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A kind of product detection method of organic electrochemical ammonia synthesis reaction system

A technology of reaction system and detection method, which is applied in the direction of analyzing materials through chemical reactions, material analysis and measuring devices by observing the effects on chemical indicators, and can solve the problems of correct evaluation of effects, few studies, and ultraviolet absorption. Spectral baseline offset and other issues, to achieve the effect of accurate calculation method, wide application range, and reduce the degree of deviation

Active Publication Date: 2021-12-21
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] As early as 1993, some researchers carried out the electrochemical synthesis of ammonia in organic systems, and obtained relatively satisfactory results. However, there were only a few other related studies in the past few decades.
Until 2019, researchers pointed out that in the actual electrochemical synthesis of ammonia test, the product test in the organic electrolyte will shift the baseline of the ultraviolet absorption spectrum, resulting in the inability to accurately calibrate the product ammonia. The correct evaluation of the product has a great impact, hindering the development of electrochemical ammonia synthesis in organic systems

Method used

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  • A kind of product detection method of organic electrochemical ammonia synthesis reaction system
  • A kind of product detection method of organic electrochemical ammonia synthesis reaction system
  • A kind of product detection method of organic electrochemical ammonia synthesis reaction system

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Experimental program
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Effect test

Embodiment 1

[0049] The electrolyte pretreatment method adopted in the product detection method of the organic electrochemical ammonia synthesis reaction system in this embodiment is to take a mixed solution of standard solution (as a sample electrolyte) and water with different ammonia concentrations for testing. Among them, the ammonia concentration range of the standard solution is 0 μg mL -1 , 0.2 μg mL -1 , 0.5 μg mL -1 , 1 μg mL -1 , 2 μg mL -1 and 5 μg mL -1 The total volume of the mixed solution is 2mL; the volume ratio of the standard solution and water in the mixed solution is 1.0 / 1.0.

[0050] Then adopt the conventional indophenol blue method to color the above mixed solution, the specific steps are: add 2mL of 1M NaOH solution (mixing 5wt% of salicylic acid and 5wt% of sodium citrate) and 1mL of 0.05M NaOH solution to 2mL of the test solution Sodium hypochlorite solution, finally add 0.2mL 1wt% sodium nitroferricyanide solution, mix well, and color for 1h.

[0051] Take ...

Embodiment 2

[0053] The product detection method of a reaction system for organic electrochemical synthesis of ammonia in this embodiment is to use standard solutions with different ammonia concentrations (as sample electrolytes) for direct testing. Among them, the ammonia concentration range of the standard solution is 0 μg mL -1 , 0.2 μg mL -1 , 0.5 μg mL -1 , 1 μg mL -1 , 2 μg mL -1 and 5 μg mL -1 ; The total volume of the electrolyte is 2mL.

[0054] Then adopt the conventional indophenol blue method to color the above mixed solution, the specific steps are: add 2mL of 1M NaOH solution (mixing 5wt% of salicylic acid and 5wt% of sodium citrate) and 1mL of 0.05M NaOH solution to 2mL of the test solution Sodium hypochlorite solution, finally add 0.2mL 1wt% sodium nitroferricyanide solution, mix well, and color for 1h.

[0055] Get the solution after above-mentioned color development and use ultraviolet spectrophotometer to carry out ultraviolet absorption spectrum analysis, test wav...

Embodiment 3

[0057] The electrolyte pretreatment method used in the product detection method of a reaction system for organic electrochemical synthesis of ammonia in this example is to mix 1mL of standard solutions with different ammonia concentrations (as the sample electrolyte) with 0.1mL of 6M hydrochloric acid, and then carry out a low temperature reaction at 40°C. Treat until the THF solvent is completely volatilized, then add 2 mL of deionized water and mix the solute thoroughly, and use this aqueous solution for testing. Among them, the ammonia concentration range of the standard solution is 0 μg mL -1 , 0.2 μg mL -1 , 0.5 μg mL -1 , 1 μg mL -1 , 2 μg mL -1 and 5 μg mL -1 .

[0058] Then adopt the conventional indophenol blue method to color the above mixed solution, the specific steps are: add 2mL of 1M NaOH solution (mixing 5wt% of salicylic acid and 5wt% of sodium citrate) and 1mL of 0.05M NaOH solution to 2mL of the test solution Sodium hypochlorite solution, finally add 0...

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Abstract

The invention discloses a product detection method of an organic electrochemical ammonia synthesis reaction system. The method comprises: carrying out the conventional indophenol blue method test on the electrolytic solution of the organic electrochemical ammonia synthesis reaction system to obtain a color-developing solution; performing ultraviolet spectrophotometric analysis on the color-developing solution to obtain a full-spectrum curve, taking the absorbance value, and calculating the product ammonia content. In the present invention, the product detection method is the optimized indophenol blue colorimetric method, and the organic electrolyte pretreatment and the ultraviolet absorption spectrum analysis are two-pronged, eliminating the baseline shift problem that sometimes occurs due to the optical fiber design of the ultraviolet spectrophotometer, thereby reducing due to Possibility of overestimating ammonia concentration due to baseline shift. The product detection method of the organic electrochemical ammonia synthesis reaction system provides an accurate quantitative and performance evaluation method for the research of synthetic ammonia under an organic system. The invention can be used for ammonia product detection in an organic system.

Description

technical field [0001] The invention belongs to the field of electrochemical ammonia synthesis, and in particular relates to a product detection method of an organic electrochemical ammonia synthesis reaction system. Background technique [0002] The production of ammonia from free nitrogen is an extremely important industrial process. Electrochemical synthesis of ammonia is a promising new route that can realize hydrogenation from a wide range of sources at room temperature and pressure. 2 O and free nitrogen synthesize product ammonia, which has attracted widespread attention. However, the most thorny problem in the field of electrochemical ammonia synthesis is the low efficiency of ammonia production caused by difficult-to-activate nitrogen molecules and overwhelming competition for hydrogen evolution. In this context, researchers have turned their attention to the electrochemical synthesis of ammonia in organic systems. The organic electrolyte has a special ionic struc...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N21/33G01N21/78
CPCG01N21/33G01N21/78G01N2021/775
Inventor 丁良鑫任诗雨王海辉陈高锋
Owner SOUTH CHINA UNIV OF TECH
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