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Preparation method of high-purity deuterated ammonia

A deuterated, high-purity technology, applied in the field of preparation of deuterated ammonia, can solve the problems of low purity of deuterated ammonia products, low utilization rate of deuterium atoms, etc., and achieves easy large-scale industrial production, safe and controllable technological process, and reaction mild conditions

Active 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

[0009] It can be seen that the hydrogen-deuterium exchange method is very suitable for industrial production of high-purity deuterated ammonia, but the hydrogen-deuterium exchange reaction will generate intermediate products NDH, NDH 2 and HDO, resulting in low purity of the deuterated ammonia product and low utilization of deuterium atoms

Method used

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  • Preparation method of high-purity deuterated ammonia
  • Preparation method of high-purity deuterated ammonia
  • Preparation method of high-purity deuterated ammonia

Examples

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Effect test

Embodiment 1

[0047] The preparation method of the pure deuterated ammonia of the present embodiment, the method is:

[0048] S1, feed the raw material heavy water stream 2 of the raw material ammonia stream 1 of 170kg / hr and 2000kg / hr into the reactive distillation tower T101, and be rectification under the condition of 1.0MPa under pressure, and extract at the tower top of described reactive rectification tower Deuterated ammonia crude product stream 3 is produced, and the dilute heavy water stream 4 is extracted in the tower still of the reactive distillation tower T101; wherein the mol ratio of heavy water and ammonia in the raw material heavy water stream 2 and the raw material ammonia stream 1 is 10:1; The theoretical plate number of the reactive distillation column T101 is 50, the reflux ratio is 10, the top temperature of the reactive distillation column T101 is 10°C, and the bottom temperature of the reactive distillation column T101 is 160°C;

[0049] S2. Pass the deuterated ammon...

Embodiment 2

[0062] The preparation method of the pure deuterated ammonia of the present embodiment, the method is:

[0063] S1, feed the raw material heavy water stream 2 of the raw material ammonia stream 1 of 170kg / hr and 1600kg / hr into the reactive distillation tower T101, be that rectification under the condition of 0.4MPa under pressure, extract at the tower top of described reactive rectification tower Deuterated ammonia crude product stream 3 is produced, and the dilute heavy water stream 4 is extracted in the tower still of the reactive distillation tower T101; wherein the mol ratio of heavy water and ammonia in the raw material heavy water stream 2 and the raw material ammonia stream 1 is 8:1; The theoretical plate number of the reactive distillation column T101 is 80, the reflux ratio is 5, the top temperature of the reactive distillation column T101 is 0°C, and the bottom temperature of the reactive distillation column T101 is 145°C;

[0064] S2, pass the deuterated ammonia cru...

Embodiment 3

[0074] The preparation method of the pure deuterated ammonia of the present embodiment, the method is:

[0075]S1, feed the raw material heavy water stream 2 of the raw material ammonia stream 1 of 170kg / hr and 200kg / hr into the reactive distillation tower T101, and be rectification under the condition of 2.0MPa under pressure, extract at the tower top of described reactive rectification tower Deuterated ammonia crude product stream 3 is produced, and the rare heavy water stream 4 is extracted in the tower still of the reactive distillation tower T101; wherein the mol ratio of heavy water and ammonia in the raw material heavy water stream 2 and the raw material ammonia stream 1 is 1:1; The theoretical plate number of the reactive distillation column T101 is 30, the reflux ratio is 20, the top temperature of the reactive distillation column T101 is 50°C, and the bottom temperature of the reactive distillation column T101 is 212°C;

[0076] S2, pass the deuterated ammonia crude ...

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Abstract

The invention provides a preparation method of high-purity deuterated ammonia, which comprises the following steps: introducing heavy water and ammonia gas into a reactive distillation tower for rectification, extracting a deuterated ammonia crude product from the tower top of the reactive distillation tower, and extracting dilute heavy water from the tower kettle; the deuterated ammonia crude product is introduced into an ammonia recovery tower for reaction, an ammonia-containing intermediate product is extracted from the tower top of the ammonia recovery tower and circularly enters the reactive distillation tower for distillation, and a product containing deuterated ammonia and water and the ammonia-containing intermediate product are extracted from the tower kettle of the ammonia recovery tower; the dilute heavy water is introduced into a heavy water recovery tower for reaction, a product containing HDO and heavy water is extracted from a tower kettle of the heavy water recovery tower and enters a rectification tower for rectification, and wastewater is extracted from the top of the heavy water recovery tower and discharged; the product containing deuterated ammonia and water is introduced into a deuterated ammonia purification tower for reaction, and a product containing deuterated water and water is extracted from a tower kettle and enters a reactive distillation tower for continuous distillation; and high-purity deuterated ammonia is extracted from the tower top of the deuterated ammonia purifying tower. The method is mild in reaction condition, mature in process, simple in route, safe, controllable and easy for large-scale industrial production.

Description

technical field [0001] The invention belongs to the technical field of preparation of deuterated ammonia, and in particular relates to a preparation method of 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. High-purity 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] At present, the methods for preparing deuterated ammonia mainly include metal nitride hydrolysis method and hydrogen-deuterium exchange method. In the published literature, Jin Zhong etc. in "Preparation and Stability of Deuterated Ammonia" (Jin Zhong Sun Linghong, Ye Zhuang. Preparation and stability of deuterated ammonia[J]. Atomic Energy...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B4/00
CPCC01B4/00Y02P20/10
Inventor 孟祥军许春建冀延治吕随强倪珊珊蒋玉虎张帅
Owner PERIC SPECIAL GASES CO LTD
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