Titanium tetrachloride gas sampling device

Abstract

The utility model belongs to the technical field of electronic gas detection devices, and particularly relates to a titanium tetrachloride gas sampling device which at least comprises a main pipeline with a titanium tetrachloride gas inlet at the front end, and the main pipeline is sequentially connected with a first nitrogen purging pipeline, a vacuumizing pipeline, a jacket type condenser, a second nitrogen purging pipeline and a reagent bottle. Wherein the first nitrogen purging pipeline and the second nitrogen purging pipeline are connected with nitrogen supply equipment, the vacuumizing pipeline is connected with vacuumizing equipment, and the tail end of the main pipeline is connected with a reagent bottle; the reagent bottle, the tail end of the main pipeline and the second nitrogen purging pipeline are all arranged in the glove box; the titanium tetrachloride gas inlet of the main pipeline, the first nitrogen purging pipeline, the vacuumizing pipeline, the main pipeline between the jacketed condenser and the glove box and the second nitrogen purging pipeline are respectively provided with a valve. The scheme provides a device which can sample titanium tetrachloride gas in the rectification process of high-purity titanium tetrachloride production, is convenient for real-time analysis and can be repeatedly used.

Description

Technical Field

[0001] The utility model belongs to the technical field of electronic gas detection devices, in particular to a titanium tetrachloride gas sampling device. Background Art

[0002] Titanium tetrachloride is a common raw material in the electronic gas industry. Adsorption distillation is a necessary process in the production of high-purity titanium tetrachloride. In order to analyze the purity and quality of titanium tetrachloride in real time during the distillation process, it is urgent to design a titanium tetrachloride gas sampling device. However, conventional existing technologies all sample liquid titanium tetrachloride. For example, a titanium tetrachloride sampling bottle provided by the Chinese utility model patent "CN208206583U" cannot sample gaseous titanium tetrachloride. Summary of the invention

[0003] In order to achieve the above object, the utility model provides a device which can sample titanium tetrachloride gas in the distillation process of high-purity titanium tetrachloride production for real-time analysis.

[0004] The specific technical solution adopted is: a titanium tetrachloride gas sampling device, which at least includes a main pipeline with a titanium tetrachloride gas inlet at the front end, and the main pipeline is connected to a first nitrogen purge pipeline, a vacuum pipeline, a jacketed condenser, a second nitrogen purge pipeline and a reagent bottle in sequence, wherein the first nitrogen purge pipeline and the second nitrogen purge pipeline are connected to a detachable nitrogen supply device, the vacuum pipeline is connected to a detachable vacuum equipment, and the end of the main pipeline is connected to a detachable reagent bottle; the reagent bottle, the end of the main pipeline and the second nitrogen purge pipeline are all arranged in a glove box; the titanium tetrachloride gas inlet of the main pipeline, the first nitrogen purge pipeline, the vacuum pipeline, the main pipeline between the jacketed condenser and the glove box, and the second nitrogen purge pipeline are respectively provided with valves.

[0005] Moreover, the nitrogen supply equipment is a nitrogen machine or a nitrogen bottle, and the vacuum equipment is a vacuum machine.

[0006] Furthermore, the jacketed condenser at least includes a gas inlet, a heat exchange coil, a gas inlet, a refrigerant inlet and a refrigerant outlet.

[0007] Moreover, the reagent bottle is made of PFA.

[0008] Moreover, all valves are regulating valves.

[0009] Compared with the prior art, the beneficial effect of the technical solution is that it provides a device that can sample titanium tetrachloride gas during the distillation process of high-purity titanium tetrachloride production for real-time analysis. The device can be reused, and the sampling process does not affect the production of high-purity titanium tetrachloride. BRIEF DESCRIPTION OF THE DRAWINGS

[0010] Figure 1 It is a structural schematic diagram of an embodiment;

[0011] Figure 2 It is a schematic diagram of the structure of the sampling device located in the glove box area;

[0012] Description of reference numerals:

[0013] Main pipeline 1, titanium tetrachloride gas inlet 2, first nitrogen purge pipeline 3, vacuum pipeline 4, jacketed condenser 5, second nitrogen purge pipeline 6, reagent bottle 7, glove box 8, first valve 9, second valve 10, third valve 11, fourth valve 12, fifth valve 13, two glove installation holes 14. DETAILED DESCRIPTION

[0014] The present invention is described in detail below with reference to the accompanying drawings and embodiments, but the present invention is not limited to the following embodiments.

[0015] A titanium tetrachloride gas sampling device, such as Figure 1 and Figure 2 As shown, the front end of the main pipeline 1 is a titanium tetrachloride gas inlet 2, which can be connected to the titanium tetrachloride gas outlet of the distillation tower. The main pipeline is connected to the first nitrogen purge pipeline 3, the vacuum pipeline 4, the jacketed condenser 5, the second nitrogen purge pipeline 6 and the reagent bottle 7 in sequence. The main pipeline is fixedly connected to the first nitrogen purge pipeline and the vacuum pipeline as a whole. The first nitrogen purge pipeline and the second nitrogen purge pipeline are also connected to a detachable nitrogen supply device (the nitrogen supply device is not drawn in the figure, and the nitrogen supply device connected to the first nitrogen purge pipeline is actually assembled in Figure 1 On the right side of the second valve 10, the nitrogen supply device connected to the second nitrogen purge pipeline is actually installed on Figure 1 the first nitrogen purge pipeline and the second nitrogen purge pipeline can be connected to the same or different nitrogen supply equipment), the vacuum pipeline is also connected to a detachable vacuum device (the vacuum device is not shown in the figure, the vacuum device is actually assembled in Figure 1 The end of the main pipeline is connected to a detachable reagent bottle. The reagent bottle, the end of the main pipeline and the second nitrogen purge pipeline are all arranged in the glove box 8, that is, in addition to the two glove installation holes 14, the glove box needs at least two holes to allow the end of the main pipeline and the second nitrogen purge pipeline to enter, respectively. Figure 1 The area enclosed by the middle dotted line is the glove box. Figure 2 The schematic diagram of the sampling device structure in the glove box area is shown in FIG. The titanium tetrachloride gas inlet of the main pipeline is provided with a first valve 9, the first nitrogen purge pipeline is provided with a second valve 10, the vacuum pipeline is provided with a third valve 11, the main pipeline between the jacketed condenser and the glove box is provided with a fourth valve 12, and the second nitrogen purge pipeline is provided with a fifth valve 13.

[0016] Moreover, the nitrogen supply equipment is a nitrogen machine or a nitrogen bottle, and the vacuum equipment is a vacuum machine.

[0017] Furthermore, the jacketed condenser at least includes a gas inlet, a heat exchange coil, a gas inlet, a refrigerant inlet and a refrigerant outlet.

[0018] Because titanium tetrachloride has a high boiling point, it is difficult to purge, easily remains on the pipeline, and is very easy to deteriorate into titanium dioxide, causing pipeline blockage, so the reagent bottle is made of PFA material, and the main pipeline between the fourth valve, the fifth valve and the reagent bottle is made of PFA material. The pipelines in other parts are all 1 / 4EP pipes.

[0019] Moreover, the first valve, the second valve, the third valve, the fourth valve and the fifth valve are all regulating valves.

[0020] Moreover, multiple reagent bottles can be arranged in the glove box.

[0021] The method of using the sampling device is as follows: Step 1. Before sampling, first close the first valve 9, the second valve 10, the third valve 11 and the fourth valve 12; then open the second valve 10 to purge with nitrogen, then close the second valve 10 and open the third valve 11 to evacuate, then close the third valve 11 and open the second valve 10 to purge with nitrogen, repeat the nitrogen purge and vacuum operation several times to replace the original air in the main pipeline.

[0022] Step 2. After the replacement is completed, open the third valve 11 to evacuate the pipeline and then close the third valve 11, then open the first valve 9 to allow the titanium tetrachloride gas sample to be tested to enter the main pipeline, then close the first valve 9 and wait for the titanium tetrachloride gas to condense in the jacketed condenser to form titanium tetrachloride liquid.

[0023] Step 3. After the titanium tetrachloride gas sample is condensed into liquid, the fourth valve 12 is opened first and then the second valve 10 is opened, and the titanium tetrachloride liquid in the pipeline is blown into the reagent bottle 7 made of PFA material with nitrogen.

[0024] Step 4. After the reagent bottle sampling is completed in the glove box, the fourth valve 12 is closed, the main pipeline is removed from the titanium tetrachloride gas outlet of the distillation tower, and then the pipeline is cleaned or purged with nitrogen.

[0025] Step 5. After completing the reagent bottle sampling in the glove box, transfer the reagent bottle to the clean room for real-time analysis.

[0026] During the whole sampling process, the fifth valve 13 is kept open and purged with nitrogen at a flow rate of 1L / min to avoid pipeline air pollution, that is, to avoid contamination of the main pipeline from the fourth valve 12 to the reagent bottle. Multiple reagent bottles can be set in the glove box, and the end of the main pipeline can be disassembled and installed with a new reagent bottle and steps 1 to 4 can be repeated to take multiple samples. The device can be reused, and the sampling process does not affect the production of high-purity titanium tetrachloride, which is convenient for real-time analysis of titanium tetrachloride gas.

Claims

1. A titanium tetrachloride gas sampling device, comprising at least a main pipeline with a titanium tetrachloride gas inlet at the front end, characterized in that: The main pipeline is connected to the first nitrogen purge pipeline, the vacuum pipeline, the jacketed condenser, the second nitrogen purge pipeline and the reagent bottle in sequence, wherein the first nitrogen purge pipeline and the second nitrogen purge pipeline are connected to a detachable nitrogen supply device, the vacuum pipeline is connected to a detachable vacuum device, and the end of the main pipeline is connected to a detachable reagent bottle; the reagent bottle, the end of the main pipeline and the second nitrogen purge pipeline are all arranged in the glove box; the titanium tetrachloride gas inlet of the main pipeline, the first nitrogen purge pipeline, the vacuum pipeline, the main pipeline between the jacketed condenser and the glove box, and the second nitrogen purge pipeline are respectively provided with valves.

2. The titanium tetrachloride gas sampling device according to claim 1, characterized in that: The nitrogen supply equipment is a nitrogen machine or a nitrogen bottle, and the vacuum equipment is a vacuum pump.

3. The titanium tetrachloride gas sampling device according to claim 1, characterized in that: The jacketed condenser at least comprises a gas inlet, a heat exchange coil, a gas inlet, a refrigerant inlet and a refrigerant outlet.

4. The titanium tetrachloride gas sampling device according to claim 1, characterized in that: The reagent bottles are made of PFA.

5. The titanium tetrachloride gas sampling device according to claim 1, characterized in that: All valves are regulating valves.

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