CN109928364B - Preparation method of deuterium - Google Patents
Preparation method of deuterium Download PDFInfo
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- CN109928364B CN109928364B CN201910328238.XA CN201910328238A CN109928364B CN 109928364 B CN109928364 B CN 109928364B CN 201910328238 A CN201910328238 A CN 201910328238A CN 109928364 B CN109928364 B CN 109928364B
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Abstract
The invention discloses a preparation method of deuterium, which sequentially comprises the following steps: 1. removing impurities from heavy water to less than 10‑6g/L; 2. heating to 1.5 atm and 403.15K superheated steam under pressure in a pressure kettle; 3. simultaneously feeding superheated steam and high-purity methane into a catalytic reactor, wherein the mol ratio of the superheated steam to the high-purity methane is 3:1, controlling the temperature in the reactor to be 1145-1155K and the pressure to be 1.8-2.2 atmospheric pressure, and keeping the temperature for 30-40 minutes; 4. introducing the mixed gas into a container, cooling and depressurizing to 1.2 atmospheric pressure and 375.15K; 5. purifying by a purifying tower; 6. circularly compressing to form mixed liquid with the temperature of 19.8K; 7. and (3) fractionating the mixed solution, keeping the temperature in the fractionating tower at 21.5K, and collecting the gas component hydrogen and the liquid component deuterium. The invention greatly reduces the energy consumption for preparing deuterium, and the obtained deuterium has higher purity.
Description
Technical Field
The invention belongs to the technical field of chemistry and chemical engineering, and relates to a preparation method of deuterium.
Background
Deuterium is an important scientific research material and an important raw material for novel energy nuclear fusion, widely exists in water in the nature, but the content of deuterium is very small, and data show that the content of deuterium in natural water is only 0.0125% -0.0145% of deuterium, so that it is very difficult to obtain high-concentration deuterium. At present, two methods for preparing deuterium are available, one is that natural water is enriched, heavy water containing deuterium is obtained by distillation and concentration, and then deuterium is obtained by electrolyzing the heavy water; the other method is to enrich the deuterium-containing aqueous solution by a "water-hydrogen sulfide exchange method", namely a GS method, and then obtain deuterium by electrolyzing the aqueous solution. The two methods have the defects that the energy consumption is large in the preparation process, the purity of the prepared deuterium is not high, and the raw material grade deuterium can be obtained through separation and concentration.
Disclosure of Invention
In view of the above, the present invention is directed to a novel method for producing deuterium, so as to reduce energy consumption during the process of producing deuterium and obtain deuterium with higher purity.
The technical scheme for realizing the purpose is that the method comprises the following steps:
(1) removing organic and inorganic impurities from deuterium-containing heavy water by osmotic membrane method, and detecting with ICP to obtain deuterium-containing heavy water with impurity content less than 10- 6g/L；
(2) Adding the heavy water after impurity removal into a pressure kettle, pressurizing and heating to generate superheated steam with the pressure of 1.5 atmospheres and the pressure of 403.15K;
(3) simultaneously feeding the superheated steam and the high-purity methane with the atmospheric pressure of 1.5 into a gas-phase catalytic reactor filled with a nickel catalyst and a cobalt catalyst, controlling the mol ratio of the superheated steam to the methane in the gas-phase catalytic reactor to be 3:1, controlling the temperature in the gas-phase catalytic reactor to be 1145-1155K, controlling the pressure to be 1.8-2.2 atmospheric pressure, and keeping the reaction time to be 30-40 minutes;
(4) introducing the mixed gas in the gas-phase catalytic reactor into a closed container, cooling and depressurizing to 1.2 atmospheric pressure, wherein the temperature is 375.15K;
(5) introducing the mixed gas in the step (4) into a gas purification tower filled with soda lime to remove carbon dioxide and residual water vapor;
(6) compressing the deuterium and hydrogen mixed gas purified in the step (5) into mixed liquid in a circulating mode through a compressor, wherein the temperature of the mixed liquid is 19.8K;
(7) fractionating the mixed liquid by an adsorption type fractionating tower filled with nickel, iron and manganese alloy, keeping the temperature in the fractionating tower at 21.5K, and collecting the gas component hydrogen and the liquid component deuterium.
The gas component obtained by fractionation is 98-99.99% of hydrogen gas and the liquid component is 84-88% of deuterium detected by a spectrum isotope detector.
The gas phase catalytic reactor in the step (3) is a stainless steel batch reactor with the diameter of 200cm and the length of 800 cm.
The purity of the methane in the step (3) is 99.99%.
The invention has the advantages of greatly reducing the energy consumption for preparing deuterium, simplifying the process flow, reducing the production equipment, obtaining deuterium with higher purity and obtaining high-purity hydrogen.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1
The preparation method of deuterium comprises the following steps:
(1) taking 100Kg of residual liquid containing deuterium and having the concentration of 11 percent after electrolysis;
(2) removing SO from the residual liquid by a permeable membrane process4 2-、Fe3+、Na+、Cl-Equal impurities, the content of the impurities is less than 10 by ICP detection-6g/L；
(3) Feeding the water after impurity removal into a stainless steel kettle with the capacity of 2 tons, the pressure resistance of 4 atmospheres and the resistance to 403K high temperature, and heating the water to form superheated steam with the pressure of 1.5 atmospheres and the temperature of 403.15K;
(4) introducing 17.8Kg of superheated steam into a stainless steel batch reactor with the diameter of 200cm and the length of 800cm through a pressure control and flow control valve, wherein the pressure resistance of the reactor is 3 atmospheric pressures, an alternating nickel and cobalt wire mesh is filled in the reactor, the reactor is heated to the temperature of 1150 +/-4K through plasma, introducing 4.5Kg of methane with the purity of 99.99 percent under the pressure of 1.5 atmospheric pressure while introducing the steam, and introducing the methane through the other pressure control and flow control valve; controlling the mol ratio of superheated steam to methane in the reactor to be 3:1, controlling the pressure in the reactor to be 1.8 +/-0.2 atmospheric pressure, guiding the reacted mixed gas into a closed container after 35 minutes, reducing the temperature and the pressure to be 1.2 atmospheric pressure, and controlling the temperature to be 375.15K;
(5) introducing the mixed gas in the step (4) into a gas purification tower filled with soda lime to remove carbon dioxide and residual water vapor;
(6) compressing the deuterium and hydrogen mixed gas purified in the step (5) into mixed liquid in a circulating mode through a compressor, wherein the temperature of the mixed liquid is 19.8K;
(7) fractionating the mixed liquid by an adsorption type normal pressure fractionating tower filled with nickel, iron and manganese alloy, keeping the temperature in the fractionating tower at 21.5K, and collecting gas component hydrogen and liquid component deuterium;
(8) and (4) repeating the steps (4) to (7), and combining the collected gas component hydrogen and the liquid component deuterium to obtain 19Kg of hydrogen with the content of 99.9 percent and 0.63Kg of deuterium with the content of 85 percent.
Example 2
(1) Taking 100Kg of deuterium-containing heavy water left after the distillation of tap water;
(2) removal of Mg from heavy water by osmotic membrane process2+、Ca2+、Na+、Fe3+、SO4 2-、Cl-After ICP detection, the content of impurities in the heavy water is less than 10-6g/L, the content of deuterium is 5 percent;
(3) the heavy water after impurity removal is sent into a stainless steel kettle with 2 ton capacity, pressure resistance of 4 atmospheres and 403K high temperature resistance, and is heated into superheated steam with 1.5 atmospheres and 403.15K temperature;
the subsequent steps were the same as the steps (4) to (8) described in example 1, and the collected gaseous component hydrogen and liquid component deuterium were combined to give 13.5Kg of hydrogen having a content of 99.9% and 0.213Kg of deuterium having a content of 85%.
Example 3
(1) Taking 1000Kg of seawater;
(2) removal of Na from seawater by osmotic membrane process+、Mg2+、Ca2+、K+、Fe3+、Ni2+、Mn2+、Cl-、Br-、I-、SO4 2-After ICP detection, the content of impurities in the heavy water is less than 10-6g/L, the content of deuterium is 0.0148%;
(3) feeding the seawater after impurity removal into a stainless steel kettle with the capacity of 2 tons, the pressure resistance of 4 atmospheres and the resistance to 403K high temperature, and heating the seawater into superheated steam with the pressure of 1.5 atmospheres and the temperature of 403.15K;
the subsequent steps were the same as the steps (4) to (8) described in example 1, and the collected gaseous component hydrogen and liquid component deuterium were combined to give 138Kg of hydrogen having a content of 99.99% and 0.0203Kg of deuterium having a content of 84%.
Claims (3)
1. The preparation method of deuterium is characterized by comprising the following steps in sequence:
(1) removing organic and inorganic impurities from deuterium-containing heavy water by osmotic membrane method, and detecting with ICP to obtain deuterium-containing heavy water with impurity content less than 10-6g/L；
(2) Adding the heavy water after impurity removal into a pressure kettle, pressurizing and heating to generate superheated steam with the pressure of 1.5 atmospheres and the pressure of 403.15K;
(3) simultaneously feeding the superheated steam and the high-purity methane with the atmospheric pressure of 1.5 into a gas-phase catalytic reactor filled with a nickel catalyst and a cobalt catalyst, controlling the mol ratio of the superheated steam to the methane in the gas-phase catalytic reactor to be 3:1, controlling the temperature in the gas-phase catalytic reactor to be 1145-1155K, controlling the pressure to be 1.8-2.2 atmospheric pressure, and keeping the reaction time to be 30-40 minutes;
(4) introducing the mixed gas in the gas-phase catalytic reactor into a closed container, cooling and depressurizing to 1.2 atmospheric pressure, wherein the temperature is 375.15K;
(5) introducing the mixed gas in the step (4) into a gas purification tower filled with soda lime to remove carbon dioxide and residual water vapor;
(6) compressing the deuterium and hydrogen mixed gas purified in the step (5) into mixed liquid in a circulating mode through a compressor, wherein the temperature of the mixed liquid is 19.8K;
(7) fractionating the mixed liquid by an adsorption type fractionating tower filled with nickel, iron and manganese alloy, keeping the temperature in the fractionating tower at 21.5K, and collecting gas component hydrogen and liquid component deuterium;
the gas component obtained by fractionation is 98-99.99% of hydrogen gas and the liquid component is 84-88% of deuterium detected by a spectrum isotope detector.
2. A process for the production of deuterium as claimed in claim 1, characterized in that: the gas phase catalytic reactor in the step (3) is a stainless steel batch reactor with the diameter of 200cm and the length of 800 cm.
3. A process for the production of deuterium as claimed in claim 1, characterized in that: the purity of the methane 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 |
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- 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 |
|---|
| 氘气中氢同位素的低温气相色谱法测定;韦桂欢等;《原子能科学技术》;20090220;第43卷(第2期);第144-146页 * |
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