Impurity removal reaction separation device for deuterated iodobenzene

Abstract

The utility model discloses an impurity removal reaction separation device for deuterated iodobenzene. The impurity removal reaction separation device comprises a reactor body and a separation assembly, the reactor body is provided with a concentrated hydrochloric acid inlet and a deuterated iodobenzene raw material inlet which are respectively used for introducing concentrated hydrochloric acid and deuterated iodobenzene into the reactor body; a plurality of iron balls are arranged in the reactor body, and the reactor body is heated through an oil bath; the deuterated iodobenzene raw materials comprise deuterated iodobenzene and deuterated nitrobenzene; the deuterated nitrobenzene can react with iron balls and concentrated hydrochloric acid in the reactor body in an oil bath heating environment to generate deuterated aniline, and the deuterated aniline generates water-soluble aniline hydrochloride under an acidic condition; the separation assembly is communicated with the reactor body and is used for separating water-soluble aniline hydrochloride and water-insoluble deuterated iodobenzene, so that impurity removal of deuterated iodobenzene is realized. According to the utility model, deuterated nitrobenzene in impurities can be removed, and high-purity deuterated iodobenzene can be obtained.

Description

Technical Field

[0001] The utility model belongs to the technical field of chemical engineering, and particularly relates to a separation device for the purification of deuterated iodobenzene from impurities. Background Art

[0002] Deuterium is an isotope of hydrogen, consisting of one proton and one neutron. Due to the mass effect, the carbon-deuterium bond has a shorter bond length and higher bond energy than the carbon-hydrogen bond. Therefore, deuterated compounds are widely used in the fields of medicine, environmental analysis and detection, and new material development.

[0003] When preparing deuterated iodobenzene, the product often contains impurities of deuterated nitrobenzene. The boiling point of deuterated iodobenzene is 188 °C, while the boiling point of deuterated nitrobenzene is 213 °C. The boiling point difference between the two is small under reduced pressure. Therefore, when purifying deuterated iodobenzene from the raw material of deuterated iodobenzene, it is difficult to obtain high-purity deuterated iodobenzene directly through simple distillation. Summary of the Utility Model

[0004] In view of this, the utility model provides a separation device for the purification of deuterated iodobenzene from impurities, which can remove deuterated nitrobenzene from the impurities and obtain high-purity deuterated iodobenzene.

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

[0006] A separation device for the purification of deuterated iodobenzene from impurities, comprising: a reactor body and a separation component; a concentrated hydrochloric acid inlet and a deuterated iodobenzene raw material inlet are arranged on the reactor body, which are respectively used for introducing concentrated hydrochloric acid and deuterated iodobenzene raw material into the reactor body;

[0007] A number of iron balls are arranged in the reactor body, and the reactor body is heated by an oil bath;

[0008] The deuterated iodobenzene raw material includes deuterated iodobenzene and deuterated nitrobenzene;

[0009] Deuterated nitrobenzene can react with iron balls and concentrated hydrochloric acid in the reactor body under the environment of oil bath heating to generate deuterated aniline, and deuterated aniline generates aniline hydrochloride soluble in water under acidic conditions;

[0010] The separation component is communicated with the reactor body, and the separation component is used for separating aniline hydrochloride soluble in water and deuterated iodobenzene insoluble in water, so as to realize the purification of deuterated iodobenzene.

[0011] Advantageous Effects:

[0012] (1) In the present utility model, the impurity deuterated nitrobenzene in the deuterated iodobenzene raw material reacts with Fe and hydrochloric acid to produce deuterated aniline, and deuterated aniline forms aniline hydrochloride under acidic conditions. This salt is easily soluble in water, so that aniline hydrochloride, Fe, FeCl2, FeCl3 and HCl in the deuterated iodobenzene can be removed by simple layering and water washing. Finally, the deuterated iodobenzene after removing impurities can obtain high-purity deuterated iodobenzene through simple rectification.

[0013] (2) A lining plate is arranged on the inner side wall of the reactor body of the present utility model to prevent the reactants in the reactor body from corroding the reactor body.

[0014] (3) Tetrafluoro balls are also arranged in the reactor body of the present utility model. The tetrafluoro balls are used to support the iron balls to prevent the iron balls from collapsing.

[0015] (4) The top end of the reactor body of the present utility model is connected with a buffer tank through a pipeline to prevent backflow.

[0016] (5) The buffer tank of the present utility model is connected with a second liquid storage tank through a pipeline. An alkali solution is provided in the second liquid storage tank. By providing the second liquid storage tank with the alkali solution, the volatilized acidic gas can be removed.

[0017] (6) The first liquid storage tank of the present utility model is used to collect the mixed solution containing FeCl2 and HCl. The mixed solution of FeCl2 and HCl recovered in the first liquid storage tank can be transported to the reactor body through a horizontal flow pump for continuous reaction, and discharged for treatment until the mixed solution is neutral. While saving the raw material cost, preliminary waste treatment is carried out.

[0018] (7) The present utility model further includes a support assembly, which can be used to support and level the reactor body. For example, when one side of the ground is uneven, the height of each support can be adjusted in real time so that the entire reaction device maintains a stable horizontal state. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] Figure 1 is a structural schematic diagram of a deuterated iodobenzene impurity removal reaction separation device of the present utility model;

[0020] Figure 2 is a connection structural schematic diagram of a flange group and a support mechanism of the present utility model;

[0021] Among them, 1 - reactor body, 2 - jacket, 3 - inlet oil pipe, 4 - outlet oil pipe, 5 - cleaning pipe, 6 - first peristaltic pump, 7 - second peristaltic pump, 8 - buffer tank, 9 - second liquid storage tank, 10 - water separator, 11 - first liquid storage tank, 12 - recovery tank, 13 - flange group, 1301 - upper flange plate, 1302 - lower flange plate, 14 - groove, 15 - support arm, 16 - threaded hole, 17 - chute, 18 - lifting nut, 19 - lifting rod, 20 - bracket, 21 - polytetrafluoroethylene lining plate, 22 - lifting screw rod, 23 - locking screw rod. Specific embodiments

[0022] Next, the technical solutions in the embodiments of the present invention will be clearly and completely described in conjunction with the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments.

[0023] Embodiment 1:

[0024] This embodiment provides a deuterated iodobenzene impurity removal reaction separation device. Refer to the attached Figure 1 , which includes a reactor body 1 and a separation component; a concentrated hydrochloric acid inlet and a deuterated iodobenzene raw material inlet are provided on the reactor body 1, which are respectively used for introducing concentrated hydrochloric acid and deuterated iodobenzene into the reactor body 1;

[0025] A number of iron balls are arranged in the reactor body 1, and the reactor body 1 is heated by an oil bath;

[0026] The deuterated iodobenzene raw material includes deuterated iodobenzene and deuterated nitrobenzene;

[0027] The deuterated nitrobenzene can react with iron balls and concentrated hydrochloric acid in the reactor body 1 under the environment of oil bath heating to generate deuterated aniline, and the deuterated aniline generates aniline hydrochloride soluble in water under acidic conditions;

[0028] The separation component is communicated with the reactor body 1, and the separation component is used to separate the aniline hydrochloride soluble in water and the deuterated iodobenzene insoluble in water, so as to realize the impurity removal of deuterated iodobenzene.

[0029] In this embodiment, the impurity deuterated nitrobenzene in the deuterated iodobenzene raw material reacts with Fe and hydrochloric acid to produce deuterated aniline, and the deuterated aniline generates aniline hydrochloride under acidic conditions. This salt is easily soluble in water. In this way, the aniline hydrochloride, Fe, FeCl2, FeCl3 and HCl in the deuterated iodobenzene can be removed by simple layering and water washing. Finally, the deuterated iodobenzene after removing impurities can obtain high-purity deuterated iodobenzene through simple rectification.

[0030] The reactor body 1 is a tubular structure with closed ends. A lining plate 21 is provided on the inner side wall of the reactor body 1 to prevent the reactants in the reactor body 1 from corroding the reactor body 1. In a specific embodiment, the material of the lining plate is polytetrafluoroethylene;

[0031] Tetrafluoro balls are also arranged in the reactor body 1. The tetrafluoro balls are used to support the iron balls to prevent the iron balls from collapsing. In a specific embodiment, the diameters of both the iron balls and the tetrafluoro balls are 2 mm;

[0032] A jacket 2 is arranged to surround the outer side wall of the reactor body 1. An annular space is formed between the jacket 2 and the outer side wall of the reactor body 1. An oil inlet pipe 3 and an oil outlet pipe 4 are arranged on the jacket 2. Both the oil inlet pipe 3 and the oil outlet pipe 4 are communicated with the annular space. The oil inlet pipe 3 is used to input heated heat-conducting oil into the annular space to achieve oil bath heating and heat preservation of the reactor body. The oil outlet pipe 4 is used to discharge the heat-conducting oil from the annular space. In a specific embodiment, the heat-conducting oil is input into the annular gap through the oil inlet pipe 3 and flows back through the oil outlet pipe 4. The temperature range of the heated heat-conducting oil is 70°C - 80°C, and the temperature of the heat-conducting oil can be adjusted by a high and low temperature integrated machine.

[0033] The deuterated iodobenzene raw material inlet of the reactor body 1 is connected with a first peristaltic pump 6 through a pipeline. The first peristaltic pump 6 is used to transport the deuterated iodobenzene raw material into the reactor body 1;

[0034] The concentrated hydrochloric acid inlet of the reactor body 1 is connected with a second peristaltic pump 7 through a pipeline. The second peristaltic pump 7 is used to transport concentrated hydrochloric acid into the reactor body 1;

[0035] A cleaning pipe 5 is connected to the top end of the reactor body 1. The top end of the reactor body 1 is also connected with a buffer tank 8 through a pipeline. By setting the buffer tank 8, backflow can be prevented;

[0036] The buffer tank 8 is connected with a second liquid storage tank 9 through a pipeline. An alkali solution is provided in the second liquid storage tank 9. By setting the second liquid storage tank 9 with an alkali solution, the volatilized acidic gas can be removed;

[0037] The separation assembly includes a water separator 10, a recovery tank 12 and a first liquid storage tank 11;

[0038] The water separator 10 is communicated with the inner bottom of the reactor body 1 through a pipeline. The water separator 10 is used to separate the reacted liquid into deuterated iodobenzene insoluble in water and aniline hydrochloride, FeCl2 and HCl soluble in water. The recovery tank 12 and the first liquid storage tank 11 are respectively communicated with the water separator 10. The recovery tank 12 is used to collect the deuterated iodobenzene after separation and impurity removal. The first liquid storage tank 11 is used to collect the mixed solution containing aniline hydrochloride, FeCl2 and HCl. The mixed solution of FeCl2 and hydrochloric acid recovered in the first liquid storage tank 11 can be transported into the reactor body 1 through a peristaltic pump for continuous reaction and discharged for treatment until the mixed solution is neutral.

[0039] In a specific embodiment, valves are installed in each pipeline and the cleaning pipe 5.

[0040] Working principle:

[0041] The deuterated iodobenzene raw material and concentrated hydrochloric acid are respectively input into the reactor body 1 through the first peristaltic pump 6 and the second peristaltic pump 7. When the deuterated iodobenzene and hydrochloric acid pass through the iron balls, a chemical reaction will occur, and the impurity deuterated nitrobenzene can be reduced to aniline hydrochloride. The mixture in the reactor body 1 can be sucked through the water separator 10, and after washing with water, the deuterated iodobenzene is separated. Finally, the deuterated iodobenzene after removing impurities can be obtained with high purity through simple distillation. The mixed solution of FeCl2 and hydrochloric acid generated therein can continue to be transported to the reactor body 1 through the peristaltic pump for reaction, and until the mixed solution is neutral, the mixed solution can be treated as hazardous waste.

[0042] Example 2:

[0043] Based on Example 1, a deuterated iodobenzene impurity removal reaction separation device of this embodiment further includes a support assembly for supporting and leveling the reactor body 1;

[0044] A flange group 13 is provided at the bottom of the reactor body 1; the flange group 13 includes an upper flange plate 1301 and a lower flange plate 1302; two or more grooves 14 are opened at the lower end of the lower flange plate 1302; a support assembly corresponding to the number of grooves is locked in the grooves 14 one by one;

[0045] See the appendix Figure 2 The support assembly includes a support arm 15, a lifting nut 18, a lifting rod 19, a bracket 20, a lifting screw rod 22 and a locking screw rod 23;

[0046] The top of the support arm 15 cooperates with the corresponding groove 14. A threaded hole A is provided on the side wall of the groove 14, and a threaded hole 16 is provided on the side wall of the support arm 15. The locking screw rod 23 sequentially passes through the threaded hole A of the groove 14 and the threaded hole 16 of the support arm 15 to lock the support arm 15 on the lower flange plate 1302;

[0047] An opening is provided at the bottom of the support arm 15. The lifting screw rod 22 is arranged in the vertical direction, and the top of the lifting screw rod 22 is rotatably connected to the inner bottom of the opening of the support arm 15. The lifting nut 18 is arranged on the lifting screw rod 22, and the bottom of the lifting nut 18 is fixedly connected to the support 20 through more than one lifting rod 19. By rotating each lifting screw rod 22, the lifting nuts 18 can be moved, and then the support 20 can be pushed to move up and down through the lifting rod 19. In this way, the height of each support 20 can be adjusted according to the actual terrain. For example, when one side of the ground is uneven, the height of each support 20 can be adjusted in real time to keep the whole reaction device in a stable horizontal state.

[0048] In summary, the above are only the 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 principle of the present invention shall be included in the protection scope of the present invention.

Claims

1. A separation device for the purification reaction of deuterated iodobenzene, characterized in that, Comprising: A reactor body and a separation component; a concentrated hydrochloric acid inlet and a deuterated iodobenzene raw material inlet are provided on the reactor body, which are respectively used for introducing concentrated hydrochloric acid and deuterated iodobenzene into the reactor body; A number of iron balls are arranged in the reactor body, and the reactor body is heated by an oil bath; The deuterated iodobenzene raw material includes deuterated iodobenzene and deuterated nitrobenzene; The deuterated nitrobenzene can react with the iron balls and concentrated hydrochloric acid in the reactor body under the environment of oil bath heating to generate deuterated aniline, and the deuterated aniline generates aniline hydrochloride soluble in water under acidic conditions; The separation component is communicated with the reactor body, and the separation component is used for separating the aniline hydrochloride soluble in water and the deuterated iodobenzene insoluble in water, so as to realize the impurity removal of deuterated iodobenzene.

2. The deuterated iodobenzene impurity removal reaction separation device according to claim 1, wherein The reactor body is a tubular structure with both ends closed, and a lining plate is arranged on the inner side wall of the reactor body.

3. The deuterated iodobenzene impurity removal reaction separation device according to claim 1, characterized in that, Tetrafluoro balls are arranged in the reactor body.

4. The deuterated iodobenzene impurity removal reaction separation device according to claim 1, wherein A jacket is arranged around the outer side wall of the reactor body, and an annular space is formed between the jacket and the outer side wall of the reactor body. An oil inlet pipe and an oil outlet pipe are arranged on the jacket; both the oil inlet pipe and the oil outlet pipe are communicated with the annular space; the oil inlet pipe is used for inputting heated heat-conducting oil into the annular space; the oil outlet pipe is used for discharging the heat-conducting oil from the annular space.

5. The deuterated iodobenzene impurity removal reaction separation device according to claim 1, wherein, A cleaning pipe is connected to the top end of the reactor body.

6. The deuterated iodobenzene impurity removal reaction separation device according to claim 1, characterized in that, The top end of the reactor body is connected with a buffer tank through a pipeline.

7. The separation device for the deuterated iodobenzene impurity removal reaction according to claim 6, characterized in that, The buffer tank is connected with a second liquid storage tank through a pipeline, and an alkali solution is provided in the second liquid storage tank.

8. The deuterated iodobenzene impurity removal reaction separation device according to claim 1, wherein The separation component includes a water separator, a recovery tank and a first liquid storage tank; The water separator is communicated with the inner bottom of the reactor body through a pipeline, and the water separator is used for separating the reacted liquid into deuterated iodobenzene insoluble in water and aniline hydrochloride, FeCl2 and HCl soluble in water; The recovery tank and the first liquid storage tank are respectively communicated with the water separator. The recovery tank is used for collecting the deuterated iodobenzene after separation and impurity removal; the first liquid storage tank is used for collecting the mixed solution containing aniline hydrochloride, FeCl2 and HCl.

9. The deuterated iodobenzene impurity removal reaction separation device according to any one of claims 1-8, characterized in that, The impurity removal reaction separation device further includes a support component for supporting and leveling the reactor body; A flange group is arranged at the bottom of the reactor body; the flange group includes an upper flange plate and a lower flange plate; wherein two or more grooves are opened at the lower end of the lower flange plate; a support component corresponding to the number of the grooves is locked and arranged in the grooves one by one; The support component includes a support arm, a lifting nut, a lifting rod, a bracket and a lifting screw; The top of the support arm is locked and connected with the groove; An opening is arranged at the bottom of the support arm, the lifting screw is arranged in the vertical direction, the top of the lifting screw is rotationally connected to the inner bottom of the opening of the support arm; the lifting nut is arranged on the lifting screw, and the bottom of the lifting nut is fixedly connected with the bracket through one or more lifting rods.

10. The deuterated iodobenzene impurity removal reaction separation device according to claim 9, characterized in that, The support component further includes a locking screw; The top of the support arm cooperates with the corresponding groove. A threaded hole A is arranged on the side wall of the groove, and a threaded hole is arranged on the side wall of the support arm. The locking screw sequentially passes through the threaded hole A of the groove and the threaded hole of the support arm to lock the support arm on the lower flange plate.

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