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Method for determining content of organic peroxide

A technology of organic peroxide and content, applied in the direction of measuring devices, instruments, scientific instruments, etc., to achieve the effect of high accuracy and precision

Pending Publication Date: 2020-05-22
CHINA SHENHUA COAL TO LIQUID & CHEM CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The purpose of the present invention is to provide a method for measuring the content of organic peroxides in order to overcome the problem of large errors in the determination of organic peroxides in the prior art, which has the advantages of accurate and precise determination of organic peroxides content effect, and capable of determining at least one of tert-butyl peroxy-2-ethylhexanoate, tert-butyl peroxyisononanoate, tert-butyl peroxypivalate and di-tert-butyl peroxide

Method used

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  • Method for determining content of organic peroxide
  • Method for determining content of organic peroxide
  • Method for determining content of organic peroxide

Examples

Experimental program
Comparison scheme
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Embodiment 1

[0058] This embodiment is used to illustrate the establishment of organic peroxide standard curve

[0059] (1) Solution preparation

[0060] Preparation of standard solution: take 250mg organic peroxide (DTBP, TBPPI, TBPEH or TBPIN) standard sample and dissolve it in 250mg isododecane, then add different amounts of methanol, shake well and mix to obtain a concentration of 1% by weight, 5 wt% and 8 wt% standard solutions.

[0061] Before the HPLC detection of the standard solution, the standard solution was filtered with a 0.45 μm filter membrane.

[0062] (2) HPLC analysis

[0063] This embodiment establishes the standard curve of DTBP, TBPPI, TBPEH and TBPIN according to the following method successively

[0064] High performance liquid chromatography: Shimadzu LC-2030;

[0065] Chromatographic column: reversed C18 column, Poroshell 120;

[0066] Detector: UV-Vis spectrophotometer LAMBDA25, wavelength 254nm;

[0067] Column temperature: 30°C;

[0068] Mobile phase: for...

Embodiment 2

[0077] This embodiment is used to illustrate the mensuration of organic peroxide test sample content

[0078] The preparation of the sample to be tested: take organic peroxide (DTBP, TBPPI, TBPEH or TBPIN) standard sample, use isododecane to be respectively formulated with the TBPPI of 25.12% by weight, the TBPEH of 30.15% by weight, the TBPIN of 30.18% by weight and 49.92% by weight DTBP.

[0079] After fully mixing 9 parts by weight of methanol and 1 part by weight of the sample to be tested, the sample solution to be tested was obtained, and before the HPLC detection of the sample solution to be tested, the sample solutions to be tested were respectively filtered using 0.45 μm filter membranes.

[0080] The concentration of the above-mentioned sample solution to be tested was determined according to the HPLC analysis method described in Example 1, with 8 parallels for each solution.

[0081] Taking TBPEH as an example, the 30.15% by weight TBPEH sample to be tested was ana...

Embodiment 3

[0086] This embodiment is used to illustrate the mensuration of organic peroxide test sample content

[0087] Preparation of sample to be tested: take organic peroxide (TBPPI, TBPEH and TBPIN) standard sample, use isododecane to prepare TBPPI (10% by weight), TBPEH (15% by weight) and TBPIN (20% by weight) Mix the samples.

[0088] After fully mixing 9 parts by weight of methanol and 1 part by weight of the sample to be tested, the sample solution to be tested was obtained, and before the HPLC detection of the sample solution to be tested, the sample solutions to be tested were respectively filtered using 0.45 μm filter membranes.

[0089] The concentration of the above-mentioned sample solution to be tested was determined according to the HPLC analysis method described in Example 1, and a total of 3 parallels were performed.

[0090] According to HPLC analysis, the content of each component in the sample to be tested is: TBPPI 10.76±0.42 wt%, TBPEH 15.56±0.57 wt%, and TBPIN ...

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Abstract

The invention relates to the field of organic peroxide analysis. The invention discloses a method for determining the content of an organic peroxide. The method comprises the following steps of: firstly drawing an organic peroxide standard curve by using a reversed-phase C18 chromatographic column through HPLC method, then acquiring the content of the organic peroxide in a to-be-detected sample under the same condition according to the standard curve, wherein the organic peroxide is selected from at least one of tert-butyl peroxy-2-ethylhexanoate, tert-butyl peroxyisononanoate, tert-butyl peroxypivalate and di-tert-butyl peroxide. The method for determining the content of the organic peroxide has the advantages of time saving, labor saving, high accuracy and good repeatability, can overcome errors during iodometry determination, and can avoid the problem that the organic peroxide is easy to decompose at a high temperature and cannot be accurately determined during gas chromatographic analysis.

Description

technical field [0001] The invention relates to the field of analysis of organic peroxides, and discloses a method for determining the content of organic peroxides. Background technique [0002] At present, high-pressure polyethylene uses tert-butyl peroxy-2-ethylhexanoate (TBPEH), tert-butyl peroxyisonononanoate (TBPIN), tert-butyl peroxypivalate (TBPPI), di-tert-butyl peroxide Oxide (DTBP) Four organic peroxides were used as initiators for the polymerization reaction. Among the four organic peroxides, TBPPI has the worst stability, the auto-accelerated degradation temperature is 20°C, and the storage temperature is below minus 5°C. During the determination process, it is easy to degrade and cause large errors in the measurement results. [0003] The current analytical method uses the iodometric method to quantify organic peroxides. Since there are by-products and unreacted raw materials in the synthesis reaction of organic peroxides, and the content of by-products and u...

Claims

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Application Information

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IPC IPC(8): G01N30/89
CPCG01N30/89
Inventor 葛喜慧姜兴剑黄起中杨红杰刘强徐特
Owner CHINA SHENHUA COAL TO LIQUID & CHEM CO LTD
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