers determines that they are difficult to separate. At present, the content detection of dipropylene glycol is to detect the total amount of all isomers, and the various isomers are not analyzed. Individual Quantitative Study

Method used

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  • Separation and detection method of dipropylene glycol isomeride
  • Separation and detection method of dipropylene glycol isomeride
  • Separation and detection method of dipropylene glycol isomeride

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Experimental program
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preparation example Construction

[0035] (2) preparation of the sample solution to be tested;

[0036] (3) adopt gas chromatography-mass spectrometer to detect standard working solution in the above-mentioned steps (1) and draw standard working curve;

[0037] (4) adopt gas chromatography-mass spectrometry to the qualitative and quantitative analysis of dipropylene glycol isomers in the sample to be tested in step (2).

[0038] In alternative embodiments, dipropylene glycol isomers include 1,1'-oxybis-2-propanol, 2-(2-hydroxypropoxy)-1-propanol and 2,2' One, two or more of -oxybis-1-propanols, see Table 2.

[0039] The details of three kinds of dipropylene glycol standard substances in table 2

[0040] serial number name CAS NO. Manufacturer purity(%) 1 1,1’-Oxybis-2-propanol 110-98-5 Sinopharm 95.0 2 2-(2-Hydroxypropoxy)-1-propanol 106-62-7 Baihua Mall 95.0 3 2,2'-Oxybis-1-propanol 108-61-2 Sinopharm 95.0

[0041] In an optional embodiment, the sample to ...

Embodiment 1

[0115] Present embodiment 1 is for dipropylene glycol pure sample:

[0116] Samples: Shanghai Xindao Chemical Co., Ltd. (A1-A10); Dongguan Heshibi New Material Co., Ltd. (A11-A20); Dow Chemical (China) Co., Ltd. (A21-A30); Shanghai Yunran Chemical Co., Ltd. ( A31-A40); Nanjing Junhe Chemical Co., Ltd. (A41-A45); Shandong Shida Shenghua Chemical Group Co., Ltd. (A46-A50). Table 4 shows.

[0117] Table 4 Total content of 3 isomers in 50 pure samples of dipropylene glycol

[0118]

[0119]

[0120]

[0121] Preparation of isomer standard working solution containing internal standard:

[0122] Accurately weigh dodecane (accurate to 0.0001g), use isopropanol as a solvent, and accurately prepare a stock solution of dodecane isopropanol with a concentration of 10.00mg / mL, and store in the dark.

[0123]Accurately weigh each isomer standard substance (accurate to 0.0001g), dilute to volume with dodecyl isopropanol stock solution, prepare concentration is 25.00mg / mL isomer ...

Embodiment 2

[0137] Present embodiment 2 is for the oil-soluble essence containing dipropylene glycol:

[0138] Sample: Brand 1 oily fragrance (B1-B10); Brand 2 oily fragrance (B11-B20); Brand 3 oily fragrance (B21-B30); Brand 4 oily fragrance (B31-B40); Brand 5 oily fragrance (B41-B50 ), the total content of its isomers is shown in Table 6.

[0139] Table 6 Total content of 50 oil-soluble flavor isomers containing dipropylene glycol

[0140]

[0141]

[0142] Accurately weigh more than 0.2500g of sample (accurate to 0.0001g), put it into a 10mL volumetric flask, use 10.00mg / mL dodecylacetone stock solution to make up the volume, oscillate and shake well, and filter the sample through 0.22μm polytetrafluoroethylene Membrane, gas chromatography-mass spectrometer injection analysis.

[0143] Then the gas chromatographic mass spectrogram that obtains sample is analyzed and processed, the ratio of three isomer peak areas of sample and the peak area of ​​dodecane is substituted into for...

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Abstract

The invention discloses a method for separating and detecting dipropylene glycol isomeride, and the dipropylene glycol isomeride comprises one, two or more of 1, 1 '-oxybis-2-propanol, 2-(2-hydroxypropoxy)-1-propanol and 2, 2'-oxybis-1-propanol, and the dipropylene glycol isomeride comprises one, two or more of 1, 1 '-oxybis-2-propanol, 2-(2-hydroxypropoxy)-1-propanol and 2, 2'-oxybis-1-propanol. The method for separating and detecting the dipropylene glycol isomeride in the sample to be detected comprises the following steps: adding an internal standard working solution into the sample to be detected for constant volume, filtering, analyzing the content of the dipropylene glycol isomeride in the sample to be detected by GC-MS (Gas Chromatography-Mass Spectrometer), and quantifying by an internal standard method, and a solvent in the internal standard working solution is any one of ethanol, isopropanol, n-butyl alcohol and acetone. The method provided by the invention solves the problem that the dipropylene glycol isomeride is difficult to separate, qualitatively and quantitatively, and provides a detection method for improving the production process of dipropylene glycol.

Description

technical field [0001] The invention relates to the technical field of analysis and detection, in particular to a method for the separation and detection of dipropylene glycol isomers. Background technique [0002] Dipropylene glycol (Dipropylene Glycol, DPG) is one of the important industrial derivatives of propylene oxide, which is mainly divided into two categories: fragrance grade and industrial grade. The former is mainly used in high-quality raw material demand fields such as spices, cosmetics, detergents, and food additives; the latter is mainly used in raw materials for industrial solvents, unsaturated polyester production, and nitrocellulose varnish. [0003] Dipropylene glycol is synthesized with propylene glycol and propylene oxide as raw materials. At present, the main processes are divided into: [0004] Using organic amines as catalysts; [0005] Using sodium methylate / sodium ethylate as catalyst; [0006] Using acidic ionic liquid as catalyst; [0007] On ...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/72
CPCG01N30/02G01N30/72
Inventor 刘振范珺孙添源
Owner JIANGSU MAYSTA CHEM
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