System for detecting and analyzing total carbon content in hydrogen containing chlorosilane gas
The system uses a combination of a ten-way valve and a chromatographic column to separate and detect the total carbon content in chlorosilane gas, solving the problem of the inability to monitor the total carbon in circulating hydrogen and ensuring the normal operation and detection accuracy of the equipment.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2025-03-18
- Publication Date
- 2026-03-24
AI Technical Summary
In the polysilicon industry, the total carbon content in circulating hydrogen cannot be monitored, leading to an increase in the total carbon content of the hydrogenation liquid, which affects product quality. Furthermore, chlorosilane gas can damage analytical equipment, causing chromatographic columns and conversion furnaces to fail.
A combined system consisting of a ten-way valve, a quantitative loop, a first chromatographic column, a second chromatographic column, a converter, and an FID detector is used to separate and detect the total carbon content in chlorosilane gas through valve switching and carrier gas purging, thus avoiding the impact of chlorosilane gas on the equipment.
It enables accurate detection of the total carbon content in circulating hydrogen, protecting the normal operation of the analytical equipment and preventing equipment blockage and failure.
Smart Images
Figure CN224035341U_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The utility model relates to the total carbon content detection technical field of hydrogen containing chlorosilane gas, specifically relates to a system for detecting and analyzing the total carbon content of hydrogen containing chlorosilane gas. BACKGROUND
[0002] In the cold hydrogenation process stage in the polysilicon industry, the total carbon in the circulating hydrogen cannot be supervised in the industry, the total carbon in the circulating hydrogen exists in the form of hydrocarbons in liquid silane in the production process, the circulating hydrogen containing high-chlorosilane hydrogen gas cannot detect the total carbon content, which will cause the total carbon in hydrogenation liquid to rise, and ultimately cause the substitution carbon in polysilicon products to rise, reducing the product grade. In addition, the circulating hydrogen contains a large amount of chlorosilane gas, the chlorosilane gas has strong corrosiveness and forms silicon dioxide when it meets air, when it enters the chromatographic column, it will deposit in the valve line, form silicon dioxide, and cause the valve line to be easily blocked. When it enters the TDX-01 column, it will cause the chromatographic column to fail. When it enters the nickel converter, it will cause the converter to fail, that is, the chlorosilane gas in the circulating hydrogen will cause great damage to the analysis and detection equipment, and even analyzing two samples will cause the chromatograph to be paralyzed. SUMMARY
[0003] The utility model discloses a system for detecting and analyzing the total carbon content of hydrogen containing chlorosilane gas, which can detect and analyze the total carbon content in the circulating hydrogen, and avoid the influence of chlorosilane on the detection and analysis device during the detection and analysis of the circulating hydrogen.
[0004] The utility model adopts the technical scheme of:
[0005] A system for detecting and analyzing the total carbon content of hydrogen containing chlorosilane gas is provided, which comprises:
[0006] The ten-way valve, the constant flow ring, the first chromatographic column, the second chromatographic column, the converter and the FID detector; the ten-way valve has ten ports, which are the first carrier gas inlet communication port, the constant flow ring inlet communication port, the sample gas inlet, the sample gas outlet, the constant flow ring outlet communication port, the first chromatographic column outlet communication port, the second carrier gas outlet, the second carrier gas inlet communication port, the first chromatographic column inlet communication port and the second chromatographic column inlet communication port in turn along the counterclockwise direction of the ten-way valve; one end of the constant flow ring is communicated with the constant flow ring inlet communication port of the ten-way valve, and the other end is communicated with the sample gas inlet of the ten-way valve; one end of the first chromatographic column is communicated with the first chromatographic column inlet communication port of the ten-way valve, and the other end is communicated with the first chromatographic column outlet communication port of the ten-way valve; one end of the second chromatographic column is communicated with the second chromatographic column inlet communication port; one end of the converter is communicated with the outlet of the second chromatographic column; one end of the FID detector is communicated with the outlet of the converter.
[0007] Optionally, when the ten-way valve is in the initial state, the first carrier gas inlet communication port is communicated with the second chromatographic column inlet communication port, the constant flow ring inlet communication port is communicated with the sample gas inlet, the sample gas outlet is communicated with the constant flow ring outlet communication port, the first chromatographic column inlet communication port is communicated with the second carrier gas outlet, and the second carrier gas inlet communication port is communicated with the first chromatographic column outlet communication port.
[0008] Optionally, when the ten-way valve is in the working state, the first carrier gas inlet communication port is communicated with the constant flow ring inlet communication port, the constant flow ring outlet communication port is communicated with the first chromatographic column inlet communication port, the second carrier gas outlet is communicated with the second carrier gas inlet communication port, and the first chromatographic column outlet communication port is communicated with the second chromatographic column inlet communication port.
[0009] Optionally, the first chromatographic column is a Porapak Q packed column.
[0010] Optionally, the second chromatographic column is a TDX-01 chromatographic column.
[0011] Optionally, the converter is a methane converter.
[0012] Optionally, the FID detector is connected with a purge pipeline, one end of the purge pipeline is connected with the FID detector inlet, and the other end is a purge gas inlet.
[0013] Optionally, the first carrier gas, the second carrier gas and the purge gas are all nitrogen.
[0014] The sample gas is filled into the quantitative ring by setting the ten-way valve, the quantitative ring, the first chromatographic column, the second chromatographic column, the converter and the FID detector, the first carrier gas enters the second chromatographic column, the converter and the FID detector in turn through the ten-way valve and is subjected to pre-evacuation treatment, the residual gas in the second chromatographic column, the converter and the FID detector is blown out, at the same time, the second carrier gas enters the first chromatographic column through the ten-way valve and is then discharged through the ten-way valve to blow out the residual gas in the first chromatographic column, so as to avoid affecting the detection and analysis of the total carbon content in the circulating hydrogen. Then, the valve path of the ten-way valve is reversed, at this time, the first carrier gas enters the quantitative ring through the ten-way valve, the sample gas in the quantitative ring is blown into the ten-way valve together with the first carrier gas, and then is discharged through the ten-way valve and enters the first chromatographic column for separation, after the methane, carbon monoxide and carbon dioxide in the circulating hydrogen are discharged from the first chromatographic column, the residual hydrogen chloride and silane gas are separated, after the methane, carbon monoxide and carbon dioxide enter the second chromatographic column, the valve path is reversed, at this time, the residual hydrogen chloride and silane gas remain in the first chromatographic column, finally, the second carrier gas enters the first chromatographic column through the ten-way valve to blow back the first chromatographic column, so as to prevent the hydrogen chloride and silane gas in the first chromatographic column from entering the second chromatographic column, the converter and the FID detector, avoid affecting the service life of the second chromatographic column, the converter and the FID detector, and accurately analyze the total carbon content in the circulating hydrogen. BRIEF DESCRIPTION OF DRAWINGS
[0015] In order to more clearly illustrate the technical solutions of the embodiments of the present application or the prior art, the drawings needed to be used in the embodiments or the prior art description will be briefly introduced. Obviously, the drawings in the following description are only some embodiments of the present application, and other drawings can be obtained by those skilled in the art without creative labor.
[0016] Fig. 1 It is a flowchart when the ten-way valve is in the initial state.
[0017] Fig. 2 It is a flowchart when the ten-way valve is in the working state (the first time the valve path is reversed).
[0018] Fig. 3 It is a marking diagram of the ten ports of the ten-way valve.
[0019] Reference signs:
[0020] 1-ten-port valve, 10-first carrier gas inlet communication port, 11-quantitative ring inlet communication port, 12-sample gas inlet, 13-sample gas outlet, 14-quantitative ring outlet communication port, 15-first chromatographic column outlet communication port, 16-second carrier gas discharge port, 17-second carrier gas inlet communication port, 18-first chromatographic column inlet communication port, 19-second chromatographic column inlet communication port;
[0021] 2-quantitative ring, 3-first chromatographic column, 4-second chromatographic column, 5-converter, 6-FID detector. DETAILED DESCRIPTION
[0022] In the description of the utility model, it is understood that the orientation or positional relationship indicated by the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", "axial", "radial", "circumferential" are based on the orientation or positional relationship shown in the drawings, and are only for the convenience of describing the utility model and simplifying the description, and therefore cannot be understood as limiting the utility model indicated or implied by the device or element must have a particular orientation, be constructed and operated in a particular orientation, and therefore cannot be understood as limiting the utility model.
[0023] The following disclosure provides many different embodiments or examples for implementing different structures of the utility model. In order to simplify the disclosure of the utility model, the components and settings of specific examples are described below. Of course, they are only examples, and the purpose is not to limit the utility model.
[0024] The embodiments of the utility model will be described in detail below with reference to the drawings.
[0025] Embodiments
[0026] Please refer to Figs. 1-3 As shown in the drawings, the embodiment provides a system for detecting the total carbon content in hydrogen containing chlorosilane gas, which comprises a ten-port valve 1, a quantitative ring 2, a first chromatographic column 3, a second chromatographic column 4, a converter 5 and an FID detector 6, wherein the ten-port valve 1 has ten ports, and the ten ports are in turn first carrier gas inlet communication port 10, quantitative ring inlet communication port 11, sample gas inlet 12, sample gas outlet 13, quantitative ring outlet communication port 14, first chromatographic column outlet communication port 15, second carrier gas discharge port 16, second carrier gas inlet communication port 17, first chromatographic column inlet communication port 18 and second chromatographic column inlet communication port 19 in counterclockwise direction.
[0027] When the ten-way valve 1 is in the initial state, the inlet of the dosing ring 2 is communicated with the dosing ring inlet communication port 11 of the ten-way valve 1, and the outlet of the dosing ring 2 is communicated with the sample gas inlet 12 of the ten-way valve 1; the inlet of the first chromatographic column 3 is communicated with the first chromatographic column inlet communication port 18 of the ten-way valve 1, and the outlet of the first chromatographic column 3 is communicated with the first chromatographic column outlet communication port 15 of the ten-way valve 1; the inlet of the second chromatographic column 4 is communicated with the second chromatographic column inlet communication port 19 of the ten-way valve 1; one end of the inlet of the converter 5 is communicated with the outlet of the second chromatographic column 4, and one end of the inlet of the FID detector 6 is communicated with the outlet of the converter 5. Then the sample gas is introduced into the dosing ring 2, and the gas in the dosing ring 2 is discharged from the sample gas outlet 13 of the ten-way valve 1, which can remove the residual gas in the dosing ring 2, and at the same time, the first carrier gas and the second carrier gas are introduced into the ten-way valve 1, specifically, the first carrier gas enters the ten-way valve 1 through the first carrier gas inlet communication port 10 of the ten-way valve 1, and is discharged from the second chromatographic column inlet communication port 19 of the ten-way valve 1 and enters the second chromatographic column 4, that is, the first carrier gas is used to discharge all the participating gas contained in the second chromatographic column 4, the converter 5 and the FID detector 6, so as to avoid the accumulation of the participating gas in the second chromatographic column 4, the converter 5 and the FID detector 6, which affects the detection of the total carbon content in the circulating hydrogen; the second carrier gas enters the inside of the first chromatographic column 3 through the first chromatographic column inlet communication port 18 of the ten-way valve 1, blows the residual gas in the first chromatographic column 3 from the outlet of the first chromatographic column 3 to the first chromatographic column outlet communication port 15 of the ten-way valve 1, and finally is discharged from the second carrier gas outlet 16 of the ten-way valve 1, that is, the introduction of the first carrier gas and the second carrier gas blows out the participating gas contained in the first chromatographic column 3, the second chromatographic column 4, the converter 5 and the FID detector 6, so as to avoid the subsequent influence on the detection and analysis of the total carbon content in the circulating hydrogen.
[0028] When the first time valve path of the ten-way valve 1 is reversed, the first carrier gas at this time enters the ten-way valve 1 through the first carrier gas inlet communication port 10 of the ten-way valve 1, then enters the dosing ring 2 from the dosing ring inlet communication port 11 of the ten-way valve 1, and the first carrier gas enters the ten-way valve 1 through the dosing ring outlet communication port 14 of the ten-way valve 1 together with the sample gas in the dosing ring 2, and then is discharged from the first chromatographic column outlet communication port 15 of the ten-way valve 1. At this time, the gas discharged is a mixed gas of the first carrier gas and the sample gas, and the mixed gas enters the first chromatographic column 3. It is worth noting that after the valve path of the ten-way valve 1 is reversed, the functions of the inlet and outlet ports of the first chromatographic column 3 are exchanged, that is, the inlet of the first chromatographic column 3 is the outlet, and the outlet is the inlet. After the mixed gas enters the first chromatographic column 3, the mixed gas is separated by the first chromatographic column 3 to separate the methane, carbon monoxide and carbon dioxide gas from the hydrogen chloride and silane gas in the mixed gas, that is, the methane, carbon monoxide and carbon dioxide are discharged from the first chromatographic column 3 through the first chromatographic column inlet communication port 18 of the ten-way valve 1, and the remaining hydrogen chloride and silane gas stays in the first chromatographic column 3. When the methane, carbon monoxide and carbon dioxide all enter the second chromatographic column 4 connected with the second chromatographic column inlet communication port 19 of the ten-way valve 1, the ten-way valve 1 is reversed again. At this time, the connection state of each port of the ten-way valve 1 returns to the initial state, and the methane, carbon monoxide and carbon dioxide gas discharged from the first chromatographic column 3 enters the converter 5 for conversion, and the converted gas is introduced into the FID detector 6 for detection and total carbon content analysis.
[0029] After the above-mentioned second time valve path reversal, the first chromatographic column 3 at this time retains hydrogen chloride and silane gas, which needs to be discharged in time to avoid the mixed gas of hydrogen chloride and silane gas entering the second chromatographic column 4 for sample gas detection and analysis and affecting the use of the equipment. Specifically, the second carrier gas enters the ten-way valve 1 through the second carrier gas inlet communication port of the ten-way valve 1, and then is discharged from the first chromatographic column inlet communication port 18 of the ten-way valve 1 and enters the first chromatographic column 3. The first carrier gas blows out the mixed gas of hydrogen chloride and silane gas remaining in the first chromatographic column 3, so that the mixed gas is discharged from the first chromatographic column 3 and then discharged through the first chromatographic column outlet communication port 15 and the second carrier gas outlet port 16 of the ten-way valve 1 in sequence, and the hydrogen chloride and silane gas remaining in the first chromatographic column 3 is removed. It is worth noting that after the CO, CH4 and CO2 gas all enter the second chromatographic column 4, the second time valve path reversal is observed and manually performed by the staff to prevent the hydrogen chloride and silane gas from entering the second chromatographic column 4.
[0030] In the embodiment, the first chromatographic column 3 is Porapak Q packed column, which can be used to separate O2, N2, CO, CH4, CO2 and other permanent gases; the second chromatographic column 4 is TDX-01 chromatographic column, which is used for analyzing the separated CO, CH4 and CO2 gases; the converter 5 is a methane converter 5, which is used to convert carbon monoxide (CO) and carbon dioxide (CO2) in the gas sample into methane (CH4) for use in gas chromatography analysis. The methane converter 5 is usually used in gas chromatography, especially when detecting trace amounts of carbon monoxide and carbon dioxide in the gas sample, which are not responsive on the thermal conductivity detector (TCD), but can be detected by converting into methane on the hydrogen flame ionization detector (FID detector 6); the first carrier gas and the second carrier gas are both nitrogen, which is used to transport the sample gas and to purge the first chromatographic column 3, the second chromatographic column 4, the converter 5 and the FID detector.
[0031] In the FID detector 6, the FID detector 6 is also connected with a purge pipeline, the other end of the purge pipeline is a purge gas inlet, and the purge gas is nitrogen, which is used to purge the FID detector 6, blow out the gas remaining in the FID detector 6, and avoid affecting the subsequent use.
[0032] Finally, it should be noted that: the above is only the preferred embodiment of the present application, and is not used to limit the present application, for those skilled in the art, the present application can have various changes and variations, in the case of no conflict, the embodiments of the present application and the features in the embodiments can be combined with each other. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application shall be included in the protection scope of the present application.
Claims
1. A system for detecting the total carbon content in hydrogen gas containing chlorosilane gas, characterized by, It comprises: a ten-way valve, a constant flow ring, a first chromatographic column, a second chromatographic column, a converter and an FID detector; the ten-way valve has ten ports, which are, in turn, a first carrier gas inlet communication port, a constant flow ring inlet communication port, a sample gas inlet, a sample gas outlet, a constant flow ring outlet communication port, a first chromatographic column outlet communication port, a second carrier gas outlet, a second carrier gas inlet communication port, a first chromatographic column inlet communication port and a second chromatographic column inlet communication port in the counterclockwise direction of the ten-way valve; one end of the constant flow ring is communicated with the constant flow ring inlet communication port of the ten-way valve, and the other end is communicated with the sample gas inlet of the ten-way valve; one end of the first chromatographic column is communicated with the first chromatographic column inlet communication port of the ten-way valve, and the other end is communicated with the first chromatographic column outlet communication port of the ten-way valve; one end of the second chromatographic column is communicated with the second chromatographic column inlet communication port; one end of the converter is communicated with the outlet of the second chromatographic column; one end of the FID detector is communicated with the outlet of the converter.
2. The system for detecting total carbon content in hydrogen gas containing chlorosilane gas according to claim 1, characterized by, When the ten-way valve is in the initial state, the first carrier gas inlet communication port is communicated with the second chromatographic column inlet communication port, the constant flow ring inlet communication port is communicated with the sample gas inlet, the sample gas outlet is communicated with the constant flow ring outlet communication port, the first chromatographic column inlet communication port is communicated with the second carrier gas outlet, and the second carrier gas inlet communication port is communicated with the first chromatographic column outlet communication port.
3. The system for detecting total carbon content in hydrogen gas containing chlorosilane gas according to claim 2, characterized by, When the ten-way valve is in the working state, the first carrier gas inlet communication port is communicated with the constant flow ring inlet communication port, the constant flow ring outlet communication port is communicated with the first chromatographic column inlet communication port, the second carrier gas outlet is communicated with the second carrier gas inlet communication port, and the first chromatographic column outlet communication port is communicated with the second chromatographic column inlet communication port.
4. The system for detecting total carbon content in hydrogen gas containing chlorosilane gas according to claim 3, characterized by, The first chromatographic column is a Porapak Q packed column.
5. The system for detecting total carbon content in hydrogen gas containing chlorosilane gas according to claim 4, characterized by, The second chromatographic column is a TDX-01 chromatographic column.
6. The system for detecting total carbon content in hydrogen gas containing chlorosilane gas according to claim 5, wherein The converter is a methane converter.
7. The system for detecting total carbon content in hydrogen gas containing chlorosilane gas according to claim 6, characterized by, The FID detector is connected with a purge pipeline, one end of the purge pipeline is connected with the FID detector inlet, and the other end is a purge gas inlet.
8. The system for detecting total carbon content in hydrogen gas containing chlorosilane gas according to claim 7, characterized by, The first carrier gas, the second carrier gas and the purge gas are all nitrogen.