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Preparation method of high-purity deuterated ammonia

A high-purity, deuterated technology, used in the preparation/separation of ammonia, chemical instruments and methods, ammonia compounds, etc., can solve problems such as being unsuitable for large-scale industrial production, easy to burn magnesium powder in the air, and high price of heavy water. , to achieve the effect of small footprint, mature and controllable process route, and reduced raw material cost

Pending Publication Date: 2022-05-17
PERIC SPECIAL GASES CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the reactant magnesium powder used in this method is easy to burn in the air, and the production process is very dangerous, so it is not suitable for large-scale industrial production.
In addition, the price of heavy water is high, and the by-product deuterated magnesium oxide generated by the preparation of deuterated ammonia will consume a part of deuterium atoms, so that the utilization rate of deuterium atoms is only 50%, which greatly increases the cost of raw materials
Therefore, this method can only be used in the laboratory to prepare a small amount of deuterated ammonia for tracer research.

Method used

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  • Preparation method of high-purity deuterated ammonia

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Comparison scheme
Effect test

Embodiment 1

[0032] Such as figure 1 Shown, the preparation method of the high-purity deuterated ammonia of the present embodiment comprises the following steps:

[0033] S1, 12kg of high-purity deuterium 2 with a purity of 99.999% and an abundance of 99.6% and 28kg of high-purity nitrogen 1 with a purity of 99.999% are passed into the feed buffer tank V101 with a pressure of 3MPa, and the mixture is high-purity nitrogen and High-purity deuterium raw material gas 3, high-purity nitrogen and high-purity deuterium raw material gas 3 are pressurized to 15MPa by the feed compressor C101 to obtain pressurized raw material gas 4, and the pressurized raw material gas 4 is combined with After the deuterium nitrogen circulating gas 16 is mixed in the buffer tank V102, the mixed gas 5 is obtained, and the mixed gas 5 is heated to 350°C by the heat exchanger E101 to obtain the heated mixed gas 6, and the heated mixed gas is 6 is passed into the reactor R101 to react to obtain the reaction mixture 7;...

Embodiment 2

[0042] The preparation method of the high-purity deuterated ammonia of the present embodiment, as figure 1 shown, including the following steps:

[0043] S1, 12kg of high-purity deuterium 2 with a purity of 99.999% and an abundance of 99.6% and 28kg of high-purity nitrogen 1 with a purity of 99.999% are passed into the feed buffer tank V101 with a pressure of 3MPa, and the mixture is high-purity nitrogen and High-purity deuterium raw material gas 3, high-purity nitrogen and high-purity deuterium raw material gas 3 are pressurized to 30MPa by the feed compressor C101 to obtain pressurized raw material gas 4, and the pressurized raw material gas 4 is combined with After the deuterium nitrogen circulating gas 16 is mixed in the buffer tank V102, the mixed gas 5 is obtained, and the mixed gas 5 is heated to 300°C by the heat exchanger E101 to obtain the heated mixed gas 6, and the heated mixed gas is 6 is passed into the reactor R101 to react to obtain the reaction mixture 7;

...

Embodiment 3

[0052] The preparation method of the high-purity deuterated ammonia of the present embodiment, as figure 1 shown, including the following steps:

[0053] S1, 12kg of high-purity deuterium 2 with a purity of 99.999% and an abundance of 99.6% and 28kg of high-purity nitrogen 1 with a purity of 99.999% are passed into the feed buffer tank V101 with a pressure of 3MPa, and the mixture is high-purity nitrogen and High-purity deuterium raw material gas 3, high-purity nitrogen and high-purity deuterium raw material gas 3 are pressurized to 15MPa by the feed compressor C101 to obtain pressurized raw material gas 4, and the pressurized raw material gas 4 is combined with After the deuterium nitrogen circulating gas 16 is mixed in the buffer tank V102, the mixed gas 5 is obtained, and the mixed gas 5 is heated to 350°C by the heat exchanger E101 to obtain the heated mixed gas 6, and the heated mixed gas is 6 is passed into the reactor R101 to react to obtain the reaction mixture 7;

...

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Abstract

The invention provides a preparation method of high-purity deuterated ammonia, which comprises the following steps: mixing high-purity deuterium gas and high-purity nitrogen gas to obtain high-purity nitrogen gas and high-purity deuterium gas feed gas, pressurizing the high-purity nitrogen gas and the high-purity deuterium gas feed gas, mixing the pressurized high-purity nitrogen gas and high-purity deuterium gas feed gas with deuterium-nitrogen recycle gas, heating, and introducing into a reactor for reaction to obtain reaction mixed gas; sequentially introducing the reaction mixed gas into a high-pressure flash tank and a low-pressure flash tank to obtain a deuterated ammonia liquid crude product; introducing the deuterated ammonia liquid crude product into a light component removal tower to remove light component impurities so as to obtain refined deuterated ammonia; and introducing the refined deuterated ammonia into a heavy component removal tower to remove heavy component impurities so as to prepare the high-purity deuterated ammonia. The whole process route is mature and controllable, large-scale industrial production can be quickly realized, the deuterium atom utilization rate is high, the equipment investment is low, the occupied area is small, and the economic benefit is high.

Description

technical field [0001] The invention belongs to the technical field of gas preparation, and in particular relates to a method for preparing high-purity deuterated ammonia. Background technique [0002] Deuterated ammonia (ND 3 , also known as deuterium ammonia, heavy ammonia), colorless with a strong pungent gas, toxic, highly corrosive, non-flammable, soluble in water. Deuterated ammonium is commonly used in gigabyte random access memory manufacturing processes to generate deuterium to form passivation layers of silicon nitride and silicon oxynitride to increase specific transistor lifetimes. [0003] The current method for preparing high-purity deuterated ammonia is to use metal nitrides and heavy water to react. Jin Zhong In the published paper "Preparation and Stability of Deuterated Ammonia", magnesium powder and high-purity nitrogen were used to react at a high temperature of 950°C to prepare high-purity magnesium nitride, and then under normal temperature and vacu...

Claims

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Application Information

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IPC IPC(8): C01C1/04C01C1/02
CPCC01C1/0411C01C1/0458C01C1/024Y02P20/52
Inventor 孟祥军许春建花莹曦岳立平田金金苏子杰黄英
Owner PERIC SPECIAL GASES CO LTD
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