A sampling method and device for the production of refined titanium tetrachloride

Abstract

The invention discloses a sampling method and device for use in a refined titanium tetrachloride production process, and relates to the technical field of refined titanium tetrachloride production. The method comprises a storage tank, wherein sampling channels are installed at the upper, middle and lower positions of the side of the storage tank, and a piston sampling rod is slidably arranged inside the sampling channel, and the end of the piston sampling rod passes through the sampling channel and is fixed with a vertical plate, a mixing tank is fixed on the outer side of the vertical plate, and a sampling syringe is installed at the lower end of the mixing tank, and an insertion stirring mechanism is installed between the mixing tank and the sampling syringe. The main effect of the invention is that the volume of the gas discharged from the sampling channel is the same as the volume of the sample liquid inhaled into the sampling channel, and the gas discharged from the sampling channel will compress the space in the storage tank of the same volume by moving a sealing breathing plate, thereby ensuring that the liquid discharge volume in the storage tank is the same as the compressed volume of the space in the tank, thereby avoiding the generation of the breathing effect.

Description

Technical Field

[0001] The invention relates to the technical field of refined titanium tetrachloride production, in particular to a sampling method and a device used in the refined titanium tetrachloride production process. Background Art

[0002] Titanium tetrachloride, or titanium (IV) chloride, is an inorganic compound with the chemical formula TiCl4, a colorless or slightly yellow liquid with a pungent sour taste.

[0003] In the production of titanium tetrachloride, in order to analyze the production process of each step, control the process parameters, and provide a basis for guiding production, it is necessary to sample titanium tetrachloride.

[0004] At present, domestic manufacturers of refined titanium tetrachloride generally use a sampling device connected by a drainage tube, a sampling valve and a sampling elbow to sample titanium tetrachloride. When sampling, the sampling liquid flows through the drainage tube, the sampling valve and the sampling elbow into the sampling bottle. However, there are many deficiencies in the actual sampling process, as follows:

[0005] Since titanium tetrachloride will react with air to generate fumes at room temperature and pressure, the refined titanium tetrachloride storage tank generally uses the exhaust method to store refined titanium tetrachloride, specifically: first fill the tank with an inert dry gas (helium) that will not react with refined titanium tetrachloride, then inject refined titanium tetrachloride to gradually discharge the helium to achieve the purpose of storing refined titanium tetrachloride without contact with air. Generally speaking, the storage tank is kept in a sealed state at room temperature and pressure, and some helium will remain on the top. When sampling through the sampling tube, the liquid will flow out of the sampling tube under liquid pressure, but under atmospheric pressure, a breathing effect will occur in the tank, that is, the outflow of liquid will inevitably be accompanied by the intake of air (when pouring water from a mineral water bottle upside down in daily life, you will feel that the water comes out very slowly and a large number of bubbles will surge to the bottom of the bottle. This is the breathing effect under atmospheric pressure). Therefore, the traditional sampling method will inevitably be accompanied by a certain amount of air entering;

[0006] Generally speaking, sampling is carried out in a refined titanium tetrachloride storage tank, where the refined titanium tetrachloride is generally in a static state. After being static, the refined titanium tetrachloride will also show stratification. The traditional method can only sample from a single location, resulting in inaccurate sampling results.

[0007] After sampling, a certain amount of titanium tetrachloride remains in the sampling tube. After the sampling bottle is taken away, the residual titanium tetrachloride in the sampling tube is directly exposed to the air, causing a reaction to produce smoke. Summary of the invention

[0008] The technical solution of the present invention aims at the technical problem that the existing technical solutions are too single, and provides a solution that is significantly different from the existing technology. Specifically, the purpose of the present invention is to provide a sampling method and device for the production process of refined titanium tetrachloride, so as to solve the problem proposed in the above background technology that when sampling through a sampling tube, under liquid pressure, the liquid will flow out of the sampling tube, but under atmospheric pressure, a breathing effect will occur in the tank, that is, the outflow of liquid will inevitably be accompanied by the suction of air, so the traditional sampling method will inevitably be accompanied by a certain amount of air entering.

[0009] To achieve the above object, the present invention provides the following technical solution: a sampling method and device for the production of refined titanium tetrachloride, comprising the following steps:

[0010] S1: Take equal amounts of upper, middle and lower sample liquids from the titanium tetrachloride storage tank at the same time, and place the three equal amounts of sample liquids in the same sampling container;

[0011] S2: When taking the upper, middle and lower layers of sample liquid at the same time, the liquid volume lost in the storage tank is replenished with an equal volume of inert gas (helium) through the upper part of the tank to avoid breathing effect and inhalation of air during sampling;

[0012] S3: When extracting the sample liquid in the container, stir the sample liquid in the container evenly to mix the upper, middle and lower layers of the sample liquid.

[0013] A sampling device used in the production process of refined titanium tetrachloride comprises a storage tank, wherein sampling channels are installed at the upper, middle and lower positions of the side of the storage tank, and a piston sampling rod is slidably arranged inside the sampling channel, and the end of the piston sampling rod passes through the sampling channel and is fixed with a vertical plate, a mixing tank is fixed on the outer side of the vertical plate, and a sampling syringe is installed at the lower end of the mixing tank, an insertion stirring mechanism is installed between the mixing tank and the sampling syringe, and the ends of the three sampling channels are commonly connected to a tank pressure-balanced breathing assembly.

[0014] Preferably, a valve is installed at the inner end of the sampling channel close to the storage tank, and a liquid outlet one-way valve is installed at the outer wall of the sampling channel close to the valve, and the end of the liquid outlet one-way valve is connected to the mixing tank through a hose.

[0015] Preferably, the insert stirring mechanism includes a stirring rod and a liquid inlet hole, and the stirring rod is installed at the top center of the mixing tank through a bearing, a through groove is opened at the lower center of the mixing tank, and a rubber sealing plug is provided inside the through groove, a threaded groove is opened through the lower end of the stirring rod, and the liquid inlet holes are symmetrically opened on the sides of the top of the threaded groove.

[0016] Preferably, the outer wall of the liquid extraction end of the sampling syringe is provided with a thread matching the thread groove at the lower end of the stirring rod.

[0017] Preferably, the pressure-balanced breathing assembly in the tank includes an exhaust one-way valve, a breathing duct, a sealed breathing plate, a connecting rod and a guide block, and an exhaust one-way valve is installed at the end of the outer wall of the sampling channel close to the vertical plate, the end of the exhaust one-way valve is connected to one end of the breathing duct through a hose, and the other end of the breathing duct is installed inside the upper end of the storage tank, the breathing duct consists of a vertical pipe and a curved pipe, and sealed breathing plates are installed inside the vertical pipe and the curved pipe, and a connecting rod is connected between the two sealed breathing plates, and guide blocks are evenly distributed in the bending channel of the curved pipe.

[0018] Preferably, the connecting rod and the guide block are in a through-type sliding connection, and the connecting rod is made of a ductile metal material that can be bent to a certain extent.

[0019] Compared with the prior art, the present invention has the following beneficial effects:

[0020] First, open the valves on the three sampling channels on the side of the storage tank, and then pull out three groups of piston sampling rods through the vertical plates. When the piston sampling rods are pulled out horizontally, the three piston sampling rods will gradually draw the refined titanium tetrachloride at the upper, middle and lower positions inside the storage tank into the sampling channels, and when the piston sampling rods move, the gas inside the sampling channel will be pressed into the breathing duct through the exhaust one-way valve and the corresponding hose. The pressure of the gas will cause the sealed breathing plate at the lower end to move upward gradually. The upward movement of the sealed breathing plate at the lower end will drive the sealed breathing plate at the upper end to move the same distance under the action of air pressure and the connecting rod. The effect achieved is: the volume of gas discharged from the sampling channel is the same as the volume of sample liquid inhaled into the sampling channel, and the gas discharged from the sampling channel will compress the same volume of storage tank space by moving the sealed breathing plate, thereby ensuring that the liquid output volume inside the storage tank is the same as the compressed volume of the tank space, thereby avoiding the generation of the breathing effect.

[0021] Next, when the piston sampling rod moves to the maximum stroke, the sample liquid is extracted into the sampling channel, and then the valve is closed. At this time, the sample liquid is locked in the sampling channel, and then the vertical plate is pushed back to gradually reset the piston sampling rod and push the sample liquid in the sampling channel into the mixing tank through the liquid outlet one-way valve and the corresponding hose. Then, the upper end of the sampling syringe is inserted into the mixing tank through the rubber sealing plug and the external thread on the upper end of the sampling syringe corresponds to the internal thread groove on the lower end of the stirring rod. Then, the sampling syringe is pushed continuously. The action between the thread and the inner thread groove at the lower end of the stirring rod forces the stirring rod to rotate adaptively, and when the stirring rod rotates, the three layers of sample liquid in the mixing tank, namely the upper, middle and lower layers, can be stirred and mixed. After the upper end of the sampling syringe is fully inserted, the injection rod is pressed down, and finally the sample liquid in the mixing tank is extracted by the negative pressure generated inside the sampling syringe, thereby solving the problem of inaccurate detection after sampling caused by static stratification of refined titanium tetrachloride in the tank. At the same time, the sampling tube is always kept in a sealed state, thereby avoiding the problem of residual refined titanium tetrachloride in the sampling tube after sampling. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] Figure 1 It is a schematic diagram of the first three-dimensional structure of the present invention;

[0023] Figure 2 It is a schematic diagram of the second three-dimensional structure of the present invention;

[0024] Figure 3 It is a schematic diagram of the third three-dimensional structure of the present invention;

[0025] Figure 4 It is a schematic diagram of the front cross-sectional structure of the present invention;

[0026] Figure 5 It is a schematic diagram of the extraction and enlarged structure of the insertion-type stirring mechanism of the present invention;

[0027] Figure 6 For the present invention Figure 4 The enlarged structural diagram at A in the middle;

[0028] Figure 7 It is a schematic diagram of the top view of the rubber sealing plug at the lower end of the mixing tank of the present invention.

[0029] In the figure: 1. storage tank; 11. sampling channel; 12. valve; 13. piston sampling rod; 14. vertical plate; 2. liquid outlet check valve; 3. exhaust check valve; 4. mixing tank; 41. stirring rod; 42. liquid inlet hole; 43. sampling syringe; 5. breathing pipe; 51. sealed breathing plate; 52. connecting rod; 53. guide block. DETAILED DESCRIPTION

[0030] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0031] See also Figure 1-7 The present invention provides a technical solution: a sampling method and device for the production of refined titanium tetrachloride, comprising the following steps:

[0032] S1: Take equal amounts of upper, middle and lower sample liquids from the titanium tetrachloride storage tank at the same time, and place the three equal amounts of sample liquids in the same sampling container;

[0033] S2: When taking the upper, middle and lower layers of sample liquid at the same time, the liquid volume lost in the storage tank is replenished with an equal volume of inert gas (helium) through the upper part of the tank to avoid breathing effect and inhalation of air during sampling;

[0034] S3: When extracting the sample liquid in the container, stir the sample liquid in the container evenly to mix the upper, middle and lower layers of the sample liquid.

[0035] A sampling device used in the production process of refined titanium tetrachloride comprises a storage tank 1, wherein sampling channels 11 are installed at the upper, middle and lower positions of the side of the storage tank 1, and a piston sampling rod 13 is slidably arranged inside the sampling channel 11, and the end of the piston sampling rod 13 passes through the sampling channel 11 and is fixed with a vertical plate 14, a mixing tank 4 is fixed on the outer side of the vertical plate 14, and a sampling syringe 43 is installed at the lower end of the mixing tank 4, an insertion stirring mechanism is installed between the mixing tank 4 and the sampling syringe 43, and the ends of the three sampling channels 11 are commonly connected to a tank pressure-balanced breathing assembly.

[0036] A valve 12 is installed at the inner end of the sampling channel 11 near the storage tank 1, and a liquid outlet one-way valve 2 is installed at the outer wall of the sampling channel 11 near the valve 12, and the end of the liquid outlet one-way valve 2 is connected to the mixing tank 4 through a hose.

[0037] The inserted stirring mechanism includes a stirring rod 41 and a liquid inlet hole 42, and the stirring rod 41 is installed at the top center of the mixing tank 4 through a bearing, a through groove is opened at the lower center of the mixing tank 4, and a rubber sealing plug is arranged inside the through groove, a threaded groove is opened through the lower end of the stirring rod 41, and the liquid inlet hole 42 is symmetrically opened on the side of the top of the threaded groove.

[0038] The outer wall of the liquid extraction end of the sampling syringe 43 is provided with a thread matching the thread groove at the lower end of the stirring rod 41 .

[0039] The pressure-balanced breathing assembly in the tank includes an exhaust one-way valve 3, a breathing pipe 5, a sealed breathing plate 51, a connecting rod 52 and a guide block 53, and an exhaust one-way valve 3 is installed at the end of the outer wall of the sampling channel 11 near the vertical plate 14, and the end of the exhaust one-way valve 3 is connected to one end of the breathing pipe 5 through a hose, and the other end of the breathing pipe 5 is installed inside the upper end of the storage tank 1, the breathing pipe 5 consists of a vertical pipe and a curved pipe, and sealed breathing plates 51 are installed inside the vertical pipe and the curved pipe, and a connecting rod 52 is connected between the two sealed breathing plates 51, and guide blocks 53 are evenly distributed in the bending channel of the curved pipe.

[0040] The connecting rod 52 and the guide block 53 are in a through-type sliding connection, and the connecting rod 52 is made of a ductile metal material that can be bent to a certain extent.

[0041] Working principle: When using the sampling method and device for the production of refined titanium tetrachloride, first open the valves 12 on the three sampling channels 11 on the side of the storage tank 1, then pull out three sets of piston sampling rods 13 through the vertical plate 14, and when the piston sampling rods 13 are pulled out horizontally, Figure 5 As shown, the three piston sampling rods 13 will gradually draw the refined titanium tetrachloride in the upper, middle and lower positions of the storage tank 1 into the sampling channel 11, and when the piston sampling rod 13 moves, the gas in the sampling channel 11 will be pressed into the breathing pipe 5 through the exhaust check valve 3 and the corresponding hose. Similarly, the gas in the three groups of sampling channels 11 are all pressed into the breathing pipe 5. Figure 6 As shown, the injection of gas will cause the sealed breathing plate 51 at the lower end to move upward gradually. Since the two sealed breathing plates 51 are in a sealed state, the upward movement of the sealed breathing plate 51 at the lower end will drive the sealed breathing plate 51 at the upper end to move the same distance under the action of air pressure and the connecting rod 52. The upper end of the breathing pipe 5 is connected to the interior of the storage tank 1. In simple terms, the volume of gas discharged from the sampling channel 11 is the same as the volume of sample liquid inhaled into the sampling channel 11, and the gas discharged from the sampling channel 11 will compress the space inside the storage tank 1 of the same volume by moving the sealed breathing plate 51, thereby ensuring that the liquid outlet volume inside the storage tank 1 is the same as the compressed volume of the space inside the tank, thereby avoiding the generation of the breathing effect.

[0042] Next, when the piston sampling rod 13 moves to the maximum stroke, the sample liquid is extracted into the sampling channel 11, and then the valve 12 is closed. At this time, the sample liquid is locked in the sampling channel 11, and then the vertical plate 14 is pushed back to gradually reset the piston sampling rod 13 and push the sample liquid in the sampling channel 11 through the liquid outlet one-way valve 2 and the corresponding hose into the mixing tank 4. Similarly, the sample liquids in the three groups of sampling channels 11 are all injected into the mixing tank 4. Then, as shown in FIG. Figure 5As shown, the upper end of the sampling syringe 43 is inserted into the mixing tank 4 through the rubber sealing plug and the external thread on the upper end of the sampling syringe 43 is aligned with the internal thread groove on the lower end of the stirring rod 41. The sampling syringe 43 is then pushed forward. The stirring rod 41 is forced to rotate adaptively under the action of the upper thread on the sampling syringe 43 and the internal thread groove on the lower end of the stirring rod 41. When the stirring rod 41 rotates, the three layers of sample liquid in the mixing tank 4 are stirred and mixed. After the upper end of the sampling syringe 43 is fully inserted, the injection rod is pressed downward. Finally, the sample liquid in the mixing tank 4 is extracted by the negative pressure generated inside the sampling syringe 43. (In this embodiment, the mixing of the three sample liquids in the upper, middle and lower parts is taken as an example. In fact, the more sampling channels 11 are set at different positions, the higher the accuracy of detection after mixed sampling).

[0043] Although the present invention has been described in detail with reference to the aforementioned embodiments, it is still possible for those skilled in the art to modify the technical solutions described in the aforementioned embodiments, or to make equivalent substitutions for some of the technical features therein. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. A sampling device for use in the production process of refined titanium tetrachloride, characterized in that: It comprises a storage tank (1), characterized in that: sampling channels (11) are installed at the upper, middle and lower parts of the side of the storage tank (1), and a piston sampling rod (13) is slidably arranged inside the sampling channel (11), and the end of the piston sampling rod (13) passes through the sampling channel (11) and is fixed with a vertical plate (14), the outer side of the vertical plate (14) is fixed with a mixing tank (4), and the lower end of the mixing tank (4) is installed with a sampling syringe (43), an insertion stirring mechanism is installed between the mixing tank (4) and the sampling syringe (43), and the ends of the three sampling channels (11) are commonly connected to a tank pressure balance type breathing assembly; The tank pressure-balanced breathing assembly comprises an exhaust check valve (3), a breathing pipe (5), a sealed breathing plate (51), a connecting rod (52) and a guide block (53), and an exhaust check valve (3) is installed at the end of the outer wall of the sampling channel (11) close to the vertical plate (14), the end of the exhaust check valve (3) is connected to one end of the breathing pipe (5) through a hose, and the other end of the breathing pipe (5) is installed inside the upper end of the storage tank (1), the breathing pipe (5) is composed of a vertical pipe and a curved pipe, and the vertical pipe and the curved pipe are both installed with sealed breathing plates (51), and a connecting rod (52) is connected between the two sealed breathing plates (51), and the guide blocks (53) are evenly distributed in the bending channel of the curved pipe.

2. A sampling device for use in the production of refined titanium tetrachloride according to claim 1, characterized in that: A valve (12) is installed at the inner end of the sampling channel (11) close to the storage tank (1), and a liquid outlet check valve (2) is installed at the outer wall of the sampling channel (11) close to the valve (12), and the end of the liquid outlet check valve (2) is connected to the mixing tank (4) through a hose.

3. A sampling device for use in the production of refined titanium tetrachloride according to claim 1, characterized in that: The insert-type stirring mechanism comprises a stirring rod (41) and a liquid inlet hole (42), and the stirring rod (41) is mounted at the top center of the mixing tank (4) via a bearing, a through groove is provided at the bottom center of the mixing tank (4), and a rubber sealing plug is provided inside the through groove, a thread groove is provided through the bottom of the stirring rod (41), and the liquid inlet holes (42) are symmetrically provided on the sides of the top of the thread groove.

4. A sampling device for use in the production of refined titanium tetrachloride according to claim 3, characterized in that: The outer wall of the liquid extraction end of the sampling syringe (43) is provided with a thread matching the thread groove at the lower end of the stirring rod (41).

5. A sampling device for use in the production of refined titanium tetrachloride according to claim 1, characterized in that: The connecting rod (52) and the guide block (53) are connected in a through-type sliding manner, and the connecting rod (52) is made of a ductile metal material that can be bent to a certain extent.

6. A sampling method according to any one of claims 1 to 5, characterized in that: The following steps are involved: S1: Take equal amounts of upper, middle and lower sample liquids from the titanium tetrachloride storage tank at the same time, and place the three equal amounts of sample liquids in the same sampling container; S2: When taking the upper, middle and lower layers of sample liquid at the same time, the liquid volume lost in the storage tank is replenished with an equal volume of inert gas through the top of the tank to avoid breathing effect and inhalation of air during sampling; S3: When extracting the sample liquid in the container, stir the sample liquid in the container evenly to mix the upper, middle and lower layers of the sample liquid.

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