CN109928364A - A kind of preparation method of deuterium - Google Patents
A kind of preparation method of deuterium Download PDFInfo
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- CN109928364A CN109928364A CN201910328238.XA CN201910328238A CN109928364A CN 109928364 A CN109928364 A CN 109928364A CN 201910328238 A CN201910328238 A CN 201910328238A CN 109928364 A CN109928364 A CN 109928364A
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Abstract
The invention discloses a kind of preparation method of deuterium, successively step is: 1, heavy water cleaning, impurity is less than 10‑6g/L；2, in autoclave pressure pressurized, heated to 1.5 atmospheric pressure, the overheated steam of 403.15K；3, overheated steam and high-purity methane are sent into catalytic reactor simultaneously, the mol ratio of the two is 3:1, and controlling the temperature in reactor is 1145~1155K, and pressure is 1.8~2.2 atmospheric pressure, is kept for 30-40 minutes；4, mixed gas is directed in container, decrease temperature and pressure to 1.2 atmospheric pressure, 375.15K；5, it is purified by purifying column；6, circulation is compressed into the mixing liquid that temperature is 19.8K；7, mixed liquor is fractionated, it is 21.5K that temperature is kept in fractionating column, collects gas composition hydrogen and liquid component deuterium.The present invention considerably reduces the energy consumption of deuterium processed, and the purity of gained deuterium is higher.
Description
Technical field
The invention belongs to technical field of chemistry and chemical engineering, are related to a kind of preparation method of deuterium.
Background technique
Deuterium is a kind of important scientific research material, is also important the raw material of new energy nuclear fusion, it is deposited extensively
It is in the water of nature, but its content is little, data is shown, the content of deuterium is only 0.0125%~0.0145% in Natural Water
Deuterium, therefore, the deuterium that obtain high concentration is extremely not easy.Currently, there are two ways to producing deuterium, one is enrichment Natural Water,
By distillation and concentration, the heavy water containing deuterium is obtained, deuterium is then obtained by electrolysis heavy water；Another kind is by " water --- hydrogen sulfide
Exchange process ", i.e. GS method are enriched with the aqueous solution containing deuterium, then obtain deuterium by being electrolysed the aqueous solution.There is systems for both methods
Greatly for energy consumption in the process, deuterium purity prepared by is not high, needs to be separated and be concentrated again the deuterium that could obtain raw material grade.
Summary of the invention
In view of this, preparing deuterium it is an object of the invention to propose a kind of preparation method of new deuterium to reduce
Energy consumption in the process, and the deuterium of higher degree can be obtained.
The technical solution for realizing above-mentioned purpose is to be sequentially completed in the steps below:
(1) deuterium heavy water infiltration film method will be contained and remove organic and inorganic impurity, detected through ICP, impurity content is less than 10- 6g/L；
(2) pressurization in autoclave pressure, heating is added in the heavy water after above-mentioned removal of impurities, generates the mistake of 1.5 atmospheric pressure, 403.15K
Hot steam；
(3) overheated steam of the step (2) and high-purity methane with 1.5 atmospheric pressure are sent into simultaneously and are filled with
Nickel, Co catalysts gas phase catalytic reaction device in, control mol ratio in the gas phase catalytic reaction device of overheated steam and methane
For 3:1, the temperature in the gas phase catalytic reaction device is 1145~1155K, and pressure is 1.8~2.2 atmospheric pressure, is kept for the reaction time
It is 30-40 minutes；
(4) mixed gas in gas phase catalytic reaction device is directed in a closed container, decrease temperature and pressure to 1.2 atmosphere
Pressure, temperature 375.15K；
(5) mixed gas of the step (4) is passed through in the gas purification tower filled with soda lime, removes carbon dioxide
With remaining water vapour；
(6) it will be compressed into mixing liquid through compressor cycle by the step (5) purified deuterium, hydrogen mixed gas,
Its temperature is 19.8K；
(7) mixing liquid is fractionated by the absorption type fractionating column filled with nickel, iron, manganese alloy, is protected in fractionating column
Holding temperature is 21.5K, collects gas composition hydrogen and liquid component deuterium.
Through spectroscopic isotope detector test, the hydrogen that fractionation gained gas component is 98%~99.99%, liquid component
For 84%~88% deuterium.
Gas phase catalytic reaction device in the step (3) is that diameter is 200cm, and length is that the stainless steel of 800cm is intermittent
Reactor.
Methane purity in the step (3) is 99.99%.
The advantage of the invention is that considerably reducing the energy consumption of deuterium processed, process flow has been simplified, has reduced production
The purity of equipment, gained deuterium is higher, while obtaining the hydrogen of high-purity.
Specific embodiment
Below with reference to embodiment, the invention will be further described.
Embodiment 1
A kind of preparation method of deuterium, is sequentially completed in the steps below:
(1) the Liquid Residue 100Kg that the heavy water concentration containing deuterium is 11% after being electrolysed is taken；
(2) SO in the Liquid Residue is removed with infiltration film method4 2-、Fe3+、Na+、Cl-Equal impurity, are detected through ICP, miscellaneous
Matter content is less than 10-6g/L；
(3) water after removal of impurities is sent into the stainless steel kettle of 2 tons of capacity, pressure-resistant 4 atmospheric pressure, the high temperature of resistance to 403K, through adding
The overheated steam that heat becomes 1.5 atmospheric pressure, temperature is 403.15K；
(4) 17.8Kg superheated vapour is introduced diameter through pressure control, flow control valve is 200cm, and length is 800cm stainless steel
In batch reactor, which is 3 atmospheric pressure, is filled with alternative expression nickel, cobalt wire mesh in reactor, instead
Answering device to pass through heating plasma to temperature is 1150 ± 4K, and the purity that pressure is 1.5 atmospheric pressure is introduced while introducing water vapour
For 99.99% methane 4.5Kg, methane is introduced by another pressure control, flow control valve；Control superheated vapour and methane in the reactor
Mol ratio be 3:1, the pressure in reactor, which is controlled, exports the mixed gas of reaction after 1.8 ± 0.2 atmospheric pressure, 35 minutes
Into a closed container, decrease temperature and pressure to 1.2 atmospheric pressure, temperature 375.15K；
(5) mixed gas of the step (4) is passed through in the gas purification tower filled with soda lime, removes carbon dioxide
With remaining water vapour；
(6) it will be compressed into mixing liquid through compressor cycle by the step (5) purified deuterium, hydrogen mixed gas,
Its temperature is 19.8K；
(7) mixing liquid is fractionated by the absorption type atmospheric fractional tower filled with nickel, iron, manganese alloy, fractionating column
Interior holding temperature is 21.5K, collects gas composition hydrogen and liquid component deuterium；
(8) step (4)~(7) are repeated, merge the gas composition hydrogen and liquid component deuterium being collected into, content, which is obtained, is
The deuterium 0.63Kg that 99.9% hydrogen 19Kg and content is 85%.
Embodiment 2
(1) the remaining 100Kg of heavy water containing deuterium after distilling is taken by tap water；
(2) Mg in heavy water is removed with infiltration film method2+、Ca2+、Na+、Fe3+、SO4 2-、Cl-Equal impurity, are detected through ICP,
Impurity content is less than 10 in heavy water-6G/L, the content of deuterium are 5%；
(3) heavy water after removal of impurities is sent into the stainless steel kettle of 2 tons of capacity, pressure-resistant 4 atmospheric pressure, the high temperature of resistance to 403K, warp
It is heated as 1.5 atmospheric pressure, the overheated steam that temperature is 403.15K；
Subsequent step is homogeneously same as step described in embodiment 1 (4)~(8), merges the gas composition hydrogen and liquid being collected into
The hydrogen 13.5Kg that content is 99.9% and the deuterium 0.213Kg that content is 85% is obtained in component deuterium.
Embodiment 3
(1) seawater 1000Kg is taken；
(2) Na in seawater is removed with infiltration film method+、Mg2+、Ca2+、K+、Fe3+、Ni2+、Mn2+、Cl-、Br-、I-、SO4 2-
Equal impurity, are detected, impurity content is less than 10 in heavy water through ICP-6G/L, the content of deuterium are 0.0148%；
(3) seawater after removal of impurities is sent into the stainless steel kettle of 2 tons of capacity, pressure-resistant 4 atmospheric pressure, the high temperature of resistance to 403K, warp
It is heated as 1.5 atmospheric pressure, the overheated steam that temperature is 403.15K；
Subsequent step is homogeneously same as step described in embodiment 1 (4)~(8), merges the gas composition hydrogen and liquid being collected into
The hydrogen 138Kg that content is 99.99% and the deuterium 0.0203Kg that content is 84% is obtained in component deuterium.
Claims (3)
1. a kind of preparation method of deuterium, it is characterized in that being sequentially completed in the steps below:
(1) deuterium heavy water infiltration film method will be contained and remove organic and inorganic impurity, detected through ICP, impurity content is less than 10-6g/L；
(2) pressurization in autoclave pressure, heating is added in the heavy water after above-mentioned removal of impurities, generates the superheated water of 1.5 atmospheric pressure, 403.15K
Steam；
(3) by the overheated steam of the step (2) and high-purity methane with 1.5 atmospheric pressure be sent into simultaneously filled with nickel,
In the gas phase catalytic reaction device of Co catalysts, controlling the mol ratio of overheated steam and methane in the gas phase catalytic reaction device is
3:1, the temperature in the gas phase catalytic reaction device are 1145~1155K, and pressure is 1.8~2.2 atmospheric pressure, are kept for the reaction time be
30-40 minutes；
(4) mixed gas in gas phase catalytic reaction device is directed in a closed container, decrease temperature and pressure to 1.2 atmospheric pressure, temperature
Degree is 375.15K；
(5) mixed gas of the step (4) is passed through in the gas purification tower filled with soda lime, removes carbon dioxide and remained
Remaining water vapour；
(6) it will be compressed into mixing liquid through compressor cycle by the step (5) purified deuterium, hydrogen mixed gas, temperature
Degree is 19.8K；
(7) mixing liquid is fractionated by the absorption type fractionating column filled with nickel, iron, manganese alloy, temperature is kept in fractionating column
Degree is 21.5K, collects gas composition hydrogen and liquid component deuterium.
Through spectroscopic isotope detector test, it is fractionated the hydrogen that gained gas component is 98%~99.99%, liquid component is
84%~88% deuterium.
2. a kind of preparation method of deuterium as described in claim 1, it is characterised in that: the gas phase catalysis in the step (3) is anti-
Answering device is diameter for 200cm, and length is the stainless steel batch reactor of 800cm.
3. a kind of preparation method of deuterium as described in claim 1, it is characterised in that: the methane purity in the step (3) is
99.99%.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1364714A (en) * | 1970-10-28 | 1974-08-29 | Gulf Research Development Co | Process for obtaining deuterium from hydrogen containing compoun ds and the production of heavy water therefrom |
| DE3118431A1 (en) * | 1981-05-09 | 1982-12-09 | Martin Dr. 3000 Hannover Schoell | Process and device for isotope separation for the enrichment of deuterium and for the preparation of heavy water |
| CN1834002A (en) * | 2005-03-15 | 2006-09-20 | 大连世纪欣科高新技术开发有限公司 | Method of producing super-high pure tritium gas by utilizing heavy-water as raw material |
| CN101264862A (en) * | 2007-03-16 | 2008-09-17 | 柯香文 | Method for preparing heavy water and deuterium gas |
-
2019
- 2019-04-23 CN CN201910328238.XA patent/CN109928364B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1364714A (en) * | 1970-10-28 | 1974-08-29 | Gulf Research Development Co | Process for obtaining deuterium from hydrogen containing compoun ds and the production of heavy water therefrom |
| DE3118431A1 (en) * | 1981-05-09 | 1982-12-09 | Martin Dr. 3000 Hannover Schoell | Process and device for isotope separation for the enrichment of deuterium and for the preparation of heavy water |
| CN1834002A (en) * | 2005-03-15 | 2006-09-20 | 大连世纪欣科高新技术开发有限公司 | Method of producing super-high pure tritium gas by utilizing heavy-water as raw material |
| CN101264862A (en) * | 2007-03-16 | 2008-09-17 | 柯香文 | Method for preparing heavy water and deuterium gas |
Non-Patent Citations (1)
| Title |
|---|
| 韦桂欢等: "氘气中氢同位素的低温气相色谱法测定", 《原子能科学技术》 * |
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