CN112778072A - Catalytic production process of deuterated benzene - Google Patents

Catalytic production process of deuterated benzene Download PDF

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Publication number
CN112778072A
CN112778072A CN202011640442.4A CN202011640442A CN112778072A CN 112778072 A CN112778072 A CN 112778072A CN 202011640442 A CN202011640442 A CN 202011640442A CN 112778072 A CN112778072 A CN 112778072A
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connecting piece
operating shaft
cavity
connector
deuterated benzene
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CN202011640442.4A
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Chinese (zh)
Inventor
张文驰
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Xuzhou Yaxing Medical Technology Co ltd
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Xuzhou Yaxing Medical Technology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C5/00Preparation of hydrocarbons from hydrocarbons containing the same number of carbon atoms
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16KVALVES; TAPS; COCKS; ACTUATING-FLOATS; DEVICES FOR VENTING OR AERATING
    • F16K1/00Lift valves or globe valves, i.e. cut-off apparatus with closure members having at least a component of their opening and closing motion perpendicular to the closing faces
    • F16K1/16Lift valves or globe valves, i.e. cut-off apparatus with closure members having at least a component of their opening and closing motion perpendicular to the closing faces with pivoted closure-members
    • F16K1/18Lift valves or globe valves, i.e. cut-off apparatus with closure members having at least a component of their opening and closing motion perpendicular to the closing faces with pivoted closure-members with pivoted discs or flaps
    • F16K1/22Lift valves or globe valves, i.e. cut-off apparatus with closure members having at least a component of their opening and closing motion perpendicular to the closing faces with pivoted closure-members with pivoted discs or flaps with axis of rotation crossing the valve member, e.g. butterfly valves
    • F16K1/221Lift valves or globe valves, i.e. cut-off apparatus with closure members having at least a component of their opening and closing motion perpendicular to the closing faces with pivoted closure-members with pivoted discs or flaps with axis of rotation crossing the valve member, e.g. butterfly valves specially adapted operating means therefor
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16KVALVES; TAPS; COCKS; ACTUATING-FLOATS; DEVICES FOR VENTING OR AERATING
    • F16K1/00Lift valves or globe valves, i.e. cut-off apparatus with closure members having at least a component of their opening and closing motion perpendicular to the closing faces
    • F16K1/16Lift valves or globe valves, i.e. cut-off apparatus with closure members having at least a component of their opening and closing motion perpendicular to the closing faces with pivoted closure-members
    • F16K1/18Lift valves or globe valves, i.e. cut-off apparatus with closure members having at least a component of their opening and closing motion perpendicular to the closing faces with pivoted closure-members with pivoted discs or flaps
    • F16K1/22Lift valves or globe valves, i.e. cut-off apparatus with closure members having at least a component of their opening and closing motion perpendicular to the closing faces with pivoted closure-members with pivoted discs or flaps with axis of rotation crossing the valve member, e.g. butterfly valves
    • F16K1/224Details of bearings for the axis of rotation
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16KVALVES; TAPS; COCKS; ACTUATING-FLOATS; DEVICES FOR VENTING OR AERATING
    • F16K1/00Lift valves or globe valves, i.e. cut-off apparatus with closure members having at least a component of their opening and closing motion perpendicular to the closing faces
    • F16K1/32Details
    • F16K1/50Preventing rotation of valve members
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16KVALVES; TAPS; COCKS; ACTUATING-FLOATS; DEVICES FOR VENTING OR AERATING
    • F16K35/00Means to prevent accidental or unauthorised actuation
    • F16K35/02Means to prevent accidental or unauthorised actuation to be locked or disconnected by means of a pushing or pulling action
    • F16K35/022Means to prevent accidental or unauthorised actuation to be locked or disconnected by means of a pushing or pulling action the locking mechanism being actuated by a separate actuating element
    • F16K35/025Means to prevent accidental or unauthorised actuation to be locked or disconnected by means of a pushing or pulling action the locking mechanism being actuated by a separate actuating element said actuating element being operated manually (e.g. a push-button located in the valve actuator)
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16KVALVES; TAPS; COCKS; ACTUATING-FLOATS; DEVICES FOR VENTING OR AERATING
    • F16K35/00Means to prevent accidental or unauthorised actuation
    • F16K35/16Means to prevent accidental or unauthorised actuation with locking member actuated by magnet
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07BGENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
    • C07B2200/00Indexing scheme relating to specific properties of organic compounds
    • C07B2200/05Isotopically modified compounds, e.g. labelled

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  • Engineering & Computer Science (AREA)
  • General Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention discloses a catalytic production process of deuterated benzene, which comprises the steps of mixing benzene and heavy water according to the volume ratio of 1:2, and adding platinum carbon; hermetically heating and stirring at 100-130 ℃, reacting for 8-15 hours, separating, and distilling to obtain a target product, namely deuterated benzene; wherein the platinum carbon is added at a rate of 15 to 35% by weight per minute. The invention designs a manual powder valve for the test, controls the adding speed of the platinum carbon through the manual powder valve, and studies the influence of the adding speed of the platinum carbon to the mixed solution of benzene and heavy water on the deuteration rate of the final target product; through experimental research, the deuteration rate of the target product is related to the adding speed of the platinum carbon, and when the adding speed of the platinum carbon is added at a speed of 15-35% of the total weight/minute, the deuteration rate of the target product is the highest and exceeds 90%.

Description

Catalytic production process of deuterated benzene
Technical Field
The invention relates to the technical field of material synthesis, in particular to a catalytic production process of deuterated benzene.
Background
The deuterated benzene is a deuterated derivative of benzene, is an important deuterated solvent and a tracer for marking aromatic compounds, has the advantages of unique isotope effect, solubility, super-strong stability, higher deuteration rate, no radioactivity and the like, and is widely applied to the synthesis of deuterated compounds and mass spectrometry detection technology.
Organic compounds with partial deuterium substitution or total deuteration show unique signals in Mass Spectrometry (MS), nuclear magnetic resonance (H-NMR) and electron spin resonance spectroscopy (ESR), and are widely used as labeled compounds in various fields such as life sciences, environmental sciences, pesticide residue detection and pollutant tracking, and material sciences, and are used for analyzing reaction mechanisms and substance metabolic pathways. As a method for producing a deuterated compound, a deuteration method in which a non-deuterated compound is treated with deuterated solvent deuterated benzene in the presence of a lewis acid H/D exchange catalyst such as aluminum trichloride, ethylaluminum chloride or acid trifluoromethanesulfonic acid is preferred, and deuterated benzene is an important deuterium source. The industrial synthesis of deuterated benzenes can be mainly divided into 3 types: a hydrogen/deuterium exchange method, a method of introducing a halogen, a method of hydrogenating again, and a method of polymerizing.
However, in the prior art, no study on the influence of the addition rate of the catalyst on the yield of the final target product has been reported, and therefore, it is necessary to study the influence of the addition rate of the catalyst on the yield of the final target product.
Disclosure of Invention
This section is for the purpose of summarizing some aspects of embodiments of the invention and to briefly introduce some preferred embodiments. In this section, as well as in the abstract and the title of the invention of this application, simplifications or omissions may be made to avoid obscuring the purpose of the section, the abstract and the title, and such simplifications or omissions are not intended to limit the scope of the invention.
The invention is provided in view of the problem that radars with different sizes in the prior art need mounting seats with different sizes to be correspondingly mounted, so that the mounting is inconvenient.
Therefore, the invention aims to provide a catalytic production process of deuterated benzene, so as to research the influence of the adding speed of platinum carbon to a mixed solution of benzene and heavy water on the deuteration rate of a final target product.
In order to solve the technical problems, the invention provides the following technical scheme: a catalytic production process of deuterated benzene comprises,
mixing benzene and heavy water according to the volume ratio of 1:2, and adding platinum carbon;
hermetically heating and stirring at 100-130 ℃, reacting for 8-15 hours, separating, and distilling to obtain a target product, namely deuterated benzene;
wherein the platinum carbon is added at a rate of 15 to 35% by weight per minute.
As a preferable embodiment of the catalytic production process of deuterated benzene of the present invention, wherein: the platinum carbon is added into a mixed solution of benzene and heavy water through a manual powder valve, the manual powder valve comprises,
a valve body;
a pivot shaft within the valve body, the pivot shaft rotatable about a pivot axis;
a valve plate located within the valve body, the valve plate supported on the pivot shaft; and the number of the first and second groups,
the pivot driving device comprises a support seat positioned outside the valve body and an operating shaft connected with the pivot shaft, and the operating shaft is rotationally connected with the support seat;
and a limiting assembly is further arranged between the operating shaft and the support and is used for limiting the operating shaft to rotate.
As a preferable embodiment of the catalytic production process of deuterated benzene of the present invention, wherein: the limiting assembly comprises a first connecting piece positioned on the operating shaft and a second connecting piece positioned on the support;
wherein the first connector is structurally complementary to the second connector and is capable of being interconnected;
wherein the first link is movable on the operating shaft to disengage the second link.
As a preferable embodiment of the catalytic production process of deuterated benzene of the present invention, wherein: the first connecting piece is provided with a sliding pipe sleeved outside the operating shaft, and the first connecting piece moves on the operating shaft through the sliding pipe;
the support is provided with an accommodating cavity for accommodating the sliding pipe, and the second connecting piece is positioned in the accommodating cavity.
As a preferable embodiment of the catalytic production process of deuterated benzene of the present invention, wherein: the operating shaft is provided with a key block, and the sliding pipe moves along the key block in a guiding mode through a key groove.
As a preferable embodiment of the catalytic production process of deuterated benzene of the present invention, wherein: the first connecting piece protrudes out of the sliding pipe, the second connecting piece is in a groove shape which is complementary to the first connecting piece in structure, and the second connecting piece is arranged on the inner wall of the accommodating cavity;
the second connecting piece extends along the axial direction, an opening is formed in one side, facing the sliding tube, of the second connecting piece, and when the sliding tube moves, the first connecting piece penetrates through the opening to be separated from the second connecting piece.
As a preferable embodiment of the catalytic production process of deuterated benzene of the present invention, wherein: the first connecting pieces are uniformly distributed along the circumferential direction of the sliding pipe, and the second connecting pieces are correspondingly and uniformly distributed.
As a preferable embodiment of the catalytic production process of deuterated benzene of the present invention, wherein: a bearing is further arranged at the opening of the accommodating cavity, an outer ring of the bearing is fixedly connected with the support, and an inner ring of the bearing is provided with matching grooves for the first connecting piece to pass through respectively;
when the first connecting piece is separated from the second connecting piece, the first connecting piece is positioned in the matching groove.
As a preferable embodiment of the catalytic production process of deuterated benzene of the present invention, wherein: the accommodating cavity comprises a first cavity and a second cavity, the second connecting piece is positioned on the inner wall of the first cavity, the inner diameter of the second cavity is larger than the distance between the first connecting pieces on two sides of the sliding pipe, and the bearing is positioned at the opening of the second cavity;
the first connecting piece is straight-tooth-shaped, a spring bead is further arranged on the inner wall of the second cavity, and the spring bead is located between the two adjacent first connecting pieces.
As a preferable embodiment of the catalytic production process of deuterated benzene of the present invention, wherein: a tension spring connected with the sliding pipe is further arranged in the first cavity, and the first connecting piece and the second connecting piece are connected in an embedded mode through the pretightening force of the tension spring;
the sliding pipe is connected with a handle, the operating shaft is connected with a rotating handle, and the handle is provided with a magnetic part which can be connected with the rotating handle.
The invention has the beneficial effects that: the invention designs a manual powder valve for the test, controls the adding speed of the platinum carbon through the manual powder valve, and studies the influence of the adding speed of the platinum carbon to the mixed solution of benzene and heavy water on the deuteration rate of the final target product; through experimental research, the deuteration rate of the target product is related to the adding speed of the platinum carbon, and when the adding speed of the platinum carbon is added at a speed of 15-35% of the total weight/minute, the deuteration rate of the target product is the highest and exceeds 90%.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without inventive exercise. Wherein:
FIG. 1 is a schematic view of a connection structure of a manual powder valve and a tank body according to the present invention;
FIG. 2 is a schematic view of the overall structure of the manual powder valve of the present invention;
FIG. 3 is a schematic half-sectional view of the pivot drive of the present invention;
FIG. 4 is a schematic view of the construction of the operating shaft of the present invention;
FIG. 5 is a schematic structural view of a slide tube according to the present invention;
FIG. 6 is a schematic view of the structure of the key slot of the slide pipe of the present invention;
FIG. 7 is a schematic half-sectional view of a mount of the present invention;
FIG. 8 is a schematic diagram of the slide tube of the present invention after moving.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in detail below.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways than those specifically described and will be readily apparent to those of ordinary skill in the art without departing from the spirit of the present invention, and therefore the present invention is not limited to the specific embodiments disclosed below.
Furthermore, reference herein to "one embodiment" or "an embodiment" means that a particular feature, structure, or characteristic described in connection with the embodiment is included in at least one implementation of the invention. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments.
Furthermore, the present invention is described in detail with reference to the drawings, and in the detailed description of the embodiments of the present invention, the cross-sectional view illustrating the structure of the device is not enlarged partially according to the general scale for convenience of illustration, and the drawings are only exemplary and should not be construed as limiting the scope of the present invention. In addition, the three-dimensional dimensions of length, width and depth should be included in the actual fabrication.
Example 1
(1) Mixing 500mL of benzene and 1000mL of heavy water, adding 30g of platinum carbon, heating and stirring in a closed environment at 110 ℃, reacting for 12 hours, separating, and distilling to obtain a target product of deuterated benzene;
wherein the platinum carbon was added at the rate as in table 1, and the deuteration ratio results of the final target product are shown in table 1.
TABLE 1
Figure BDA0002879923710000041
Figure BDA0002879923710000051
As can be seen from the data in table 1, the deuteration ratio of the target product is related to the addition rate of platinum carbon, and when the addition rate of platinum carbon is 15 to 35% of the total weight/min, the deuteration ratio of the target product is the highest, and both are more than 90%; the addition speed of the platinum carbon is too high, if the sample 9 is adopted, the platinum carbon is completely added at one time, and the deuteration rate of the target product is only 74 percent; if the rate of addition of platinum carbon is too slow, as in sample 1, the rate of addition at 1.5g/min lowers the deuteration ratio of the target product from the optimum value.
Example 2
Referring to fig. 1 to 3, for a first embodiment of the present invention, there is provided a manual powder valve through which platinum carbon is added to a mixed solution of benzene and heavy water, the manual powder valve being specially designed for a test, by which an addition rate of platinum carbon is controlled to study an influence of the addition rate of platinum carbon to the mixed solution of benzene and heavy water on a final target product deuteration rate.
Specifically, as shown in fig. 1, the manual powder valve is disposed at the discharge port 501 of the tank 500, and the platinum carbon is pre-stored in the tank 500, and the discharge speed of the platinum carbon is controlled by the operation of the manual powder valve.
In this embodiment, the structure of the manual powder valve is similar to a butterfly valve in the prior art, and the manual powder valve includes a valve body 100, a pivot shaft 200, a valve plate 300, and a pivot driving device 400; the pivot shaft 200 is located within the valve body 100, the pivot shaft 200 being rotatable about a pivot axis; the valve plate 300 is positioned in the valve body 100, and the valve plate 300 is supported on the pivot shaft 200; through the pivot shaft 200 rotating around the pivot axis, the rotation of the valve plate 300 can be realized, so that the opening or closing of the valve is realized;
wherein, the pivot driving device 400 comprises a support 401 positioned outside the valve body 100 and an operating shaft 402 connected with the pivot shaft 200, the operating shaft 402 is rotatably connected with the support 401, and the rotation of the pivot shaft 200 around the pivot axis is realized by rotating the operating shaft 402 outside the valve body 100;
in this embodiment, a limiting component 403 is further disposed between the operating shaft 402 and the support 401, the limiting component 403 is used for limiting the rotation of the operating shaft 402, and when the limiting component 403 limits the rotation of the operating shaft 402, the pivot shaft 200, that is, the valve plate 300, can be maintained at a certain rotational position; if the valve plate 300 is located at the valve closing position, the restricting member 403 restricts the operating shaft 402, so that the valve closing state can be maintained at all times, and the valve can be opened only when the restricting member 403 is removed, thereby preventing a certain degree of erroneous operation.
It should be noted that the limiting assembly 403 includes a first connecting member 403a located on the operating shaft 402 and a second connecting member 403b located on the support 401; the first connecting member 403a and the second connecting member 403b are complementary and can be connected to each other, the first connecting member 403a and the second connecting member 403b are both located at the circumferential position of the operating shaft 402, and when the first connecting member 403a and the second connecting member 403b are connected to each other, the operating shaft 402 is prevented from rotating in the circumferential direction;
it should be noted that the first connecting member 403a can move on the operating shaft 402 to separate from the second connecting member 403b, the direction of the first connecting member 403a moving on the operating shaft 402 is axial movement, and after the axial movement reaches a certain position, the first connecting member 403a can separate from the second connecting member 403b at a circumferential position, and at this time, the operating shaft 402 can freely rotate without limitation.
Example 3
Referring to fig. 2 to 6, this embodiment is different from the first embodiment in that: in order to facilitate the axial movement of the first connecting piece 403a on the operating shaft 402, a sliding pipe 404 sleeved outside the operating shaft 402 is arranged on the first connecting piece 403a, the first connecting piece 403a moves on the operating shaft 402 through the sliding pipe 404, and the first connecting piece 403a can be moved axially conveniently by operating the sliding pipe 404;
the holder 401 is provided with an accommodating cavity N1 for accommodating the sliding tube 404 and a through hole N4 for the operating shaft 402 to pass through, the inner diameter of the accommodating cavity N1 is larger than the inner diameter of the through hole N4, one end of the through hole N4 is further provided with a rotating bearing connected with the operating shaft 402, the operating shaft 402 passes through the through hole N4 and can rotate in the through hole N4 under the support of the rotating bearing, the second connecting piece 403b is located in the accommodating cavity N1, when the sliding tube 404 moves axially on the operating shaft 402, the sliding tube 404 can enter the accommodating cavity N1 and connect the first connecting piece 403a with the second connecting piece 403b, and when the sliding tube 404 moves towards the outside of the accommodating cavity N1, the first connecting piece 403a can be separated from the second connecting piece 403 b.
Since the first connecting member 403a is axially movable on the operating shaft 402, a key 402a is fixed on the operating shaft 402, the key 402a extends in the axial direction of the operating shaft 402, a key groove N2 extending in the axial direction is provided in the inner cavity of the slide pipe 404, and the slide pipe 404 is guided to move along the key 402a through the key groove N2.
Specifically, the first connecting piece 403a protrudes from the sliding tube 404, the second connecting piece 403b is in a groove shape with a structure complementary to that of the first connecting piece 403a, and the second connecting piece 403b is arranged on the inner wall of the accommodating cavity N1; the second connecting member 403b extends in the axial direction, and the second connecting member 403b forms an opening toward a side of the slide pipe 404, and the first connecting member 403a passes through the opening to be disengaged from the second connecting member 403b when the slide pipe 404 moves.
Example 4
Referring to fig. 2 to 7, this embodiment is different from the above embodiment in that: since the sliding tube 404 is guided to move along the key block 402a on the operating shaft 402, when the operating shaft 402 rotates, the sliding tube 404 and the operating shaft 402 rotate synchronously, which may cause a problem that the first connecting member 403a and the second connecting member 403b cannot be ensured to correspond to each other in the axial position during the rotation process, and therefore, the first connecting member 403a and the second connecting member 403b cannot be connected to each other by moving the sliding tube 404 in the axial direction, and the rotation of the operating shaft 402 cannot be limited; therefore, the first connecting pieces 403a of the present embodiment are uniformly distributed along the circumferential direction of the sliding tube 404, the second connecting pieces 403b are correspondingly uniformly distributed, and the plurality of first connecting pieces 403a are arranged, so that the fault tolerance rate can be improved, and the larger the number of the first connecting pieces 403a is, the higher the fault tolerance rate is, and the smaller the rotation angle is, the first connecting pieces 403a and the second connecting pieces 403b can be ensured to be corresponding to each other in the axial position; if the operation shaft 402 is limited to rotate at the valve opening position, that is, the opening size of the valve is fixed, the valve is opened due to the action of the rotation operation shaft 402, when the valve is rotated to the valve opening position, the first connecting piece 403a and the second connecting piece 403b may not correspond to each other at the axial positions, at this time, the first connecting piece 403a and the second connecting piece 403b can be corresponding to each other only by adjusting a small angle, the more the number of the first connecting pieces 403a is designed, the smaller the angle of adjustment at this time is, and even the influence on the opening size of the valve can be ignored.
It should be noted that a bearing 405 is further disposed at an opening of the accommodating cavity N1, an outer ring 405a of the bearing 405 is fixedly connected to the support 401, an inner ring 405b of the bearing 405 is provided with a matching groove N3 through which the first connecting member 403a respectively passes, the sliding tube 404 can extend into the matching groove N3 through the first connecting member 403a to realize connection with the bearing 405, when the sliding tube 404 and the operating shaft 402 rotate synchronously, the operating shaft 402 is supported by the bearing 405 through the sliding tube 404, and the rotation stability of the operating shaft 402 is ensured;
when the first connecting piece 403a is disengaged from the second connecting piece 403b, the first connecting piece 403a is located in the matching groove N3, that is, when the operating shaft 402 can freely rotate without limitation, the operating shaft 402 can be supported by the bearing 405 through the sliding tube 404; preferably, the first link 403a extends axially on the slide 404, and the first link 403a is always located in the mating groove N3, and the bearing 405 always supports the operating shaft 402 without worrying about the problem that the bearing 405 is disengaged from the slide 404 during the movement of the slide 404.
Example 5
Referring to fig. 2 to 7, this embodiment is different from the above embodiment in that: the accommodating cavity N1 comprises a first cavity N1a and a second cavity N1b, the inner diameter of the second cavity N1b is larger than that of the first cavity N1a, the first cavity N1a is communicated with a through hole N4, an opening is formed in one side, far away from the through hole N4, of the second cavity N1b on the support 401, a second connecting piece 403b is located on the inner wall of the first cavity N1a, the inner diameter of the second cavity N1b is larger than the distance between the first connecting pieces 403a on two sides of the sliding tube 404, free rotation of the operating shaft 402 can be guaranteed, and the bearing 405 is located at the opening of the second cavity N1 b;
furthermore, the first connecting members 403a are straight-toothed, a plurality of first connecting members 403a uniformly distributed along the circumferential direction of the sliding tube 404 form a structure similar to a gear, and correspondingly, the second connecting members 403b form straight grooves capable of accommodating the gear structure;
the inner wall of the second cavity N1b is further provided with a spring ball 406, the spring ball 406 is located between two adjacent first connecting pieces 403a, and in the synchronous rotation process of the sliding tube 404 and the operating shaft 402, the sliding tube 404 can rotate once at an angle of a single tooth under the action of the spring ball 406, and the angle of each rotation is ensured to be fixed, so that the first connecting piece 403a always corresponds to the axial position of the second connecting piece 403b in the rotation process.
It should be noted that during the movement of the sliding tube 404, the spring ball 406 can be always located between two adjacent first connecting members 403a, so as to ensure that the spring ball 406 is located between two adjacent teeth when the first connecting members 403a are disengaged from the second connecting members 403 b.
Specifically, the spring ball 406 can adopt a prior art means, a mounting hole N5 along the radial direction of the sliding tube 404 is formed on the side wall of the support 401, the spring ball 406 comprises a ball 406a, an elastic member 406b and an adjusting block 406c, the ball 406a slides in the mounting hole N5 and is positioned between two adjacent teeth of the gear, and the elastic member 406b is connected between the ball 406a and the adjusting block 406 c; when the highest position of the first connecting piece 403a contacts the ball 406a, the ball 406a is pushed to compress the elastic piece 406b to move, and when the lowest position of the first connecting piece 403a is contacted, the elastic piece 406b pushes the ball 406a to reset, and so on, so as to ensure that the angle of each rotation is fixed;
the adjusting block 406c is in threaded connection with the mounting hole N5, the pretightening force of the elastic element 406b can be adjusted by rotating the adjusting block 406c, and the rotating force of the sliding tube 404 can be adjusted.
Example 6
Referring to fig. 2 to 8, this embodiment is different from the above embodiment in that: a tension spring 407 connected with the sliding pipe 404 is further arranged in the first cavity N1a, the pretightening force of the tension spring 407 enables the first connecting piece 403a and the second connecting piece 403b to be embedded and connected, namely, the operation shaft 402 is limited to rotate as an initial state, and when no external force is applied, the operation shaft 402 is limited to rotate;
the sliding tube 404 is further connected with a handle 404a, the operating shaft 402 is further connected with a rotating handle 402b, the handle 404a is provided with a magnetic part 404b capable of being connected with the rotating handle 402b, the handle 404a is pulled out of the accommodating cavity N1, the sliding tube 404 pulls the tension spring 407 to move until the handle 404a is fixedly connected with the rotating handle 402b through the magnetic part 404b, at the moment, the first connecting part 403a is separated from the second connecting part 403b, meanwhile, the spring beads 406 are positioned between two adjacent teeth, the operating shaft 402 can freely rotate without limitation, and the rotating handle 402b is operated, so that the opening or closing action of the valve can be realized;
it should be noted that the acting force of the magnetic member 404b is greater than the elastic force of the tension spring 407, so that when the rotating handle 402b is operated, the sliding tube 404 cannot move; because the axial positions of the first connecting piece 403a and the second connecting piece 403b correspond to each other, after the handle 404a is separated from the rotating handle 402b, the sliding tube 404 can be quickly pulled under the action of the tension spring 407, so that the first connecting piece 403a quickly enters the second connecting piece 403b, i.e., the operating shaft 402 can be quickly fixed, and the valve can be quickly maintained in a certain state.
It is important to note that the construction and arrangement of the present application as shown in the various exemplary embodiments is illustrative only. Although only a few embodiments have been described in detail in this disclosure, those skilled in the art who review this disclosure will readily appreciate that many modifications are possible (e.g., variations in sizes, dimensions, structures, shapes and proportions of the various elements, values of parameters (e.g., temperatures, pressures, etc.), mounting arrangements, use of materials, colors, orientations, etc.) without materially departing from the novel teachings and advantages of the subject matter recited in this application. For example, elements shown as integrally formed may be constructed of multiple parts or elements, the position of elements may be reversed or otherwise varied, and the nature or number of discrete elements or positions may be altered or varied. Accordingly, all such modifications are intended to be included within the scope of this invention. The order or sequence of any process or method steps may be varied or re-sequenced according to alternative embodiments. In the claims, any means-plus-function clause is intended to cover the structures described herein as performing the recited function and not only structural equivalents but also equivalent structures. Other substitutions, modifications, changes and omissions may be made in the design, operating conditions and arrangement of the exemplary embodiments without departing from the scope of the present inventions. Therefore, the present invention is not limited to a particular embodiment, but extends to various modifications that nevertheless fall within the scope of the appended claims.
Moreover, in an effort to provide a concise description of the exemplary embodiments, all features of an actual implementation may not be described (i.e., those unrelated to the presently contemplated best mode of carrying out the invention, or those unrelated to enabling the invention).
It should be appreciated that in the development of any such actual implementation, as in any engineering or design project, numerous implementation-specific decisions may be made. Such a development effort might be complex and time consuming, but would nevertheless be a routine undertaking of design, fabrication, and manufacture for those of ordinary skill having the benefit of this disclosure, without undue experimentation.
It should be noted that the above-mentioned embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, which should be covered by the claims of the present invention.

Claims (10)

1. A catalytic production process of deuterated benzene is characterized by comprising the following steps: comprises the steps of (a) preparing a mixture of a plurality of raw materials,
mixing benzene and heavy water according to the volume ratio of 1:2, and adding platinum carbon;
hermetically heating and stirring at 100-130 ℃, reacting for 8-15 hours, separating, and distilling to obtain a target product, namely deuterated benzene;
wherein the platinum carbon is added at a rate of 15 to 35% by weight per minute.
2. The catalytic process for the production of deuterated benzene as recited in claim 1, wherein: the platinum carbon is added into a mixed solution of benzene and heavy water through a manual powder valve, the manual powder valve comprises,
a valve body (100);
a pivot shaft (200) located within the valve body (100), the pivot shaft (200) being rotatable about a pivot axis;
a valve plate (300) located within the valve body (100), the valve plate (300) supported on the pivot shaft (200); and the number of the first and second groups,
a pivoting driving device (400), wherein the pivoting driving device (400) comprises a support (401) positioned outside the valve body (100) and an operating shaft (402) connected with the pivoting shaft (200), and the operating shaft (402) is rotatably connected with the support (401);
wherein a limiting component (403) is further arranged between the operating shaft (402) and the support (401), and the limiting component (403) is used for limiting the rotation of the operating shaft (402).
3. The catalytic process for the production of deuterated benzene as recited in claim 2, wherein: the limiting assembly (403) comprises a first connection (403a) on the operating shaft (402) and a second connection (403b) on the support (401);
wherein the first connector (403a) and the second connector (403b) are complementary in structure and are connectable to each other;
wherein the first connector (403a) is movable on the operating shaft (402) to disengage the second connector (403 b).
4. The catalytic process for the production of deuterated benzene as recited in claim 3, wherein: a sliding pipe (404) sleeved outside the operating shaft (402) is arranged on the first connecting piece (403a), and the first connecting piece (403a) moves on the operating shaft (402) through the sliding pipe (404);
an accommodating cavity (N1) for accommodating the sliding tube (404) is formed in the support (401), and the second connecting piece (403b) is located in the accommodating cavity (N1).
5. The catalytic process for the production of deuterated benzene as recited in claim 4, wherein: the operating shaft (402) is provided with a key block (402a), and the sliding pipe (404) moves along the key block (402a) in a guiding way through a key slot (N2).
6. The catalytic process for the production of deuterated benzene as recited in claim 4 or 5, wherein: the first connecting piece (403a) protrudes out of the sliding pipe (404), the second connecting piece (403b) is in a groove shape which is complementary to the first connecting piece (403a), and the second connecting piece (403b) is arranged on the inner wall of the accommodating cavity (N1);
wherein the second connector (403b) extends along the axial direction, an opening is formed on one side of the second connector (403b) facing the sliding tube (404), and when the sliding tube (404) moves, the first connector (403a) passes through the opening to be separated from the second connector (403 b).
7. The catalytic process for the production of deuterated benzene as recited in claim 6, wherein: the first connecting pieces (403a) are uniformly distributed along the circumferential direction of the sliding tube (404), and the second connecting pieces (403b) are correspondingly uniformly distributed.
8. The catalytic process for the production of deuterated benzene as recited in any one of claims 4, 5 and 7, wherein: a bearing (405) is further arranged at an opening of the accommodating cavity (N1), an outer ring (405a) of the bearing (405) is fixedly connected with the support (401), and an inner ring (405b) of the bearing (405) is provided with a matching groove (N3) for the first connecting piece (403a) to pass through respectively;
wherein the first connector (403a) is positioned in the mating slot (N3) when the first connector (403a) is disengaged from the second connector (403 b).
9. The catalytic process for the production of deuterated benzene as recited in claim 8, wherein: the containing cavity (N1) comprises a first cavity (N1a) and a second cavity (N1b), the second connecting piece (403b) is positioned on the inner wall of the first cavity (N1a), the inner diameter of the second cavity (N1b) is larger than the distance between the first connecting pieces (403a) on two sides of the sliding pipe (404), and the bearing (405) is positioned at the opening of the second cavity (N1 b);
the first connecting pieces (403a) are in a straight tooth shape, the inner wall of the second cavity (N1b) is further provided with a spring ball (406), and the spring ball (406) is located between every two adjacent first connecting pieces (403 a).
10. The catalytic process for the production of deuterated benzene as recited in claim 9, wherein: a tension spring (407) connected with the sliding pipe (404) is further arranged in the first cavity (N1a), and the first connecting piece (403a) is connected with the second connecting piece (403b) in an embedded manner through the pretightening force of the tension spring (407);
the sliding pipe (404) is further connected with a handle (404a), the operating shaft (402) is further connected with a rotating handle (402b), and a magnetic part (404b) capable of being connected with the rotating handle (402b) is arranged on the handle (404 a).
CN202011640442.4A 2020-12-31 2020-12-31 Catalytic production process of deuterated benzene Pending CN112778072A (en)

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TW200413274A (en) * 2002-12-27 2004-08-01 Wako Pure Chem Ind Ltd Deuteration or tritiation method
CN1906143A (en) * 2004-01-23 2007-01-31 和光纯药工业株式会社 Method of deuteration using mixed catalyst
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