Method for determining conversion rate during p-polyisobutylene phenol synthesis process through quantitative nuclear magnetic resonance spectroscopy

A polyisobutylene phenol and hydrogen nuclear magnetic resonance spectroscopy technology is applied in the field of chemical analysis to achieve the effects of ensuring high efficiency, saving money and high accuracy

Active Publication Date: 2018-06-12
CHAMBROAD CHEM IND RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Due to the advantages of high sensitivity, high precision, and fast analysis, the hydrogen spectrum nuclear magnetic resonance method has been widely used in the structural ana...

Method used

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  • Method for determining conversion rate during p-polyisobutylene phenol synthesis process through quantitative nuclear magnetic resonance spectroscopy
  • Method for determining conversion rate during p-polyisobutylene phenol synthesis process through quantitative nuclear magnetic resonance spectroscopy
  • Method for determining conversion rate during p-polyisobutylene phenol synthesis process through quantitative nuclear magnetic resonance spectroscopy

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] There are a batch of self-synthesized p-polyisobutylene phenol samples. According to the synthesis process estimated by the synthesizers, the conversion rate of polyisobutylene is 90%. The conversion rate of polyisobutylene needs to be determined and analyzed by hydrogen nuclear magnetic spectroscopy. The specific steps include:

[0041] Weigh 13.5067 mg of self-synthesized p-polyisobutylene phenol sample into a clean glass sample bottle, add 0.5 mL of deuterated chloroform to dissolve it and transfer it to the NMR tube. 1 H NMR test. The resonance frequency of the NMR spectrometer is 400MHz, the pulse tilt angle is 30°, D 1 It is 20s, the number of acquisition and accumulation is 32 times, the spectrum width is 12ppm, and the test temperature is 23±1℃.

[0042] Such as Figure 4 Shown in 1 In the H NMR spectrum, A 1 = 117.70, A 2 =1.00,A 3 =(2.41+5.41), according to the conversion rate calculation formula, the conversion rate of polyisobutylene in the process of self-made p-...

Embodiment 2

[0049] There is a batch of self-synthesized polyisobutylene phenol samples. According to the synthesis process estimated by the synthesizer, the conversion rate of polyisobutylene is 80%. The conversion rate of polyisobutylene needs to be determined and analyzed by hydrogen nuclear magnetic spectroscopy. The specific steps include:

[0050] Weigh 15.5031 mg of self-synthesized p-polyisobutylene phenol sample into a clean glass sample bottle, add 0.5 mL deuterated chloroform to dissolve it and transfer it to the NMR tube. 1 H NMR test. The resonance frequency of the NMR spectrometer is 400MHz, the pulse tilt angle is 30°, D 1 It is 20s, the number of acquisition and accumulation is 32 times, the spectrum width is 12ppm, and the test temperature is 23±1℃.

[0051] Such as Figure 5 Shown in 1 In the H NMR spectrum, A 1 = 70.88, A 2 = 1.10, A 3 =(1.56+5.89), the conversion rate of polyisobutylene in the process of self-made synthetic p-polyisobutylene phenol was calculated according to...

Embodiment 3

[0058] There is a batch of self-synthesized p-polyisobutylene phenol samples. According to the synthesis process estimated by the synthesizer, the conversion rate of polyisobutylene is 30%. The conversion rate of polyisobutylene needs to be determined and analyzed by hydrogen nuclear magnetic spectroscopy. The specific steps include:

[0059] Weigh 11.9022 mg of self-synthesized p-polyisobutylene phenol sample into a clean sample glass bottle, add 0.5 mL of deuterated chloroform to dissolve it and transfer it to a nuclear magnet tube for 1H NMR test. The resonance frequency of the NMR spectrometer is 400MHz, the pulse tilt angle is 30°, D 1 It is 20s, the number of acquisition and accumulation is 32 times, the spectrum width is 12ppm, and the test temperature is 23±1℃.

[0060] Such as Image 6 Shown in 1 In the H NMR spectrum, A 1 = 12.42, A 2 =6.43,A 3 =(3.99+3.87), the conversion rate of polyisobutylene in the process of self-made p-polyisobutylene phenol was calculated according...

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Abstract

The invention relates to a method for determining the conversion rate of polyisobutylene, in particular to a method for determining the conversion rate of the polyisobutylene during a process of generating p-polyisobutylene phenol through reaction of the polyisobutylene and excessive phenol through a quantitative nuclear magnetic resonance spectroscopy. The method comprises the steps of respectively acquiring a polyisobutylene phenol sample, and a polyisobutylene and phenol nuclear magnetic resonance spectroscopy, obtaining chemical shift of the p-polyisobutylene phenol through spectrogram comparison and spectrogram reasoning; determining longitudinal relaxation time T1 of a p-polyisobutylene phenol sample in a deuteration reagent, setting a pulse flip angle and relaxation time of a nuclear magnetic resonance spectrometer according to the T1, utilizing the nuclear magnetic resonance spectrometer for determining the nuclear magnetic resonance spectroscopy of a solution to be tested, obtaining a peak area of each part of hydrogen through integration, and calculating to obtain the conversion rate of the polyisobutylene through the number of hydrogen actually contained in a target product and raw materials. The method provided by the invention is low in cost, can be used for quickly and accurately evaluating the type and the conversion rate of a synthetic product of the polyisobutylene and the phenol, and provides a powerful evidence for synthesis.

Description

Technical field [0001] The invention relates to the technical field of chemical analysis, in particular to a method for quantitative hydrogen nuclear magnetic resonance spectroscopy to determine the conversion rate in the process of synthesizing p-polyisobutylene phenol. Background technique [0002] Energy conservation and environmental protection have now become a topic that must be paid attention to in the development of all walks of life. With the improvement of people's living standards, automobiles have become a necessity for every family and even everyone, so the consumption of gasoline and diesel will continue to increase. With the increasing awareness of environmental protection and energy conservation, fuels such as gasoline and diesel must be developed to be cleaner and more efficient. [0003] The Mannich type cleaner with polyisobutylene Mannich base as the main component is an efficient and excellent cleaning and combustion aid. Adding a small amount to gasoline can...

Claims

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Application Information

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IPC IPC(8): G01N24/08
CPCG01N24/088
Inventor 赵红波马韵升王岳华柴晓飞史会兵李晓红张锐韩立霞王兴之路建
Owner CHAMBROAD CHEM IND RES INST CO LTD
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