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A preparation method of stable isotope 15n labeled nitrous oxide

A nitrous oxide and isotope technology, which is applied in the field of preparation of stable isotope 15N labeled nitrous oxide products, can solve problems such as harsh reaction conditions, side reactions, and cumbersome process operations, and achieve mild reaction conditions, reduce research and development costs, The effect of simple purification process

Active Publication Date: 2015-12-16
SHANGHAI RES INST OF CHEM IND
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  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

[0009] The above method may be suitable for the preparation of natural abundant nitrous oxide, but for the preparation of isotope gas, there are some disadvantages: the process of method 1 is difficult to control, and there is still a danger of explosion due to the high temperature heating of ammonium nitrate; method 2 The temperature in the process is very sensitive to the reaction. If the temperature is not well controlled, a side reaction will occur, that is, an equimolar amount of nitrous oxide and carbon dioxide will be generated, which will increase the difficulty of separating the mixed gas; in the process of method 3, not only precious metals should be used Catalysts increase the cost of raw materials, and the reaction needs to be completed under high temperature and high pressure, and the reaction conditions are harsh
The purification technologies disclosed above are all used in the industrial production of nitrous oxide, and have the characteristics of cumbersome process operation, high economic cost of purification and harsh purification process conditions, and are not suitable for stable isotope 15 Preparation of N-labeled nitrous oxide

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Accurately weigh 7g 15N-labeled hydroxylamine hydrochloride (provided by Shanghai Institute of Chemical Industry, abundance 99.16atom%, purity > 99%), and its preparation concentration is 20% aqueous solution, joins in the dropping funnel; Accurately weigh 14.1gNa 15 NO 2 (provided by Shanghai Research Institute of Chemical Industry, abundance 99.16atom%, purity > 99%), and it is mixed with the aqueous solution that concentration is 20%, joins in the gas generating bottle, 15 N labeled hydroxylamine hydrochloride and Na 15 NO 2 The molar ratio should be 0.5:1; connect the experimental device, the gas generating bottle is connected to the dryer, cold trap, sampling tube and air bag in sequence, and the gas generating system is connected to the vacuum oil pump and helium. Vacuumize the gas generating system and replace it with helium, keep the system in a negative pressure state for 30 minutes, add dropwise the aqueous solution of hydroxylamine hydrochloride at a rate ...

Embodiment 2

[0039] Adopt the same operating steps as in Example 1, but change some of the conditions: accurately weighed 7g 15 N-marked hydroxylamine hydrochloride is prepared into an 80% aqueous solution, 15 N labeled hydroxylamine hydrochloride and Na 15 NO 2 The molar ratio should be 1:1, and the Na 15 NO 2 Should be 7.05g, reaction temperature is 50 ℃, and the reaction time is 3h, collects and obtains gas 1.20L, and yield is 53.57% (with 15 N marks hydroxylamine hydrochloride meter). Sampling was sent to gas chromatograph and isotope mass spectrometer for analysis. It can be seen from the analysis that the generated 15 The purity of N-labeled nitrous oxide gas is ≥99.0%, the abundance is ≥99.08atom%, the oxygen content is ≤0.19%, and the carbon dioxide content is ≤0.24%.

Embodiment 3

[0041] Adopt the same operating steps as in Example 1, but change some of the conditions: 3.53gNa accurately weighed 15 NO 2 Prepared as a 70% aqueous solution, 15 N labeled hydroxylamine hydrochloride and Na 15 NO 2 The mol ratio should be 2: 1, and the temperature of reaction is 70 ℃, collects and obtains gas 1.05L, and yield is 46.88% (with 15 N marks hydroxylamine hydrochloride meter). Sampling was sent to gas chromatograph and isotope mass spectrometer for analysis. It can be seen from the analysis that the generated 15 The purity of N-labeled nitrous oxide gas is ≥99.0%, the abundance is ≥99.15atom%, the oxygen content is ≤0.18%, and the carbon dioxide content is ≤0.20%.

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Abstract

The invention relates to a method for preparing stable isotope 15N marked nitrous oxide. The method comprises the followings steps of: making a stable isotope 15N marked sodium nitrite (15N-NaNO2) aqueous solution of certain concentration react with a stable isotope 15N marked hydroxylamine hydrochloride (15N-NH2OH.HCl) aqueous solution at the temperature of 20-120 DEG C for 1-5 hours; and separating obtained 15N marked nitrous oxide gas from mixed gas. Compared with the prior art, the method has the advantages of mild reaction conditions, freeness from explosion danger, no need of any expensive precious metal catalyst, simple post-treatment purification process of a reaction process, reduction in the quantity of factors influencing isotope abundance dilution in a reaction process, and capability of better ensuring that the abundance of a 15N marked isotope gas product is not diluted.

Description

technical field [0001] The invention belongs to the field of stable isotope-labeled compound production, and relates to a laboratory preparation method for a stable isotope-labeled gas, in particular to a stable isotope 15 N labeled nitrous oxide ( 15 N-N 2 O) The method of preparation of the product. Background technique [0002] Climate change is a major challenge facing the world today. It is the common mission of all mankind to curb climate warming and save the home of the earth. The natural greenhouse effect of the Earth system keeps the Earth's surface temperature within a range suitable for human existence. However, with the intensification of human activities such as burning of fossil fuels and deforestation, atmospheric CO 2 、CH 4 and N 2 The increasing concentration of greenhouse gases such as O has greatly enhanced the Earth's natural greenhouse effect, leading to global warming. The global warming phenomenon caused by the greenhouse effect is intensifying...

Claims

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Application Information

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IPC IPC(8): C01B21/22
Inventor 王伟杜晓宁宋明鸣田小叶李杰周建跃
Owner SHANGHAI RES INST OF CHEM IND
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