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A preparation method of MOFs material and its application in hydrogen isotope separation
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A hydrogen isotope, a certain amount of technology, applied in the application of hydrogen isotope separation, the field of preparation of MOFs materials, to achieve good separation selectivity, low risk, low energy consumption
Active Publication Date: 2022-03-29
MATERIAL INST OF CHINA ACADEMY OF ENG PHYSICS
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However, there are very limited reports on the efficient separation of hydrogen isotope gases at liquid nitrogen temperatures of 77K and above.
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preparation example Construction
[0035] Specifically, according to the present invention, a method for preparing MOFs materials is provided, comprising the steps of:
[0036] Step S1, a certain amount of MCl 2 Dissolved in a mixed solution of methanol and hydrochloric acid to obtain solution 1; H 2 BBTA is dissolved in DMF solution, denoted as solution 2, where, H 2 The mass of BBTA is MCl 2 0.5 to 10 times the amount of the substance, M is one of Ni, Co, Fe, Mn;
[0037]Step S2, mix solution 1 and solution 2 obtained in step S1 evenly, and place them in a hydrothermal reactor for reaction, wherein the temperature in the hydrothermal reactor is 50°C-100°C, and the reaction time is 24-72h;
[0038] Step S3, taking out the reaction product obtained in step S2 after cooling to room temperature, centrifuging to remove the supernatant under the condition of rotating speed of 5000r / min~10000r / min, washing and separating the precipitate to obtain M 2 Cl 2 BBTA material.
[0039] Specifically, M in the step S3 ...
Embodiment 1
[0047] Preparation of Ni 2 Cl 2 BBTA material.
[0048] Take 297mgNiCl 2 ·6H 2 O, add 20ml of methanol and 2ml of hydrochloric acidmixed solution, stir well, record as solution 1; add 100mg of H 2 BBTA was dissolved in 20ml of DMF solution, which was recorded as solution 2; mixed solution 1 and solution 2, stirred evenly, and placed in a polytetrafluoro reactor for reaction; put the polytetrafluoro reactor into an oven, and reacted at 75°C for 72 hours Finally, take it out, place it for centrifugation at a centrifugal speed of 5000r / min, then pour out the centrifugate, and wash three times with DMF solution and methanol solution respectively to obtain the blue solid Ni 2 Cl 2 BBTA material.
[0049] Ni 2 Cl 2 The microscopic morphology of BBTA material is as follows: figure 1 Shown, analyzed figure 1 It can be seen that the Ni 2 Cl 2 The microscopic morphology of BBTA material, in which, Figure a is the Ni at a scale of 3 μm 2 Cl 2 SEM image of BBTA material, pi...
Embodiment 2
[0051] Preparation of Co 2 Cl 2 BBTA material.
[0052] The reaction material used in this embodiment is CoCl 2 .
[0053] Take 100mgCoCl 2 ·6H 2 O, add 13ml of methanol and 0.2ml of hydrochloric acid mixed solution, stir well, record as solution 1; 66.5mg of H 2 BBTA was dissolved in 13ml of DMF solution, which was recorded as solution 2; mixed solution 1 and solution 2, stirred evenly, and placed in a polytetrafluoro reactor for reaction; put the polytetrafluoro reactor into an oven, and reacted at 75°C for 72 hours Finally, take it out, and place it for centrifugation at a centrifugal speed of 5000r / min, pour out the centrifugate, and wash three times with DMF solution and methanol solution respectively to obtain Co 2 Cl 2 BBTA material.
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Abstract
The invention discloses a preparation method of MOFs material, comprising the following steps: step S1, adding a certain amount of MCl 2 Dissolved in a mixed solution of methanol and hydrochloric acid to obtain solution 1; H 2 BBTA is dissolved in DMF solution, denoted as solution 2, where, H 2 The mass of BBTA is MCl 2 0.5 to 10 times the amount of the substance; step S2, mix the solution 1 and solution 2 obtained in step S1 evenly, and place them in a hydrothermal reaction kettle for reaction; step S3, cool the reaction product obtained in step S2 to room temperature Take out, centrifuge to remove the supernatant and wash and separate the precipitate to obtain M 2 Cl 2 BBTA material; prepared M 2 Cl 2 BBTA material undergoes displacement reaction with KF, KBr or KOH solution respectively, M 2 Cl 2 Cl in BBTA material ‑ replace with F ‑ 、Br ‑ or OH ‑ , get the corresponding M 2 x 2 BBTA material. The invention also provides the application of the MOFs material in hydrogenisotope separation. The preparation method of the invention is safe and simple; the prepared MOFs material has good hydrogenisotope separation selectivity at a temperature of 77K-100K; and the energy consumption is low when separating and selecting the hydrogenisotope.
Description
technical field [0001] The invention relates to the technical field of metal organic framework materials, in particular to a preparation method of MOFs material and its application in hydrogen isotope separation. Background technique [0002] Deuterium is a stable isotope of hydrogen, which has very important applications in scientific research and industry. Different from non-renewable energy and conventional clean energy, fusion energy has the advantages of unlimited resources, no pollution to the environment, and no high-radioactive nuclear waste. It is one of the dominant forms of human energy in the future. In a fusion reactor, deuterium gas is used as fuel to participate in the reaction, and the energy released by nuclear fusion of deuterium extracted from 1 liter of seawater is equivalent to the energy released by burning 300 liters of gasoline. Since the abundance of deuterium in natural hydrogen is only about 150ppm, while hydrogen (H) and deuterium (D) have almost...
Claims
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Application Information
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Patent Type & Authority Patents(China)
IPC IPC(8): C08G83/00B01D59/00B01J20/22
CPCC08G83/008B01D59/00B01J20/226
Inventor 冯兴文李信佟李敏王祥霖王泽骥姚伟志罗军洪何康昊宋江锋
Owner MATERIAL INST OF CHINA ACADEMY OF ENG PHYSICS
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