Preceding-stage separation device for D2O and H2O

Abstract

The utility model relates to a preceding-stage separation device for D2O and H2O, and belongs to the field of chemical equipment. The preceding-stage separation device comprises a separation column module, a separation column tank, a pressure pipeline, a circulating water pump, a solvent tank and a recovery tank, according to the device, the content of D2O in water can be increased by utilizing the difference of the diffusion rates of different solvents in ZIF8, further separation of D2O and H2O is facilitated, and compared with an existing separation method, the device can greatly reduce energy consumption and consumable cost, and is suitable for large-scale production. The current green and environment-friendly concept is met.

Description

TECHNICAL FIELD

[0001] The utility model relates to the technical field of chemical equipment, concretely relates to the primary separation device of integrated separation device of continuous flow method. BACKGROUND

[0002] The content of D2O in water in nature is usually very low. Deuterium (D) is a stable isotope of hydrogen, and its natural abundance in nature is about 0.0156%. This means that in water in nature, about 1 out of every 6400 hydrogen atoms is a deuterium atom. In order to increase the content of D2O in water, further separate D2O and H2O, there are currently some separation technologies, such as low-temperature distillation method, chemical exchange method, membrane separation technology, etc. But these separation methods still face some technical and economic difficulties. For example, low-temperature distillation method requires very low temperature and high pressure conditions, and the energy consumption is very high. Although the separation efficiency is high, the cost of large-scale application is difficult to bear; chemical exchange method needs multiple cycles and processing of a large amount of chemical byproducts, and the overall efficiency is still low; the cost of membrane material of membrane separation technology is high, and it needs to be replaced or regenerated regularly, increasing the operation cost, etc. Therefore, in the face of the above problems, how to efficiently separate D2O and H2O is still a current problem. SUMMARY

[0003] In view of the problems existing in the prior art, the utility model provides a kind of D2O and H2O's front stage separation device, and operator can quickly and efficiently realize the front stage separation of D2O and H2O by the D2O and H2O's front stage separation device, and it is easy to operate, green and environmental protection.

[0004] In order to solve the technical problem of the present application, the technical scheme is as follows: a kind of D2O and H2O's front stage separation device, the front stage separation device includes: sample introduction unit, mixing unit, recovery unit;Sample introduction unit is communicated with mixing unit, mixing unit is communicated with recovery unit, recovery unit is communicated with sample introduction unit;

[0005] The sample introduction unit includes first solvent tank (1) and second solvent tank (2), one side of first solvent tank (1) is communicated with the inlet end of first pressure pipeline (3), the outlet end of first pressure pipeline (3) is communicated with separation column tank (8), the inlet end of second pressure pipeline (4) is communicated with second solvent tank (2), the outlet end of second pressure pipeline (4) is communicated with separation column tank (8);

[0006] The mixing unit includes separation column tank (8), separation column tank (8) contains separation column module (7), the two sides of separation column tank (8) are respectively communicated with the outlet end of first pressure pipeline (3) and second pressure pipeline (4), the two sides of separation column tank (8) are respectively communicated with the inlet end of third pressure pipeline (9) and fourth pressure pipeline (10).

[0007] The recovery unit comprises a recovery tank chamber one (13) and a recovery tank chamber two (14), the two chambers are communicated by a round hole channel (15), a separation device polyamide reverse osmosis membrane (16) is installed in the recovery tank chamber two (14), and the recovery tank chamber one (13) is communicated with the outlet ends of the third pressure pipeline (9) and the fourth pressure pipeline (10) on the two sides respectively; the recovery tank chamber two (14) is communicated with the inlet ends of the fifth pressure pipeline (17) and the sixth pressure pipeline (18) on the two sides respectively, and the fifth pressure pipeline (17) and the sixth pressure pipeline (18) respectively deliver liquid back to the first solvent tank (1) and the second solvent tank (2).

[0008] Preferably, the separation column tank (8) contains 11 separation column modules (7), and the separation column module (7) is a block-shaped filter element synthesized by pressing operation of graphite and ZIF8. 2-methyl imidazole reacts with zinc acetate to generate metal organic framework material ZIF8, and sodium fluorescein is directly embedded in the channel of the ZIF8 framework structure in the process of forming the ZIF8 framework structure; the molar ratio of 2-methyl imidazole, zinc acetate and sodium fluorescein is 1203:60.2:1, and the separation column module (7) is filled with ZIF8 to realize the amplification of the difference between the diffusion rate of methanol to D2O and H2O and the diffusion rate of D2O and H2O to methanol.

[0009] Preferably, the first pressure pipeline (3), the second pressure pipeline (4), the third pressure pipeline (9), the fourth pressure pipeline (10), the fifth pressure pipeline (17) and the sixth pressure pipeline (18) are respectively provided with a first circulating water pump (5), a second circulating water pump (6), a third circulating water pump (11), a fourth circulating water pump (12), a fifth circulating water pump (19) and a sixth circulating water pump (20) to control the inflow and outflow and flow rate of liquid.

[0010] Preferably, the first circulating water pump (5), the second circulating water pump (6), the third circulating water pump (11), the fourth circulating water pump (12), the fifth circulating water pump (19) and the sixth circulating water pump (20) are controlled and adjusted by a total control panel (22), the total control panel (22) comprises a flow rate key, a start key and a stop key, and the flow rate key can adjust the flow rate.

[0011] Preferably, the front of the separation column tank (8) comprises a visual window for observing the internal condition.

[0012] Preferably, the separation column tank cover (21) is arranged above the separation column module (7) to ensure the isolation between the inside and the outside.

[0013] Beneficial effects:

[0014] The device can realize the increase of the content of D2O in water by using the difference in the diffusion rate of different solvents D2O and H2O in ZIF8, which is conducive to further separating D2O and H2O, and compared with the existing separation method, the device can greatly reduce the energy consumption and the cost of consumables, and conforms to the current green and environmental protection concept.

[0015] Compared with the prior art, the device has simple structure, mild operation condition, significantly reduced energy consumption, more economical and environmental separation process, and improved universal applicability of the device. The separation device utilizes the lower diffusion rate of D2O than H2O in ZIF8, so that more D2O is retained in the separation column module 7 after multiple flow circulation, and finally all the pipelines are closed, the separation column module 7 in the separation column tank 8 is taken out, a mixed solution with high content of D2O is obtained, the pre-separation of D2O and H2O is realized, and high-purity D2O can be further obtained. BRIEF DESCRIPTION OF DRAWINGS

[0016] Figure 1 The pre-separation device for D2O and H2O of Example 1.

[0017] Figure 2 The front view of the pre-separation device for D2O and H2O of Example 1.

[0018] Figure 1 The pre-separation device for D2O and H2O of Example 1. DETAILED DESCRIPTION

[0019] Example 1

[0020] A pre-separation device for D2O and H2O comprises a sample injection unit, a mixing unit and a recovery unit; the sample injection unit is connected to the mixing unit, the mixing unit is connected to the recovery unit, and the recovery unit is connected to the sample injection unit.

[0021] The sample injection unit includes a first solvent tank 1 and a second solvent tank 2, one side of the first solvent tank 1 is connected with the inlet end of the first pressure pipeline 3, the outlet end of the first pressure pipeline 3 is connected with the separation column tank 8, the inlet end of the second pressure pipeline 4 is connected with the second solvent tank 2, and the outlet end of the second pressure pipeline 4 is connected with the separation column tank 8;

[0022] The mixing unit includes the separation column tank 8, the separation column tank 8 contains the separation column module 7, and the two sides of the separation column tank 8 are respectively connected with the outlet ends of the first pressure pipeline 3 and the second pressure pipeline 4, and the two sides of the separation column tank 8 are respectively connected with the inlet ends of the third pressure pipeline 9 and the fourth pressure pipeline 10;

[0023] The recovery unit includes recovery tank chamber one 13 and recovery tank chamber two 14, and the two chambers are connected by a round hole passage 15, the recovery tank chamber two 14 is provided with a separation device polyamide reverse osmosis membrane 16, the two sides of the recovery tank chamber one 13 are respectively connected with the outlet ends of the third pressure pipeline 9 and the fourth pressure pipeline 10, the two sides of the recovery tank chamber two 14 are respectively connected with the inlet ends of the fifth pressure pipeline 17 and the sixth pressure pipeline 18, and the fifth pressure pipeline 17 and the sixth pressure pipeline 18 respectively deliver liquid back to the first solvent tank 1 and the second solvent tank 2.

[0024] The separation column tank 8 contains 11 separation column modules 7, and the separation column module 7 is a block-shaped filter element synthesized by pressing operation of graphite and ZIF8. 2-methyl imidazole reacts with zinc acetate to generate metal organic framework material ZIF8, and fluorescein sodium is directly embedded in the channel of the ZIF8 framework structure in the process of forming the ZIF8 framework structure; the molar ratio of 2-methyl imidazole, zinc acetate and fluorescein sodium is 1203:60.2:1, and specific patent: 2024105272044. The separation column module (7) is filled with ZIF8 to realize the amplification of the difference between the diffusion rate of methanol into D2O and H2O and the diffusion rate of D2O and H2O into methanol.

[0025] The first pressure pipeline 3, the second pressure pipeline 4, the third pressure pipeline 9, the fourth pressure pipeline 10, the fifth pressure pipeline 17 and the sixth pressure pipeline 18 are respectively provided with a first circulating water pump 5, a second circulating water pump 6, a third circulating water pump 11, a fourth circulating water pump 12, a fifth circulating water pump 19 and a sixth circulating water pump 20 to control the inflow and outflow and flow rate of liquid.

[0026] The first circulating water pump 5, the second circulating water pump 6, the third circulating water pump 11, the fourth circulating water pump 12, the fifth circulating water pump 19 and the sixth circulating water pump 20 are controlled and adjusted by a total control panel 22, and the total control panel 22 includes a flow rate key, a start key and a stop key, and the flow rate key can adjust the flow rate.

[0027] The front of the separation column tank 8 contains a visual window for observing the internal situation.

[0028] The separation column module 7 is provided with a separation column tank cover 21 to ensure the isolation of the interior from the outside.

[0029] Water is injected into the second solvent tank 2, and methanol is injected into the first solvent tank 1. The second pressure pipeline 4 at the inlet end of the second water circulating pump 6 is introduced into the water, and the first pressure pipeline 3 at the inlet end of the first water circulating pump 5 is introduced into the methanol. The total control panel 22 is adjusted, the appropriate flow rate is set, the start key is pressed to start water injection, and the liquid flow in the separation column tank 8 is observed through the visual window. When the water is fully injected into the separation column tank 8, the total control panel 22 switch of the second water circulating pump 6 is closed, the total control panel 22 is adjusted, the appropriate flow rate is set, the start key is pressed to start methanol injection, and the fourth water circulating pump 12 is started. The third pressure pipeline 9 discharges the mixed solution of methanol and water through the entry of methanol into the recovery tank chamber one 13. The above operation is repeated to inject water into the separation column tank 8, and the third water circulating pump 11 is started. The fourth pressure pipeline 10 discharges the mixed solution of methanol and water through the entry of water into the recovery tank chamber one 13. The mixed solution of water and methanol in the recovery tank chamber one 13 enters the recovery tank chamber two 14 through the round hole passage 15. In the recovery tank chamber two 14, the polyamide reverse osmosis membrane is used to make the water in the mixed solution pass through the polyamide reverse osmosis membrane from the sixth pressure pipeline 18 to return to the second solvent tank 2, and the methanol returns to the first solvent tank 1 from the fifth pressure pipeline 17. The above operation is repeated for several cycles, and finally all the related pipelines for methanol flow are closed, and the water is continuously circulated in the separation column tank 8.

[0030] When the water in the ZIF8 diffuses into the methanol, the D2O has a lower diffusion rate than the H2O, so that more D2O is retained in the separation column module 7 after multiple circulation cycles. Finally, all the pipelines are closed, and the separation column module 7 in the separation column tank 8 is taken out, so that a mixed solution with a higher content of D2O is obtained, the pre-separation of D2O and H2O is realized, and sufficient preparation is made for further obtaining high-purity D2O.

[0031] The utility model is not limited to the above-mentioned embodiments. Any technical solution formed by equivalent replacement falls within the protection scope required by the utility model.

Claims

1. A pre-separation device for D2O and H2O, characterized in that: The pre-separation device includes: a sample injection unit, a mixing unit, and a recovery unit; the sample injection unit is connected to the mixing unit, the mixing unit is connected to the recovery unit, and the recovery unit is connected to the sample injection unit. The injection unit includes a first solvent tank (1) and a second solvent tank (2). One side of the first solvent tank (1) is connected to the inlet end of the first pressure line (3), and the outlet end of the first pressure line (3) is connected to the separation column tank (8). The inlet end of the second pressure line (4) is connected to the second solvent tank (2), and the outlet end of the second pressure line (4) is connected to the separation column tank (8). The mixing unit includes a separation column groove (8), which contains a separation column module (7). The two sides of the separation column groove (8) are connected to the outlet ends of the first pressure pipeline (3) and the second pressure pipeline (4), respectively. The two sides of the separation column groove (8) are connected to the inlet ends of the third pressure pipeline (9) and the fourth pressure pipeline (10), respectively. The recovery unit includes a recovery tank chamber one (13) and a recovery tank chamber two (14), which are connected by a circular channel (15). A polyamide reverse osmosis membrane (16) is installed in the recovery tank chamber two (14). The two sides of the recovery tank chamber one (13) are connected to the outlet ends of the third pressure pipeline (9) and the fourth pressure pipeline (10), respectively. The two sides of the recovery tank chamber two (14) are connected to the inlet ends of the fifth pressure pipeline (17) and the sixth pressure pipeline (18), respectively. The fifth pressure pipeline (17) and the sixth pressure pipeline (18) respectively transport the liquid back to the first solvent tank (1) and the second solvent tank (2).

2. The pre-stage separation device for D2O and H2O according to claim 1, characterized in that: The separation column groove (8) contains 11 separation column modules (7), which are block filter elements synthesized from graphite and ZIF8 through a pressure operation.

3. The pre-stage separation device for D2O and H2O according to claim 1, characterized in that: The first pressure pipeline (3), the second pressure pipeline (4), the third pressure pipeline (9), the fourth pressure pipeline (10), the fifth pressure pipeline (17), and the sixth pressure pipeline (18) are respectively equipped with a first circulating water pump (5), a second circulating water pump (6), a third circulating water pump (11), a fourth circulating water pump (12), a fifth circulating water pump (19), and a sixth circulating water pump (20).

4. The pre-stage separation device for D2O and H2O according to claim 3, characterized in that: The first circulating water pump (5), the second circulating water pump (6), the third circulating water pump (11), the fourth circulating water pump (12), the fifth circulating water pump (19), and the sixth circulating water pump (20) are controlled and regulated by the main control panel (22), which includes a flow rate key, a start key, and a stop key.

5. The pre-stage separation device for D2O and H2O according to claim 1, characterized in that: The front of the separation column groove (8) has a viewing window for observing the internal situation.

6. The pre-stage separation device for D2O and H2O according to claim 1, characterized in that: The separation column module (7) is equipped with a separation column groove cover (21) to ensure the isolation between the inside and the outside.

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