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Method for identifying alkane-doped plasticizer organosilicon product by nuclear magnetic resonance hydrogen spectrum

A hydrogen nuclear magnetic resonance spectrum and silicone technology, applied in the field of nuclear magnetic detection, can solve the problems of misjudgment as alkane plasticizer and long test cycle, etc., and achieve the effect of small sample volume, simple and intuitive principle, and simple sample processing

Pending Publication Date: 2020-11-03
中蓝晨光成都检测技术有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The use of infrared spectroscopy described in the CN101887014A patent, the selected sample is to use acetone to swell the silicone rubber, extract the swollen solution for infrared spectrum testing, and use the characteristic absorption peaks of chain hydrocarbons in the infrared spectrum to qualitatively determine whether the silicone rubber contains White oil, the pretreatment period of the swelling process mentioned above is 7 days, the test period is long, and it is easy to misjudge the additives in the silicone rubber product formula as alkane plasticizers

Method used

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  • Method for identifying alkane-doped plasticizer organosilicon product by nuclear magnetic resonance hydrogen spectrum
  • Method for identifying alkane-doped plasticizer organosilicon product by nuclear magnetic resonance hydrogen spectrum
  • Method for identifying alkane-doped plasticizer organosilicon product by nuclear magnetic resonance hydrogen spectrum

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] 1.1 Test sample

[0049] Uncured, one-part silicone sample containing 5% alkane plasticizer.

[0050] 1.2 Test steps

[0051] Weigh about 10 mg of organosilicon sample into an NMR tube, add 1 tube (about 0.6 ml, purity 99.8%) of deuterated chloroform (CDCl 3 ) to fully dissolve the sample, and carry out nuclear magnetic resonance spectrum testing to the sample, and the test conditions are as follows:

[0052] a) Pulse program: single pulse;

[0053] b) Test temperature: room temperature;

[0054] c) Pulse angle: 90°;

[0055] d) Acquisition time: 4s;

[0056] e) Relaxation time: 1s;

[0057] f) Number of scans: 16 times;

[0058] g) Empty scan times: 2 times.

[0059] The NMR spectrum of the sample of this embodiment is as figure 2 shown. from figure 2 It can be seen from the figure that the characteristic peak of methylene hydrogen appears near the chemical shift of 1.29ppm, and the characteristic peak of methyl hydrogen appears near the chemical shift of ...

Embodiment 2

[0062] 2.1 Test sample

[0063] Cured one-part silicone sample containing 5% alkane plasticizer.

[0064] 2.2 Experimental steps

[0065] Take by weighing about 100mg of the solidified sample, cut it into 5 splines with a length of about 5mm, put the splines into an NMR tube and use 2 (about 1.2ml, purity 99.8%) deuterated chloroform (CDCl 3 ) soaked for 24h; the soaking liquid was transferred to another NMR tube for NMR spectrum testing. The test conditions are as follows:

[0066] a) Pulse program: single pulse;

[0067] b) Test temperature: room temperature;

[0068] c) Pulse angle: 90°;

[0069] d) Acquisition time: 10s;

[0070] e) Relaxation time: 1s;

[0071] f) Number of scans: 16 times;

[0072] g) Empty scan times: 2 times.

[0073] The NMR spectrum of the sample of this embodiment is as image 3 shown. As can be seen from the figure, the characteristic peak of methylene hydrogen appears in the chemical shift of 1.29ppm, and the characteristic peak of meth...

Embodiment 3

[0075] 3.1 Test sample

[0076] Cured two-part silicone sample containing 5% alkane plasticizer.

[0077] 3.2 Experimental steps

[0078] Weigh about 150 mg of the cured sample, cut it into 5 splines with a length of about 5 mm, put the splines into an NMR tube and soak them in 2 sticks (about 1.2 ml, purity 99.8%) of deuterated acetone for 24 hours; The soaking liquid was transferred to another NMR tube for NMR spectroscopy. The test conditions are as follows:

[0079] a) Pulse program: single pulse;

[0080] b) Test temperature: room temperature;

[0081] c) Pulse angle: 90°;

[0082] d) Acquisition time: 4s;

[0083] e) Relaxation time: 4s;

[0084] f) Number of scans: 16 times;

[0085] g) Empty scan times: 2 times.

[0086] The NMR spectrum of the sample of this embodiment is as Figure 4 shown. As can be seen from the figure, the characteristic peak of methylene hydrogen appears in the chemical shift of 1.29ppm, and the characteristic peak of methyl hydrogen a...

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Abstract

The invention provides a method for identifying an alkane-doped plasticizer organic silicon product through a nuclear magnetic resonance hydrogen spectrum, and belongs to the technical field of nuclear magnetic detection. The nuclear magnetic resonance hydrogen spectrum of the alkane plasticizer doped in the organic silicon sample needs to meet the following requirements: 1) a characteristic peakof methylene hydrogen appears near the chemical shift 1.29 ppm; 2) a characteristic peak of methyl hydrogen appears near the chemical shift of 0.89 ppm; and 3) a series of weak peaks also appear in achemical shift range of 0.7-1.8 ppm. According to the method, a nuclear magnetic resonance spectrometer is used for testing an uncured organic silicon sample solution dissolved by a deuterated reagentand a cured organic silicon sample leaching solution soaked by the deuterated reagent, and characteristic peaks corresponding to the alkane plasticizer in a nuclear magnetic spectrogram are analyzed,so that whether the alkane plasticizer is doped into an organic silicon product or not is judged. Nuclear magnetic resonance hydrogen spectrum analysis is adopted to identify whether the alkane plasticizer is added into the organosilicon product, and the method has the advantages of high test accuracy, simple and visual principle, short sample test period, simple sample treatment and less required sample amount.

Description

technical field [0001] The invention belongs to the technical field of nuclear magnetic detection, and specifically relates to a method for identifying organic silicon products mixed with alkane plasticizers by hydrogen nuclear magnetic resonance spectroscopy. Background technique [0002] In recent years, the organic silicon industry has grown stronger and stronger, and more and more organic silicon products have appeared in the market. The price of raw materials such as silicon monomer and silicone oil is on the rise. In order to pursue greater profits and improve the initial gloss and workability of products, many companies use relatively cheap alkane plasticizers (such as white oil, liquid Paraffin, etc.) instead of silicone oil as a plasticizer to produce so-called "oil-extended rubber" with high oil-extended ratio and high filler ratio. The addition of alkane plasticizer does not affect the initial physical and chemical properties of the product. In the existing quali...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N24/08
CPCG01N24/08
Inventor 幸荣勇李天祥陈敏剑罗晓霞彭斌
Owner 中蓝晨光成都检测技术有限公司
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