Liquid metal vacuum titration device

Abstract

The invention relates to the technical field of vacuum titration devices, in particular to a liquid metal vacuum titration device. According to the technical scheme, the device comprises a vacuum chamber, the vacuum chamber comprises a vacuum cavity body, and one side of the vacuum cavity body is fixedly connected with an air extractor unit; the vacuum titration mechanism is fixedly mounted at the top of the vacuum cavity; the vacuum moving platform comprises a heating disc which is arranged in the vacuum cavity in a sliding manner, one side of the vacuum cavity is provided with a vacuum moving device which is used for driving the heating disc to horizontally move, and a crucible and a titration plate are fixedly arranged on the heating disc. According to the invention, liquid extraction and titration are realized in a mechanical transmission manner under the condition that a vacuum environment is not damaged, the size of titration liquid drops can be conveniently controlled, and the convenience and precision of titration are improved.

Description

Technical Field

[0001] The invention relates to the technical field of vacuum titration devices, in particular to a liquid metal vacuum titration device. Background Art

[0002] The vacuum environment provides good reaction conditions for some demanding chemical reactions, which can maintain the accuracy and repeatability of the reaction and prevent unnecessary side reactions. Two or more reactant samples are placed in a vacuum environment. How to titrate one of the reactants into another or several other reactants in a vacuum environment is a difficult problem that needs to be solved. Take the liquid metal wetting system as an example: Usually, in a vacuum heating environment, a syringe is used to suck the titration sample in the crucible into the injection chamber, and then titrate it onto the titration plate, and a high-speed camera is used to take pictures and measure the droplet titration angle. However, the injection port of the syringe is in a vacuum environment. If the vacuum degree in the syringe chamber is higher than the vacuum in the device at this time, the syringe will automatically discharge the reactants in the chamber, and it will also affect the vacuum in the device; on the contrary, if the vacuum in the syringe is lower than the vacuum in the device, the reactants in the syringe chamber will be difficult to be discharged.

[0003] Therefore, how to ensure that the vacuum in the device is not affected while being able to easily control the titration liquid is a problem to be solved. The present application proposes a liquid metal vacuum titration device. Summary of the invention

[0004] The purpose of the present invention is to propose a liquid metal vacuum titration device in view of the problem in the background technology of how to ensure that the vacuum in the device is not affected while being able to easily control the titration liquid.

[0005] The technical solution of the present invention is a liquid metal vacuum titration device, comprising:

[0006] A vacuum chamber, wherein the vacuum chamber comprises a vacuum cavity body, and a vacuum unit is fixedly connected to one side of the vacuum cavity body;

[0007] A vacuum titration mechanism fixedly mounted on the top of the vacuum chamber;

[0008] The vacuum moving platform comprises a heating plate slidably mounted in the vacuum chamber, a vacuum moving device for driving the heating plate to move horizontally is arranged on one side of the vacuum chamber, and a crucible and a titration plate are fixedly mounted on the heating plate.

[0009] Optionally, the vacuum titration mechanism includes a telescopic tube, an aperture disk and a vacuum magnetic rod fixed on the vacuum chamber, a CF35 sealing port is fixedly installed on the top of the vacuum magnetic rod, a spiral linear introducer is rotatably installed on the CF35 sealing port, the bottom of the spiral linear introducer is threadedly connected to a titration rod slidably installed in the vacuum magnetic rod, the inner shaft of the vacuum magnetic rod is fixedly connected to the rotating disk of the aperture disk via the telescopic tube, and the outer shaft of the vacuum magnetic rod is fixedly connected to the fixed disk of the aperture disk via the telescopic tube.

[0010] Optionally, a heating rod is fixedly installed in the titration rod, the titration rod is a hollow structure, and one end of the power cord of the heating rod passes through the titration rod and the spiral linear introducer, is pulled out and connected to an external power supply.

[0011] Optionally, a cover plate is fixed on the top of the vacuum chamber, a plurality of snap-on quick clamps in a circular array are welded between the cover plate and the vacuum chamber, a KF40 connection port 1 is installed on the cover plate, and the vacuum titration mechanism is sealed and connected to the vacuum chamber through the KF40 connection port 1.

[0012] Optionally, an observation window and a KF25 vacuum electrode are installed on the vacuum chamber.

[0013] Optionally, a KF40 connecting port 2 is fixed to the side of the vacuum chamber, and the vacuum moving platform is sealed and connected to the vacuum chamber through the KF40 connecting port 2.

[0014] Optionally, a KF40 connection port 3 is welded on one side of the vacuum chamber, and the vacuum unit is sealed and connected via the KF40 connection port 3.

[0015] Optionally, a heating plate power cord is connected to the bottom of the heating plate, and a copper nose is fixedly connected to one end of the heating plate power cord.

[0016] Optionally, the vacuum moving device includes an L-shaped base, on which a roller screw is rotatably mounted, a rotating handle is fixed to one end of the roller screw, a sliding plate is slidably mounted on the L-shaped base and threadedly connected to the roller screw, a bellows is installed between the sliding plate and one end of the L-shaped base, one end of the bellows is fixedly connected to the vacuum chamber, a moving rod is fixed in the bellows, one end of the moving rod extends into the vacuum chamber and is fixedly connected to the heating plate.

[0017] Compared with the prior art, the present invention has at least one of the following beneficial technical effects:

[0018] The vacuum magnetic rod is used as the power device of the titration device, and the aperture structure is used as the titration plate structure, so that the extraction and titration of the liquid can be realized without destroying the vacuum environment by mechanical transmission.

[0019] A pointed titration rod with a thread is used as a drainage rod, and the titration sample falls along the titration rod under the action of gravity; at the same time, the size of the titration droplet is controlled in conjunction with the opening and closing angle of the aperture disk;

[0020] A heating rod is installed between the spiral linear introducer and the titration rod to heat the titration rod to prevent the titration sample from solidifying on the titration rod.

[0021] The present invention realizes the extraction and titration of liquid without destroying the vacuum environment by means of mechanical transmission, which facilitates the control of the size of the titration droplet and improves the convenience and accuracy of the titration. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] Figure 1 It is a schematic diagram of the structure of a titration device used in a vacuum environment;

[0023] Figure 2 It is a schematic diagram of the structure of a vacuum titration device;

[0024] Figure 3 Schematic diagram of the vacuum chamber structure;

[0025] Figure 4 This is a schematic diagram of the vacuum mobile platform structure.

[0026] Reference numerals: 1. vacuum titration mechanism; 2. vacuum chamber; 3. vacuum mobile platform; 101. spiral linear introducer; 102. CF35 sealing port; 103. vacuum magnetic rod; 104. titration rod; 105. telescopic tube; 106. aperture disk; 107. heating rod; 201. cover plate; 202. observation window; 203. vacuum chamber; 204. exhaust unit; 205. KF40 connection port 1; 206. buckle-type quick clamp; 2 07. KF40 connector 2; 208. KF25 vacuum electrode; 209. KF40 connector 3; 3. Vacuum moving platform; 301. Crucible; 302. Titration plate; 303. Heating plate; 304. Heating plate power cord; 305. Copper nose; 306. Vacuum moving device; 3061. Roller screw; 3062. Turning handle; 3063. Bellows; 3064. Moving rod; 3065. L-shaped base; 3066. Sliding plate. DETAILED DESCRIPTION

[0027] The following will be combined with the drawings in the embodiments of the present application to clearly and completely describe the technical solutions in the embodiments of the present application. Obviously, the described embodiments are only part of the embodiments of the present application, not all of the embodiments. Based on the embodiments in the application, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of this application.

[0028] Example

[0029] like Figure 1 As shown, a liquid metal vacuum titration device proposed in the present invention includes three parts: a vacuum titration mechanism 1, a vacuum chamber 2 and a vacuum moving platform 3. Each part is described in detail below.

[0030] See also Figure 2 In this embodiment, the vacuum titration mechanism 1 includes a telescopic tube 105, an aperture disk 106 and a vacuum magnetic rod 103 fixed on the vacuum chamber 203. The telescopic tube 105 is made of 316 stainless steel, with a thickness of 2 to 4 mm and a telescopic range of 10 to 20 mm. The telescopic tube 105 can provide a certain activity margin for the vacuum magnetic rod.

[0031] In this embodiment, a CF35 sealing port 102 is fixedly installed on the top of the vacuum magnetic rod 103, a spiral linear introducer 101 is rotatably installed on the CF35 sealing port 102, the bottom of the spiral linear introducer 101 is threadedly connected to a titration rod 104 slidably installed in the vacuum magnetic rod 103, the inner axis of the vacuum magnetic rod 103 is fixedly connected to the rotating disk of the aperture disk 106 via a telescopic tube 105, and the outer axis of the vacuum magnetic rod 103 is fixedly connected to the fixed disk of the aperture disk 106 via a telescopic tube 105. When extracting a sample, press and rotate the vacuum magnetic rod 103 clockwise to drive the aperture disk 106 to move down and expand to extract the titration sample; lift and rotate the vacuum magnetic rod 103 counterclockwise to drive the aperture disk 106 to rise and close. When titrating a sample, adjust the spiral linear introducer 101 to slowly lower the titration rod 104, and at the same time rotate the vacuum magnetic rod 103 at a constant speed to slowly open the aperture disk to an angle large enough for only the tip of the titration rod to pass through. The titration sample drips along the titration rod 104 under the action of gravity, and the size of the droplets is controlled by adjusting the spiral linear introducer 101 and the aperture disk 106.

[0032] It is worth noting that the aperture disk 106 is made of SUS316 stainless steel with a thickness of 3 to 5 mm, a fixed disk diameter of 20 mm, a rotating disk diameter of 15 mm, and a scale is marked on the outside of the fixed disk. The scale is calculated by the formula: π×square of the radius of the rotating disk×height of the fixed disk in millimeters. During the experiment, the titration sample is quantitatively extracted by observing the scale extending into the crucible 301 through the observation window.

[0033] Among them, a heating rod 107 is fixedly installed in the titration rod 104. The titration rod 104 is a hollow structure. One end of the power cord of the heating rod 107 passes through the titration rod 104 and the spiral linear introducer 101 and is pulled out and connected to an external power supply to heat the titration rod 104 to prevent the titration sample from solidifying.

[0034] See also Figure 3In this embodiment, the vacuum chamber 2 includes a vacuum cavity 203, and a vacuum pump 204 is fixedly connected to one side of the vacuum cavity 203. The vacuum pump 204 is composed of a 680L / s turbomolecular pump and a mechanical pump connected in sequence, which can achieve a background vacuum of 3.7E-3Pa. The vacuum pump 204 is used to extract gas from the vacuum cavity 203. A cover plate 201 is fixed on the top of the vacuum cavity 203. The cover plate 201 and the vacuum cavity 203 are both made of 316 stainless steel with a thickness of 3 to 5mm. A plurality of snap-on quick clamps 206 in a circular array are welded between the cover plate 201 and the vacuum cavity 203. There are eight snap-on quick clamps 206, which can conveniently seal the cover plate 201 and the vacuum cavity 203. The snap-on quick clamps 206 are made of galvanized iron. The large snap-on quick clamps 206 are selected to provide a clamping force of 350KG. A KF40 connection port 205 is installed on the cover plate 201 , and the vacuum titration mechanism 1 is sealedly connected to the vacuum chamber 203 via the KF40 connection port 205 .

[0035] An observation window 202 and a KF25 vacuum electrode 208 are installed on the vacuum chamber 203 . The outer end of the KF25 vacuum electrode 208 is connected to a power supply. Two observation windows 202 are provided for observing the titration condition in the vacuum chamber 2 .

[0036] In addition, a second KF40 connection port 207 is fixed on the side of the vacuum chamber 203, and the vacuum moving platform 3 is sealed and connected to the vacuum chamber 2 through the second KF40 connection port 207. A third KF40 connection port 209 is welded on one side of the vacuum chamber 203, and the exhaust unit 204 is sealed and connected through the third KF40 connection port 209.

[0037] See also Figure 4 In this embodiment, the vacuum moving platform 3 includes a heating plate 303 slidably installed in the vacuum chamber 203. A vacuum moving device 306 for driving the heating plate 303 to move horizontally is provided on one side of the vacuum chamber 203. A crucible 301 and a titration plate 302 are fixedly installed on the heating plate 303. The crucible 301 is used to hold the titration sample. The heating plate 303 adopts a radiation heating method to uniformly heat the samples on the crucible 301 and the titration plate 302. The aperture disk 106 moves down and expands to extract the titration sample in the crucible 301.

[0038] A heating plate power line 304 is connected to the bottom of the heating plate 303, and one end of the heating plate power line 304 is fixedly connected to a copper nose 305. A certain margin can be provided when the heating plate moves to prevent the joint from breaking.

[0039] The vacuum moving device 306 includes an L-shaped base 3065, on which a roller screw 3061 is rotatably mounted, and a rotating handle 3062 is fixed at one end of the roller screw 3061. The roller screw 3061 is rotated by rotating the rotating handle 3062. A sliding plate 3066 threadedly connected to the roller screw 3061 is slidably mounted on the L-shaped base 3065. The sliding plate 3066 is moved by rotating the roller screw 3061. The sliding plate 3066 is moved between the sliding plate 3066 and one end of the L-shaped base 3065. A bellows 3063 is installed, one end of which is fixedly connected to the vacuum chamber 203, a moving rod 3064 is fixed inside the bellows 3063, the sliding plate 3066 moves to drive the bellows 3063 to extend and retract, and drives the moving rod 3064 to move horizontally, one end of the moving rod 3064 extends into the vacuum chamber 203 and is fixedly connected to the heating plate 303, the horizontal movement of the operating rod 3064 drives the heating plate 303 to move horizontally, and the vacuum degree of the device as a whole is ensured by the setting of the bellows 3063. Adjust the vacuum moving device 306 to move the titration plate 302 to the right below the vacuum titration mechanism 1 for titration.

[0040] Working principle: The vacuum titration mechanism 1 and the vacuum moving platform 3 are sealed and connected to the vacuum chamber 2, the exhaust unit 204 is turned on to put the vacuum chamber 2 in a vacuum environment, the KF25 vacuum electrode 208 is connected to the power supply, and the switch of the heating plate 303 is turned on to heat the sample in the crucible 301, the position of the crucible 301 is checked through the observation window 202, and the vacuum moving device 306 is adjusted until the crucible 301 is under the vacuum titration mechanism 1. Press and rotate the vacuum magnetic rod 103 clockwise to drive the aperture disk 106 to move down and expand to extract the titration sample in the crucible 301; lift and rotate the vacuum magnetic rod 103 counterclockwise to drive the aperture disk 106 to rise and close to achieve sample extraction; at this time, adjust the vacuum moving device 306 to make the titration plate 302 under the vacuum titration mechanism 1, and then adjust the spiral linear introducer 101 to slowly lower the titration rod 104, and at the same time, rotate the vacuum magnetic rod 103 at a uniform speed to slowly open the aperture disk 106 to an angle large enough for only the tip of the titration rod 104 to pass through, and the titration sample drips along the titration rod 104 under the action of gravity, and the size of the titration droplet is controlled by adjusting the spiral linear introducer 101 and the aperture disk 106.

[0041] The above specific embodiments are only several optional embodiments of the present invention. Based on the technical solutions of the present invention and the relevant inspirations of the above embodiments, those skilled in the art can make various alternative improvements and combinations to the above specific embodiments.

Claims

1. A liquid metal vacuum titration device, characterized in that: include: A vacuum chamber (2), the vacuum chamber (2) comprising a vacuum cavity (203), one side of the vacuum cavity (203) being fixedly connected to a vacuum unit (204); A vacuum titration mechanism (1) fixedly mounted on the top of the vacuum chamber (203); A vacuum movable platform (3), the vacuum movable platform (3) comprising a heating plate (303) slidably mounted in the vacuum chamber (203), a vacuum movable device (306) for driving the heating plate (303) to move horizontally is arranged on one side of the vacuum chamber (203), and a crucible (301) and a titration plate (302) are fixedly mounted on the heating plate (303).

2. A liquid metal vacuum titration device according to claim 1, characterized in that: The vacuum titration mechanism (1) comprises a telescopic tube (105), an aperture disk (106), and a vacuum magnetic rod (103) fixed on the vacuum chamber (203); a CF35 sealing port (102) is fixedly mounted on the top of the vacuum magnetic rod (103); a spiral linear introducer (101) is rotatably mounted on the CF35 sealing port (102); a titration rod (104) slidably mounted in the vacuum magnetic rod (103) is threadedly connected to the bottom of the spiral linear introducer (101); an inner shaft of the vacuum magnetic rod (103) is fixedly connected to a rotating disk of the aperture disk (106) via the telescopic tube (105); and an outer shaft of the vacuum magnetic rod (103) is fixedly connected to a fixed disk of the aperture disk (106) via the telescopic tube (105).

3. A liquid metal vacuum titration device according to claim 2, characterized in that: A heating rod (107) is fixedly installed in the titration rod (104); the titration rod (104) is a hollow structure; one end of a power cord of the heating rod (107) passes through the titration rod (104) and the spiral linear introducer (101), is pulled out, and is connected to an external power supply.

4. A liquid metal vacuum titration device according to claim 1, characterized in that: A cover plate (201) is fixed on the top of the vacuum chamber (203); a plurality of snap-on quick clamps (206) in a ring array are welded between the cover plate (201) and the vacuum chamber (203); a KF40 connection port 1 (205) is installed on the cover plate (201); and the vacuum titration mechanism (1) is sealedly connected to the vacuum chamber (203) via the KF40 connection port 1 (205).

5. A liquid metal vacuum titration device according to claim 4, characterized in that: An observation window (202) and a KF25 vacuum electrode (208) are installed on the vacuum chamber (203).

6. A liquid metal vacuum titration device according to claim 5, characterized in that: A second KF40 connection port (207) is fixed on the side of the vacuum cavity (203), and the vacuum movable platform (3) is sealedly connected to the vacuum chamber (2) via the second KF40 connection port (207).

7. A liquid metal vacuum titration device according to claim 6, characterized in that: A KF40 connection port three (209) is welded on one side of the vacuum chamber (203), and the vacuum unit (204) is sealed and connected via the KF40 connection port three (209).

8. A liquid metal vacuum titration device according to claim 1, characterized in that: The bottom of the heating plate (303) is connected to a heating plate power line (304), and one end of the heating plate power line (304) is fixedly connected to a copper nose (305).

9. A liquid metal vacuum titration device according to claim 8, characterized in that: The vacuum moving device (306) comprises an L-shaped base (3065), on which a roller screw (3061) is rotatably mounted, one end of which is fixed with a rotating handle (3062), and on which a sliding plate (3066) threadedly connected to the roller screw (3061) is slidably mounted, and a bellows (3063) is mounted between the sliding plate (3066) and one end of the L-shaped base (3065), one end of which is fixedly connected to the vacuum chamber (203), and a moving rod (3064) is fixed in the bellows (3063), and one end of which extends into the vacuum chamber (203) and is fixedly connected to the heating plate (303).

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