Deuterated iodobenzene distillation decompression device

Abstract

The utility model discloses a deuterated iodobenzene distillation decompression device which comprises a vacuumizing device, a condensation collection pipeline and an evaporation component, the vacuumizing device, the condensation collecting pipeline and the evaporation assembly are connected in sequence; the evaporation assembly is used for heating the deuterated iodobenzene mixed with impurities, so that the deuterated iodobenzene is evaporated and enters the condensation collection pipeline; a finished product storage tank and a plurality of condensers are arranged on the condensation collection pipeline, the condensers are used for condensing the evaporated deuterated iodobenzene, and the finished product storage tank is used for storing the condensed deuterated iodobenzene; the vacuumizing device is used for extracting gas in the condensation collection pipeline and the evaporation assembly and reducing the gas pressure in the evaporation assembly, so that the boiling point of the deuterated iodobenzene is reduced; according to the deuterated iodobenzene distillation device, the boiling point of deuterated iodobenzene can be reduced, so that a mixed material is uniformly heated in the distillation process, the separation speed of the deuterated iodobenzene is accelerated, and the distillation efficiency is improved.

Description

Technical Field

[0001] The utility model belongs to the technical field of iodobenzene distillation, and specifically relates to a deuterated iodobenzene distillation pressure reducing device. Background Art

[0002] Distillation is a thermodynamic separation process. It uses the different boiling points of the components in a mixed liquid or liquid-solid system to evaporate the low-boiling-point component and then condense it to separate the entire component. It is a unit operation process that combines the two unit operations of evaporation and condensation, such as a distillation device disclosed in the patent with publication number CN206660635U. Compared with other separation methods, such as extraction, filtration and crystallization, distillation has the advantage that it does not require the use of other solvents other than the system components, thereby ensuring that no new impurities are introduced. Deuterated iodobenzene mixed with impurities is often separated by oil bath distillation.

[0003] However, there are two problems in the traditional oil bath distillation of deuterated iodobenzene. First, the boiling point of deuterated iodobenzene is 188°C. While the boiling point is high, the iodine in tritiated iodobenzene is unstable under long-term high temperature and is prone to dehalogenation and side reactions. Second, in traditional distillation equipment, the still is higher than the highest liquid level of the oil bath, so the tritiated benzene produced will flow back into the still after cooling above the still, greatly affecting the distillation efficiency. In addition, during the distillation process, it is necessary to wait for the upper cover to be fully preheated before a large amount of steam can enter the condenser. This process lasts for a long time, which also leads to low distillation efficiency. Utility Model Content

[0004] In view of this, the utility model provides a deuterated iodobenzene distillation pressure reducing device, which can reduce the boiling point of deuterated iodobenzene, make the mixed material heated evenly during the distillation process, accelerate the separation speed of deuterated iodobenzene, and improve the distillation efficiency.

[0005] The utility model is realized by the following technical solutions:

[0006] A deuterated iodobenzene distillation decompression device, comprising: a vacuum pumping device, a condensation collection pipeline and an evaporation component;

[0007] The vacuum device, condensation collection pipeline and evaporation component are connected in sequence;

[0008] The evaporation component is used to heat the deuterated iodobenzene mixed with impurities, so that the deuterated iodobenzene evaporates and enters the condensation collection pipeline;

[0009] The condensation collection pipeline is provided with a finished product storage tank and a plurality of condensers, the condenser is used to condense the evaporated deuterated iodobenzene, and the finished product storage tank is used to store the condensed deuterated iodobenzene;

[0010] The vacuum device is used to extract the gas in the condensation collection pipeline and the evaporation component, reduce the gas pressure in the evaporation component, and thus reduce the boiling point of deuterated iodobenzene.

[0011] Beneficial effects:

[0012] (1) The utility model provides a deuterated iodobenzene distillation pressure reducing device. By setting a vacuum pumping device, on the one hand, the air pressure in the evaporation component can be reduced, the boiling point of deuterated iodobenzene can be reduced, and the iodine in the tritiated iodobenzene can be prevented from being unstable under high temperature for a long time, resulting in dehalogenation reaction and side reaction. On the other hand, the vacuum pumping device can extract the gas in the condensation collection pipeline, so that the deuterated iodobenzene can be quickly condensed and flowed into the finished product storage tank, effectively improving the distillation efficiency.

[0013] (2) The top of the distillation kettle of the utility model is lower than the oil bath outlet. When performing oil bath distillation, high-temperature oil is filled into the heating tank through the oil bath inlet until the liquid level of the heating oil reaches the oil bath outlet. The distillation kettle below the oil bath outlet is heated evenly, and the deuterated iodobenzene inside the distillation kettle can be fully heated, thereby improving the distillation efficiency.

[0014] (3) The utility model provides an air intake assembly. Due to the provision of a vacuum pump, as the steam is discharged from the steam discharge pipe, the pressure inside the still can change and external air can be sucked into the still through the air intake assembly. Furthermore, since the air intake assembly extends into the inner bottom of the still, that is, below the liquid surface of the deuterated iodobenzene solution, the air entering during this process will cause the deuterated iodobenzene solution inside the still to tumble and accelerate evaporation, thereby improving the evaporation efficiency and preventing the generated tritiated benzene from cooling above the still and flowing back into the still.

[0015] (4) The air intake assembly of the utility model also includes a drying tank, and the setting of the drying tank makes the incoming air dry to prevent affecting the distillation effect.

[0016] (5) The air intake assembly of the utility model also includes a buffer tank. When the vacuum device is turned off, the pressure in the evaporation assembly increases, which may cause the liquid mixed with impurities in the distillation kettle to overflow from the air intake pipe. The buffer tank can buffer the overflowing liquid to ensure the safety of the device.

[0017] (6) The evaporation assembly of the utility model also includes a pressure detection device to monitor the pressure state inside the distillation kettle in real time.

[0018] (7) The first condenser of the utility model is arranged on the outer wall of the steam discharge pipe, and the second condenser is arranged on the outer wall of the connecting pipe. The first condenser and the second condenser both play the role of cooling the deuterated iodobenzene, thereby improving the condensation efficiency of the deuterated iodobenzene and further avoiding the iodine in the tritiated iodobenzene from being unstable under high temperature for a long time, resulting in dehalogenation reaction and side reactions.

[0019] In addition, the second condenser is arranged on the outer wall of the connecting pipe connected to the vacuum pumping device, which can further prevent the uncondensed deuterated iodobenzene vapor from entering the vacuum pumping device and prevent damage to the vacuum pumping device.

[0020] (8) The utility model is also provided with a third condenser, which is arranged around the finished product storage tank to further prevent the iodine in the tritiated iodobenzene from becoming unstable under high temperature for a long time, causing dehalogenation reaction and side reactions.

[0021] (9) The utility model is also provided with a front fraction storage tank, which can first collect deuterated benzene in the impurities, thereby recovering the deuterated benzene and saving production costs. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] Figure 1 It is a schematic diagram of the overall structure of the deuterated iodobenzene pressure reducing device of the utility model;

[0023] Figure 2 for Figure 1 A schematic diagram of a local A enlargement;

[0024] Figure 3 for Figure 1 A partial enlarged schematic diagram of B;

[0025] Among them, 1-heating tank, 101-oil bath inlet, 102-oil bath outlet, 2-distillation kettle, 201-waste discharge outlet, 202-inlet pipe, 3-steam discharge pipe, 4-vacuum monitoring tube, 5-feed pipe, 6-cleaning pipe, 7-first condenser, 8-second condenser, 9-vacuum pumping device, 901-connecting pipe, 10-buffer tank, 11-drying tank, 12-inlet control valve, 13-third condenser, 14-finished product storage tank, 15-fore fraction storage tank. DETAILED DESCRIPTION

[0026] The present invention will be described in detail below with reference to the accompanying drawings and in combination with embodiments. It should be noted that the embodiments and features in the embodiments of the present application can be combined with each other without conflict.

[0027] Embodiment 1:

[0028] This embodiment provides a deuterated iodobenzene distillation pressure reducing device, see attached Figure 1 , including: a vacuum device 9, a condensation collection pipeline and an evaporation component;

[0029] The vacuum device 9, the condensation collection pipeline and the evaporation component are connected in sequence; the evaporation component is used to heat the deuterated iodobenzene mixed with impurities, so that the deuterated iodobenzene evaporates and enters the condensation collection pipeline; the condensation collection pipeline is provided with a finished product storage tank 14 and a plurality of condensers, the condenser is used to condense the evaporated deuterated iodobenzene, and the finished product storage tank 14 is used to store the condensed deuterated iodobenzene;

[0030] The vacuum device 9 is used to extract the gas in the condensation collection pipeline and the evaporation component, reduce the gas pressure in the evaporation component, and thus reduce the boiling point of deuterated iodobenzene.

[0031] By providing the vacuum pumping device 9, the embodiment can reduce the air pressure in the evaporation component, reduce the boiling point of deuterated iodobenzene, and prevent the iodine in the deuterated iodobenzene from being unstable under high temperature for a long time, causing dehalogenation reaction and side reaction. On the other hand, the vacuum pumping device can extract the gas in the condensation collection pipeline, so that the deuterated iodobenzene can be quickly condensed and flowed into the finished product storage tank 14, effectively improving the distillation efficiency.

[0032] The evaporation assembly includes a heating tank 1, a distillation kettle 2, a pressure detection device, a feed pipe 5 and a cleaning pipe 6;

[0033] An oil bath inlet and an oil bath outlet are provided on the heating tank 1, and the oil bath outlet is located above the oil bath inlet; the distillation kettle 2 is arranged inside the heating tank 1, and the top of the distillation kettle 2 is lower than the oil bath outlet; when performing oil bath distillation, high-temperature oil is filled into the heating tank 1 through the oil bath inlet 101 until the liquid level of the heating oil reaches the oil bath outlet 102. In this embodiment, the top of the distillation kettle 2 is lower than the oil bath outlet on the heating tank 1, so that the distillation kettle 2 is heated evenly, the deuterated iodobenzene inside the distillation kettle 2 can be fully heated, and the distillation efficiency is improved.

[0034] The feed pipe 5 is connected to the distillation kettle 2 and is used to introduce deuterated iodobenzene mixed with impurities into the distillation kettle 2. A valve is provided on the feed pipe 5. The distillation kettle 2 is also provided with a waste discharge port 201, which passes through the heating tank 1 and extends to the outside of the heating tank 1, and is used to discharge the waste after distillation. A valve is provided at the waste discharge port 201.

[0035] The pressure detection device is connected to the still 2 via the vacuum monitoring tube 4, and is used to monitor the pressure state inside the still 2;

[0036] The cleaning pipe 6 is connected to the distillation kettle 2. A valve is provided on the cleaning pipe 6 so that the valve can be opened to clean the distillation kettle 2 after the distillation is completed.

[0037] In a specific embodiment, the pressure detection device, the cleaning pipe 6 and the feeding pipe 5 are connected to the top of the distillation kettle 2, and the waste discharge port 201 is arranged at the bottom of the distillation kettle 2.

[0038] The condensation collection pipeline also includes a steam discharge pipe 3, and the aforementioned several condensers are respectively a first condenser 7, a second condenser 8 and a third condenser 13;

[0039] One end of the steam discharge pipe 3 is connected to the distillation kettle 2, and the other end is connected to the finished product storage tank 14. The finished product storage tank 14 is also connected to the vacuum device 9 through the connecting pipe 901; the first condenser 7 is arranged on the outer wall of the steam discharge pipe 3, the second condenser 8 is arranged on the outer wall of the connecting pipe 901, and the third condenser 13 is arranged to surround the finished product storage tank 14;

[0040] In the present embodiment, the first condenser 7, the second condenser 8 and the third condenser 13 all play the role of cooling the deuterated iodobenzene, improve the condensation efficiency of the deuterated iodobenzene, and further avoid the iodine in the deuterated iodobenzene to be unstable at high temperature for a long time, and dehalogenation reaction and side reaction occur. In addition, the second condenser 8 is arranged on the outer wall of the connecting pipe 901 connected to the vacuum pumping device 9, which can further prevent the uncondensed deuterated iodobenzene steam from entering the vacuum pumping device 9, and prevent the vacuum pumping device 9 from being damaged.

[0041] In a specific embodiment, the third condenser 13 and the second condenser 8 are both filled with a coolant at -40°C.

[0042] The condensation collection pipeline also includes a front fraction storage tank 15, which is connected to the steam exhaust pipe 3 through a valve body and is located between the finished product storage tank 14 and the distillation kettle 2; a valve body is also provided between the finished product storage tank 14 and the steam exhaust pipe 3.

[0043] The front fraction storage tank 15 is used to collect deuterated benzene in deuterated iodobenzene mixed with impurities. Deuterated benzene is a raw material for the reaction to generate deuterated iodobenzene, and its boiling point is 80°C, which is lower than that of deuterated iodobenzene. The impurities before distillation contain deuterated benzene. By setting the front fraction storage tank 15, closing the valve body between the finished product storage tank 14 and the steam exhaust pipe 3, and opening the valve body between the front fraction storage tank 15 and the steam exhaust pipe 3, the deuterated benzene can be collected first, thereby recovering the deuterated benzene and saving production costs.

[0044] Working principle:

[0045] When performing oil bath distillation, high temperature oil is filled into the heating tank 1 through the oil bath inlet 101 until the liquid level of the heating oil reaches the oil bath outlet 102. At this time, the entire distillation kettle 2 is located below the liquid level of the heating oil, so that the deuterated iodobenzene inside the distillation kettle 2 can be fully and evenly heated.

[0046] During the distillation process, the vacuum pumping device 9 is turned on to reduce the boiling point of tritiated iodobenzene on the one hand; on the other hand, the vacuum pumping device 9 evacuates the air inside the finished product storage tank 14 through the connecting pipe 901, and then utilizes the pressure ratio change to make the steam quickly flow into the finished product storage tank 14 through the steam discharge pipe 3, and cools the steam through the first condenser 7, the second condenser 8 and the third condenser 13, so that it is cooled to a solution and stored in the finished product storage tank 14, which effectively improves the distillation efficiency and avoids the iodine in tritiated iodobenzene from being unstable under high temperature for a long time, resulting in dehalogenation reaction and side reactions.

[0047] Embodiment 2:

[0048] This embodiment is based on Embodiment 1. A deuterated iodobenzene distillation pressure reducing device also includes an air intake assembly, one end of which is connected to the distillation kettle 2 and extends into the inner bottom of the distillation kettle 2. An air intake control valve 12 is provided at the other end of the air intake assembly. The air intake control valve 12 is a one-way valve, and air can enter the distillation kettle 2 from the outside along the air intake assembly.

[0049] In this embodiment, the air intake assembly is provided. Due to the provision of the vacuum device 9, as the steam is discharged from the steam discharge pipe 3, the internal pressure of the still 2 changes and the external air can be sucked into the still 2 through the air intake assembly; and because the air intake assembly extends into the inner bottom of the still 2, that is, below the liquid surface of the deuterated iodobenzene solution, the air entering during this process will cause the deuterated iodobenzene solution inside the still 2 to roll and accelerate evaporation, thereby improving the evaporation efficiency and preventing the generated tritiated benzene from cooling above the still 2 and flowing back into the still 2. The provision of the one-way valve allows the air to enter and the flow rate to be controlled, and avoids backflow.

[0050] The air intake assembly includes an air intake pipe 202, a drying tank 11 and a buffer tank 10;

[0051] One end of the air inlet pipe 202 extends into the inner bottom of the distillation kettle 2, and the air inlet control valve 12 is arranged at the other end of the air inlet pipe 202; the buffer tank 10 and the drying tank 11 are connected and arranged on the air inlet pipe 202, and are located between the distillation kettle 2 and the air inlet control valve 12; the drying tank 11 is adjacent to the air inlet control valve 12, and the buffer tank 10 is adjacent to the distillation kettle 2; a buffer mechanism is fixedly arranged inside the buffer tank 10.

[0052] When the vacuum device is turned off, the pressure in the evaporation component increases, which may cause the liquid mixed with impurities in the distillation kettle 2 to overflow from the air inlet pipe 202. The setting of the buffer tank 10 can buffer the overflowing liquid to ensure the safety of the device; the setting of the drying tank 11 makes the incoming air dry to prevent affecting the distillation effect.

[0053] In a specific embodiment, the steam exhaust pipe 3 , the feed pipe 5 and the air inlet pipe 202 are arranged on the same side of the top of the distillation kettle 2 .

[0054] In summary, the above are only preferred embodiments of the present invention and are not intended to limit the protection scope of the present invention. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principles of the present invention shall be included in the protection scope of the present invention.

Claims

1. A deuterated iodobenzene distillation decompression device, characterized in that, include: Vacuuming device, condensation collection pipeline and evaporation components; The vacuum device, condensation collection pipeline and evaporation component are connected in sequence; The evaporation component is used to heat the deuterated iodobenzene mixed with impurities, so that the deuterated iodobenzene evaporates and enters the condensation collection pipeline; The condensation collection pipeline is provided with a finished product storage tank and a plurality of condensers, the condenser is used to condense the evaporated deuterated iodobenzene, and the finished product storage tank is used to store the condensed deuterated iodobenzene; The vacuum device is used to extract the gas in the condensation collection pipeline and the evaporation component, reduce the gas pressure in the evaporation component, and thus reduce the boiling point of deuterated iodobenzene.

2. A deuterated iodobenzene distillation pressure reducing apparatus as claimed in claim 1, characterized in that: The evaporation assembly includes a heating tank and a distillation kettle; The heating tank is provided with an oil bath inlet and an oil bath outlet, and the oil bath outlet is located above the oil bath inlet; the distillation kettle is arranged inside the heating tank, and the top of the distillation kettle is lower than the oil bath outlet.

3. A deuterated iodobenzene distillation pressure reducing apparatus as claimed in claim 2, characterized in that: The pressure reducing device also includes an air intake assembly, one end of which is connected to the distillation kettle and extends into the inner bottom of the distillation kettle. The other end of the air intake assembly is provided with an air intake control valve, which is a one-way valve. Air can enter the distillation kettle from the outside along the air intake assembly.

4. A deuterated iodobenzene distillation pressure reducing apparatus as claimed in claim 3, characterized in that: The air intake assembly includes an air intake pipe and a drying tank; One end of the air inlet pipe extends into the inner bottom of the distillation kettle, and the air inlet control valve is arranged at the other end of the air inlet pipe; the drying tank is connected and arranged on the air inlet pipe and is located between the distillation kettle and the air inlet control valve.

5. A deuterated iodobenzene distillation pressure reducing apparatus as claimed in claim 4, characterized in that: The air intake assembly also includes a surge tank; The buffer tank is connected to the air inlet pipe and is located between the distillation kettle and the drying tank.

6. A deuterated iodobenzene distillation pressure reducing device as claimed in any one of claims 2 to 5, characterized in that: The evaporation component also includes a pressure detection device, which is connected to the distillation kettle through a vacuum monitoring tube and is used to monitor the pressure state inside the distillation kettle.

7. A deuterated iodobenzene distillation pressure reducing device as claimed in any one of claims 2 to 5, characterized in that: The evaporation component also includes a cleaning pipe; the cleaning pipe is connected to the distillation kettle, and a valve is arranged on the cleaning pipe.

8. A deuterated iodobenzene distillation pressure reducing device as claimed in any one of claims 2 to 5, characterized in that: The condensation collection pipeline also includes a steam discharge pipe; the plurality of condensers include a first condenser and a second condenser; One end of the steam discharge pipe is connected to the distillation kettle, and the other end is connected to the finished product storage tank. The finished product storage tank is also connected to the vacuum device through a connecting pipe; The first condenser is arranged on the outer wall of the steam discharge pipe, and the second condenser is arranged on the outer wall of the connecting pipe.

9. A deuterated iodobenzene distillation pressure reducing apparatus as claimed in claim 8, characterized in that: The plurality of condensers further includes a third condenser; the third condenser is arranged surrounding the finished product storage tank.

10. A deuterated iodobenzene distillation decompression device as claimed in claim 8, characterized in that: The condensate collection line also includes a fore fraction storage tank; The fore fraction storage tank is connected to the steam discharge pipe through the valve body and is located between the finished product storage tank and the distillation kettle; A valve body is arranged between the finished product storage tank and the steam discharge pipe.

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