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Nuclear magnetic resonance detection method of glycerol hydrogenation reaction mixture

A hydrogenation reaction and nuclear magnetic resonance technology, which is applied in the analysis by nuclear magnetic resonance, material analysis by resonance, and measurement devices, etc., can solve the problems of signal overlap, redundancy, loss of nuclear magnetic information, etc., and achieve good stability and applicability , The effect of fast detection speed and high sensitivity

Active Publication Date: 2017-11-07
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Liquid chromatography can avoid complex derivatization operations in most cases by adjusting the polarity of the mobile phase, but usually requires the use of more expensive analytical standards to assist in the completion of structure identification
[0004] Conventional NMR spectra, such as 1 H and 13 C spectrum is very convenient and quick to analyze pure substances, but the detection of mixtures has the following limitations: 1 In the H NMR spectrum, the peaks of the components of the mixture are crowded in a narrow spectrum range (about 20ppm), which easily leads to signal overlap and increases the difficulty of spectrum analysis
Usually need to use two-dimensional graph, such as 1 H- 1 H correlation (COSY, TOCSY) and 1 H- 13 C-correlation (HSQC, HMBC), etc., perform complex spectral assignment, which is very tedious work for experimenters who want to quickly interpret the composition of the mixture
13 Although the C NMR spectrum has a large spectral width (about 200ppm), but 13 C spectrum will lose many important NMR information, such as coupling constants, splitting conditions, spectral peak integration, etc., which will also cause great difficulties for material analysis

Method used

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  • Nuclear magnetic resonance detection method of glycerol hydrogenation reaction mixture
  • Nuclear magnetic resonance detection method of glycerol hydrogenation reaction mixture
  • Nuclear magnetic resonance detection method of glycerol hydrogenation reaction mixture

Examples

Experimental program
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Effect test

Embodiment 1

[0034] (1) Take 1,3-propanediol (1,3-POD), 1,2-propanediol (1,2-POD), glycerol (Glycerol), n-propanol (n-PO) and isopropanol (2 -PO) each 4 mg mixed, added to 400 μL deuterated methanol solvent, after being completely dissolved, added to a 5 mm NMR tube as an analysis model for the glycerol hydrogenation reaction mixture. Put the sample tube into the main magnet of the 400MHz liquid nuclear magnetic resonance spectrometer, and the maximum gradient field strength that can be generated by the z-axis gradient coil of the nuclear magnetic resonance spectrometer is 0.5T m -1 . Put the mixture sample into the main magnet of the nuclear magnetic resonance spectrometer, set the magnet temperature to 298K, the compressed air flow to 400lph, and keep the temperature constant for 5 minutes;

[0035] (2) Call out the BPPLED pulse sequence of the diffusion sorting spectrum, set the gradient recovery delay to 2ms, the eddy current delay to 5ms, the number of scans to 8, the number of empty...

Embodiment 2

[0041] (1) Take 100 μL of the real glycerin hydrogenation reaction mixture, put it into an NMR tube, add 300 μL of deuterated methanol, and after it is completely dissolved, put the sample tube into the main magnet of a 400MHz liquid NMR spectrometer. The maximum gradient field strength that can be generated by the z-axis gradient coil of the instrument is 0.5T m -1 . Set the magnet temperature to 323K, the airflow to 500lph, and keep the temperature constant for 40 minutes;

[0042] (2) Call out the BPPLED pulse sequence of the diffusion sorting spectrum, set the gradient recovery delay to 2ms, the eddy current delay to 5ms, the number of scans to 16, the number of empty scans to 8, and the number of sampling points (TD) for each image to be 64k. Set the diffusion time (Δ) to 50ms, the gradient application time (δ / 2) to 600μs, and the gradient strength (GPZ6) to be 2% of the maximum gradient strength, collect the first one-dimensional hydrogen spectrum; set the diffusion tim...

Embodiment 3

[0048] (1) Mix 4mg of 1,2-propanediol (1,2-POD), 6mg of glycerol (n-PO) and 0.015mg of n-propanol, dissolve them in 500 deuterated dimethyl sulfoxide, and add In the NMR tube, the mass concentration of n-propanol is 34ppm (one part per million), and the sample tube is placed in the main magnet of the 400MHz liquid NMR spectrometer. The maximum gradient that can be produced by the z-axis gradient coil of the NMR spectrometer is The field strength is 0.5T·m -1. Set the magnet temperature to 300K, the air flow to 500lph, and keep the temperature constant for 60 minutes; (2) Call out the BPPLED pulse sequence of the diffusion sorting spectrum, set the gradient recovery delay to 2ms, the eddy current delay to 5ms, set the number of scans to 16, and the number of empty scans to 4 , the number of sampling points (TD) of each image is 16k. Set the diffusion time (Δ) to 50ms, the gradient application time (δ / 2) to 1500μs, and the gradient strength (GPZ6) to be 2% of the maximum gradi...

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Abstract

The invention discloses a nuclear magnetic resonance detection method of a glycerol hydrogenation reaction mixture. The method comprises the steps of dissolving a glycerol hydrogenation reaction mixture sample in a deuterated reagent, putting the sample into a nuclear magnetic resonance spectrometer, detecting a component of the mixture sample by utilizing BPPLED pulse of a diffusion ordered spectroscopy technology, performing preliminary attribution, and then further confirming the component of the mixture sample by utilizing SELMLGP pulse of a one-dimensional selective excitation total correlation spectroscopy (TOCSY) technology. An analysis result obtained by the method is visual and clear; the detection sensitivity is higher; the glycerol hydrogenation reaction mixture sample can be well detected; and the method is also applicable to qualitative detection of a component of low carbon alcohol.

Description

technical field [0001] The invention relates to a nuclear magnetic resonance detection method for a glycerin hydrogenation reaction mixture Background technique [0002] With the overexploitation of petrochemical resources and the aggravation of environmental pollution caused by fossil fuels, the research and development of renewable liquid fuels has become a current research hotspot. As a renewable energy source, biodiesel (fatty acid methyl ester) has been highly valued, and its output is increasing year by year. For every ton of biodiesel produced by transesterification, 100kg of by-product glycerin will be obtained at the same time. Efficient utilization of glycerol is one of the key factors to promote the healthy development of biodiesel industry. Glycerol conversion reactions are diverse and complicated. Among them, converting glycerin into 1,3-propanediol, 1,2-propanediol, n-propanol and isopropanol, etc., through hydrogenation reaction, is one of the more common w...

Claims

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Application Information

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IPC IPC(8): G01N24/08
CPCG01N24/087
Inventor 乔岩吕泽祥延秀银王英雄
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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