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In-situ nuclear magnetic resonance test reactor and detection method thereof

A nuclear magnetic resonance and reactor technology, which is used in the analysis of nuclear magnetic resonance, material analysis through resonance, and instruments, etc., can solve problems such as inability to meet experimental conditions, and achieve the effects of low cost, simple operation, and ingenious design.

Inactive Publication Date: 2017-10-13
EAST CHINA UNIV OF SCI & TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

It solves the problem of light, normal temperature and pressure, gas-liquid-solid experimental conditions that cannot be met by similar methods in the current prior art

Method used

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  • In-situ nuclear magnetic resonance test reactor and detection method thereof
  • In-situ nuclear magnetic resonance test reactor and detection method thereof
  • In-situ nuclear magnetic resonance test reactor and detection method thereof

Examples

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specific Embodiment 1

[0042] Specific embodiment 1: study the generation process of hydrogen-containing gas in the solution in the photolysis water reaction process

[0043] Step 1. Catalyst preparation and sample loading preparation

[0044] Appropriate amount of PdCl 2 Aqueous solution was added to the solution containing 100 mg TiO 2 in the crucible, at 80 o Stir and dry under the condition of C; put the crucible in the muffle furnace, with 5 o The rate of C / min raises the temperature of the muffle furnace to 300 o C, treated at constant temperature for 1 h; then, cool down to room temperature naturally, and take out the crucible. Subsequently, the sample was taken out and placed in the quartz ark, and the quartz ark was pushed into the central hot zone of the tube furnace, and the flange was sealed; the hydrogen and argon were measured by the rotameter (hydrogen flow and argon flow than 20 % H 2 / Ar) into the tube furnace after being fully mixed; with 5 o C / min rate to heat up the tube fur...

specific Embodiment 2

[0049] Specific Example 2: Study H 2 O / CD 3 OD and D 2 O / CH 3 Generation of hydrogen-containing gas and intermediate products in OH system

[0050] Pd / TiO 2 The synthesis method of the catalyst is similar to that of Example 1. 2 mg Pd / TiO 2 Catalyst, 20 μL CH 3 OH and 500 μL D 2 O (sample A) and 2 mg Pd / TiO 2 Catalyst, 20 μL H 2 O and 500 μL CD 3 OD (sample B) was added into different NMR tubes, and the ultrasonic dispersion was uniform. Subsequent sample loading preparations are similar to those in Implementation 1.

[0051] Under the condition of shielding from light, carry out in situ on the sample in the in situ NMR reactor 1 H NMR test. The nuclear magnetic resonance instrument in the embodiment is a 700 MHz Agilent nuclear magnetic resonance instrument. Then turn on the xenon light source, and after a certain period of time, the in-situ nuclear magnetic resonance reactor in the liquid 1 H signal is collected. refer to Figure 7 with Figure 8 , against...

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Abstract

The invention relates to an in-situ nuclear magnetic resonance test reactor and a detection method, which can realize the tracking and detection of hydrogen-containing compounds in the real solid-liquid gas photocatalytic reaction process. The in-situ reactor includes: a nuclear magnetic cap that is fixedly connected to the nuclear magnetic tube and the optical fiber and the gas path; the upper and lower holes are opened in the middle of the nuclear magnetic cap, and the hole is covered with a sealing ring, which is respectively connected to the nuclear magnetic tube and the optical fiber; the upper port is used to make the customized optical fiber Go deep into the nuclear magnetic tube, and inject the light into the heterogeneous solid-liquid suspension to be tested; open a hole near the edge above the nuclear magnetic cap, cover the hole with a sealing ring, and connect with the gas circuit; this port is used to pass the gas into the Inside the NMR tube. Using the device of the present invention, the evolution process of hydrogen-containing reactants in the heterogeneous reaction process and their diffusion properties in the liquid can be tracked in situ, the structural information of the reaction intermediate products can be quantitatively analyzed, and the influencing factors and mechanism of the catalytic process can be clarified . This test method can study the reaction performance mechanism in the field of solid-liquid-gas catalysis related to hydrocarbons. The in-situ reactor has ingenious design, simple operation and low cost, and is favorable for popularization and application in other photoreaction and heterogeneous catalytic reaction systems.

Description

technical field [0001] The invention relates to an in-situ nuclear magnetic resonance test reactor and a detection method in a solid-liquid-gas reaction environment, and is especially suitable for hydrogen-containing compounds and carbon-containing compounds in reaction processes such as photolysis of water for hydrogen production, fuel cells, and carbon dioxide photoreduction / photoelectric reduction. Tracking of compound changes, the reactor and method have potential capabilities for studying the reaction performance mechanism in the field of solid-liquid-gas catalysis related to hydrocarbons. Background technique [0002] Energy shortage, environmental pollution and climate problems are global problems that restrict the sustainable and healthy development of human society in the 21st century. Compared with the "carbon economy" represented by traditional fossil energy production, hydrogen production technology driven by solar energy has the advantages of high calorific valu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N24/08
CPCG01N24/082
Inventor 杨化桂姚叶锋王雪璐刘文卿宋艳红房文祺
Owner EAST CHINA UNIV OF SCI & TECH
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