Titanium sponge distillation gas phase magnesium spectrum absorption detection device and titanium sponge distillation system
By using a spectral absorption detection device to directly measure the concentration of Mg gas phase volatiles in the sponge titanium distillation system, the problem of inaccurate distillation endpoint determination in the prior art is solved, and accurate, real-time determination of the distillation endpoint and energy consumption optimization are achieved.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- NORTHEASTERN UNIV CHINA
- Filing Date
- 2026-06-08
- Publication Date
- 2026-07-21
AI Technical Summary
Existing methods for determining the endpoint of sponge titanium distillation rely on indirect approaches, which are easily affected by differences in equipment condition, charge quantity, and personnel experience, leading to problems such as insufficient distillation or increased energy consumption.
A sponge titanium distillation gas phase magnesium spectral absorption detection device is used. By setting an observation window, light source assembly, optical processing assembly and spectrometer on the connecting pipe, the concentration of Mg gas phase volatiles is directly measured. The light absorption characteristics in the 285.2nm band are used to determine the distillation endpoint, and the effects of observation window contamination and optical path drift are reduced by correcting parameters.
It enables objective, real-time, and accurate determination of the distillation endpoint of sponge titanium, improves distillation efficiency and product quality, reduces energy consumption and the labor intensity of operators, and enhances the level of production automation.
Smart Images
Figure CN224535788U_ABST
Abstract
Description
Technical Field
[0001] This utility model relates to the field of sponge titanium production technology, and in particular to a sponge titanium distillation gas phase magnesium spectral absorption detection device and a sponge titanium distillation system. Background Technology
[0002] Sponge titanium is typically produced using the Krauer process. After the reduction reaction, the product still contains a certain amount of impurities such as magnesium and magnesium chloride. Vacuum distillation under high temperature and low pressure conditions is necessary to purify the sponge titanium by transferring the volatiles, such as magnesium and magnesium chloride, from the distillation vessel through connecting pipes into a condenser. The distillation process is lengthy, and accurately determining the distillation endpoint is crucial for ensuring product quality, reducing energy consumption, and improving production efficiency.
[0003] Existing methods for determining the endpoint of sponge titanium distillation mostly rely on distillation time, temperature changes, vacuum changes, current changes, or operator experience. These methods are typically indirect and easily affected by equipment status, charge quantity, operating condition fluctuations, and differences in operator experience. They can lead to problems such as premature shutdown resulting in insufficient distillation or delayed shutdown leading to increased energy consumption. Therefore, there is an urgent need for a device that can objectively, accurately, and in real-time determine the endpoint of sponge titanium distillation. Utility Model Content
[0004] The present invention introduces a series of simplified concepts, which will be further explained in detail in the detailed description section. This part of the present invention is not intended to limit the key features and essential technical features of the claimed technical solution, nor is it intended to determine the scope of protection of the claimed technical solution.
[0005] An embodiment of this utility model provides a gas-phase magnesium spectral absorption detection device for sponge titanium distillation, used in a sponge titanium distillation system. The device includes: observation windows; the sponge titanium distillation system includes a distillation container, a condenser container, and a connecting pipe connecting the distillation container and the condenser container; paired observation windows are arranged perpendicular to the flow direction of the connecting pipe and are respectively disposed on the pipe walls on opposite sides of the connecting pipe; and a light source assembly disposed outside the connecting pipe for emitting detection light, the detection light including a first detection light and a second detection light, the first detection light at least covering a first preset wavelength band. The second detection light does not cover the first preset wavelength band, which is 285.2nm. An optical processing component is located on one side of the connecting pipe, opposite to the observation window, and connected to the light source component. The detection light is transmitted into the connecting pipe through the optical processing component and the observation window. An optical receiving component is located on the other side of the connecting pipe, opposite to the observation window, and is used to receive the detection light passing through the connecting pipe and the observation window. A spectrometer is located outside the connecting pipe and connected to the optical receiving component. A processing module is connected to the spectrometer signal and is configured to determine the distillation endpoint based on the analysis information from the spectrometer.
[0006] For example, the light source assembly includes: a first light source for emitting a first detection light; a second light source for emitting a second detection light; and an optical path combining unit located on the outgoing optical path of the first light source and the second light source, the optical path combining unit being configured to combine the first detection light and the second detection light into a coaxial beam before entering the optical processing assembly.
[0007] For example, the first light source is one of a magnesium hollow cathode lamp, an LED lamp, or a deuterium lamp with a wavelength selector; the second light source includes one of an LED lamp or a deuterium lamp with a wavelength selector.
[0008] For example, the optical processing assembly includes: a emitting mask, an emitting optical fiber, and a collimating lens located inside the emitting mask. The first end of the emitting mask is connected to a connecting pipe and covers the outside of the observation window. The second end of the emitting mask is provided with a first optical fiber interface. The emitting optical fiber is installed at the first optical fiber interface and connected to the light source assembly.
[0009] For example, the optical processing assembly also includes an aperture stop located within the emitting diaphragm, the aperture stop being arranged between the collimating lens and the viewing window.
[0010] For example, the optical receiving assembly includes: a receiving mask, a receiving optical fiber, and a receiving lens located inside the receiving mask. The first end of the receiving mask is connected to a connecting pipe and covers the outside of the observation window. The second end of the receiving mask is provided with a second optical fiber interface. The receiving optical fiber is installed at the second optical fiber interface and connected to the spectrometer.
[0011] For example, the observation window is made of fused silica or sapphire and is sealed to the wall of the connecting pipe.
[0012] For example, the sponge titanium distillation gas phase magnesium spectral absorption detection device further includes: a mounting base, an observation window mounted on the mounting base, and the mounting base being sealed to a connecting pipe; a sealing element disposed between the mounting base and the observation window; and a heat insulation element and / or a heating element, wherein the heat insulation element is located outside the connecting pipe and surrounds the outer wall of the mounting base, and the heating element is disposed outside the connecting pipe and configured to heat the mounting base.
[0013] For example, the observation window includes a first observation window and a second observation window. The first observation window and the optical processing component are located on the same side of the connecting pipe, and the second observation window and the optical receiving component are located on the same side of the connecting pipe. The optical processing component, the first observation window, the second observation window and the optical receiving component are located on the same detection optical axis, which passes through the connecting pipe and intersects the migration direction of the volatiles in the connecting pipe.
[0014] An embodiment of this utility model also provides a sponge titanium distillation system, including: the sponge titanium distillation gas phase magnesium spectral absorption detection device of any of the preceding claims.
[0015] The sponge titanium distillation vapor phase magnesium spectral absorption detection device and sponge titanium distillation system provided in this embodiment can directly measure the concentration of Mg vapor phase volatiles in the connecting pipe, transforming the judgment of the distillation endpoint from subjective experience into objective data, which is accurate and reliable. It realizes automatic and real-time judgment of the distillation endpoint of the sponge titanium distillation system, and can reduce the influence of observation window contamination, particle scattering, and MgCl2-related condensation deposition on the judgment of the distillation endpoint, thereby improving the accuracy, timeliness, and objectivity of the distillation endpoint judgment. This is beneficial to improving product quality, increasing distillation efficiency, reducing energy consumption, and reducing the labor intensity of operators, thus improving the automation level of sponge titanium production.
[0016] The above description is merely an overview of the technical solution of this utility model. In order to better understand the technical means of this utility model and to implement it in accordance with the contents of the specification, and to make the above and other objects, features and advantages of this utility model more obvious and understandable, specific embodiments of this utility model are given below. Attached Figure Description
[0017] Various other advantages and benefits will become apparent to those skilled in the art upon reading the following detailed description of preferred embodiments. The accompanying drawings are for illustrative purposes only and are not intended to limit the scope of the invention. Furthermore, the same reference numerals denote the same parts throughout the drawings. Wherein: Figure 1One of the structural schematic diagrams of the sponge titanium distillation system provided in the embodiment of this utility model is shown; Figure 2 This illustration shows one of the partial structural schematic diagrams of the sponge titanium distillation gas phase magnesium spectral absorption detection device provided in an embodiment of the present invention; Figure 3 This is one of the cross-sectional views of a partial structure of the sponge titanium distillation gas phase magnesium spectral absorption detection device provided in an embodiment of the present invention.
[0018] in, Figures 1 to 3 The correspondence between the reference numerals and component names in the attached drawings is as follows: 100. Sponge titanium distillation gas phase magnesium spectral absorption detection device; 110. Observation window; 111. First observation window; 112. Second observation window; 120. Light source assembly; 121. First light source; 122. Second light source; 123. Optical path beam combining unit; 130. Optical processing assembly; 131. Emitting photomask; 132. Emitting optical fiber; 133. Collimating lens; 134. Aperture; 140. Optical receiving assembly; 141. Receiving photomask; 142. Receiving optical fiber; 143. Receiving lens; 150. Spectrometer; 160. Processing module; 170. First mounting base; 180. Second mounting base; 200. Sponge titanium distillation system; 210. Distillation container; 220. Condensation container; 230. Connecting pipe; 240. Vacuum pump. Detailed Implementation
[0019] The following description provides numerous specific details to offer a more thorough understanding of the technical solutions provided by this invention. However, it will be apparent to those skilled in the art that the technical solutions provided by this invention can be implemented without one or more of these details.
[0020] It should be noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the exemplary embodiments according to the present invention. As used herein, the singular form is intended to include the plural form as well, unless the context clearly indicates otherwise. Furthermore, it should be understood that when the terms “comprising” and / or “including” are used in this specification, they indicate the presence of features, integrals, steps, operations, elements, and / or components, but do not exclude the presence or addition of one or more other features, integrals, steps, operations, elements, components, and / or combinations thereof.
[0021] Exemplary embodiments according to the present invention will now be described in more detail with reference to the accompanying drawings. However, these exemplary embodiments may be implemented in many different forms and should not be construed as being limited to the embodiments set forth herein. It should be understood that these embodiments are provided so that the disclosure of the present invention is thorough and complete, and that the concept of these exemplary embodiments is fully conveyed to those skilled in the art.
[0022] like Figures 1 to 3 As shown in the embodiment of this utility model, a sponge titanium distillation gas phase magnesium spectral absorption detection device 100 and a sponge titanium distillation system 200 are provided. The sponge titanium distillation gas phase magnesium spectral absorption detection device 100 is applied to the sponge titanium distillation system 200 to determine when the sponge titanium distillation system 200 has completed distillation and reached the distillation endpoint.
[0023] like Figure 1 and Figure 2 As shown, an embodiment of the first aspect of this utility model provides a sponge titanium distillation gas-phase magnesium spectral absorption detection device 100 for use in a sponge titanium distillation system 200. The sponge titanium distillation gas-phase magnesium spectral absorption detection device 100 includes: an observation window 110; the sponge titanium distillation system 200 includes a distillation container 210, a condenser container 220, and a connecting pipe 230 connecting the distillation container 210 and the condenser container 220; pairs of observation windows 110 are arranged in a direction perpendicular to the flow direction of the connecting pipe 230 and are respectively disposed on the pipe walls on opposite sides of the connecting pipe 230; a light source assembly 120 is disposed outside the connecting pipe 230 for emitting detection light, the detection light including a first detection light and a second detection light, the first detection light at least covering a first preset wavelength band, and the second detection light... The photometric measurement does not cover the first preset wavelength band, which is 285.2nm. An optical processing component 130 is located on one side of the connecting pipe 230, opposite the observation window 110, and connected to the light source component 120. The detection light is transmitted through the optical processing component 130 and the observation window 110 into the connecting pipe 230. An optical receiving component 140 is located on the other side of the connecting pipe 230, opposite the observation window 110, and is used to receive the detection light passing through the connecting pipe 230 and the observation window 110. A spectrometer 150 is located outside the connecting pipe 230 and connected to the optical receiving component 140. A processing module 160 is connected to the spectrometer 150 and configured to determine the distillation endpoint based on the analytical information from the spectrometer 150.
[0024] like Figure 1As shown, the sponge titanium distillation system 200 includes a distillation container 210, a condenser container 220, and a connecting pipe 230 connecting the distillation container 210 and the condenser container 220. During distillation, high-temperature volatile gases such as magnesium and magnesium chloride flow from the distillation container 210 into the condenser container 220 via the connecting pipe 230. Specifically, the distillation container 210 is used to contain the reduced sponge titanium material, and the condenser container 220 is used to receive and condense the magnesium, magnesium chloride, and related volatiles volatilized from the distillation container 210; the connecting pipe 230 connects the distillation container 210 and the condenser container 220 to form a volatile migration channel.
[0025] The sponge titanium distillation gas phase magnesium spectral absorption detection device 100 is installed in the connecting pipe 230. Specifically, the sponge titanium distillation gas phase magnesium spectral absorption detection device 100 can be located on the connecting pipe 230 between the distillation vessel 210 and the condensation vessel 220. For example, if the connecting pipe 230 includes a detection section in the middle, the sponge titanium distillation gas phase magnesium spectral absorption detection device 100 is installed in the detection section of the connecting pipe 230. In this way, the sponge titanium distillation gas phase magnesium spectral absorption detection device 100 can be used to perform online detection during the migration of volatiles from the distillation vessel 210 to the condensation vessel 220, so that the detection result can reflect the change in the concentration of gas phase volatiles in the connecting pipe 230, thereby realizing the determination of the distillation endpoint.
[0026] The sponge titanium distillation gas-phase magnesium spectral absorption detection device 100 provided in this embodiment includes an observation window 110, a light source assembly 120, an optical processing assembly 130, an optical receiving assembly 140, a spectrometer 150, and a processing module 160. The observation windows 110 are arranged in pairs, i.e., there are two observation windows 110. The two observation windows 110 are arranged in a direction perpendicular to the flow direction of the connecting pipe 230, and the two observation windows 110 are respectively disposed on the pipe walls on opposite sides of the connecting pipe 230, i.e., the line connecting the two observation windows 110 is perpendicular to the flow direction of the connecting pipe 230. The optical processing assembly 130 and the optical receiving assembly 140 are respectively disposed on opposite sides of the connecting pipe 230, and are respectively disposed opposite to the observation window 110 on their respective sides. The optical processing component 130 is connected to the light source component 120, and the optical receiving component 140 is connected to the spectrometer 150. In this way, the detection light emitted by the light source component 120 can be processed by the optical processing component 130 and transmitted through the observation window 110 into the connecting pipe 230. The optical receiving component 140 can receive the detection light passing through the connecting pipe 230 and the observation window 110 and couple it to the spectrometer 150. The spectrometer 150 analyzes the detection light, and the processing module 160 can determine whether the distillation has reached the endpoint based on the analysis information from the spectrometer 150.
[0027] Furthermore, the light source assembly 120 can emit a first detection light and a second detection light. The first detection light covers at least a first preset wavelength band, that is, the first detection light can cover the 285.2nm wavelength band and other wavelength bands near 285.2nm. The second detection light does not cover the first preset wavelength band, that is, the second detection light does not cover 285.2nm. Since Mg gaseous volatiles have the strongest light absorption effect in the 285.2nm ultraviolet band, the detection light emitted by the light source assembly 120 includes the first detection light covering the 285.2nm wavelength band. The first detection light serves as the main detection wavelength band. By using the processing module 160 to extract the characteristic absorption signal of the 285.2nm wavelength band based on the analysis information of the spectrometer 150, the concentration of Mg gaseous volatiles in the connecting pipe 230 can be determined. Since MgCl2-related condensation deposition, particle scattering, contamination of the observation window 110, light source attenuation, and optical path drift also affect light transmittance, the detection light emitted by the light source assembly 120 includes a second detection light that does not cover 285.2nm. The second detection light serves as a non-characteristic reference band. By using the processing module 160 to extract the characteristic absorption signal of the second detection light band based on the analysis information from the spectrometer 150, the influence of MgCl2-related condensation deposition, particle scattering, contamination of the observation window 110, light source attenuation, and optical path drift on light transmittance within the connecting pipe 230 can be determined. Based on this, correction parameters can be determined. Thus, the processing module 160 can correct the extracted characteristic absorption signal of the 285.2nm band based on the correction parameters determined by the characteristic absorption signal of the second detection light band, and determine whether the distillation has reached its endpoint based on the correction result. Therefore, the sponge titanium distillation gas phase magnesium spectral absorption detection device 100 can directly measure the concentration of Mg gas phase volatiles and reduce the influence of contamination, particle scattering, and MgCl2-related condensation deposition on the distillation endpoint determination of the observation window 110, which is beneficial to improving the accuracy of distillation endpoint determination.
[0028] Specifically, before distillation begins, the first and second detection lights emitted by the light source assembly 120 are transmitted through the optical processing assembly 130 and an observation window 110 to the connecting pipe 230. The optical receiving assembly 140 receives the detection light transmitted through the connecting pipe 230 and another observation window 110 and couples it to the spectrometer 150. Since distillation is not currently underway, i.e., no Mg or MgCl2-related volatiles enter the connecting pipe 230, the processing module 160 acquires a baseline signal through the spectrometer 150. The baseline signal can be the transmission spectrum signal when no volatiles are generated, or it can be a reference signal at the initial stage of distillation. Specifically, the baseline signal can include the band baseline signal of the first detection light (e.g., the 285.2nm band baseline signal) and the band baseline signal of the second detection light. The 285.2nm band baseline signal is used to represent the characteristic absorption intensity of Mg, and the baseline signal of the second detection light is used to characterize the combined light intensity attenuation caused by contamination of the observation window 110, particle scattering, MgCl2-related condensation deposition, light source attenuation, and optical path drift.
[0029] During distillation, Mg and MgCl2-related volatiles in the distillation vessel 210 enter the connecting pipe 230. Mg vapor volatiles cause characteristic absorption changes in the transmitted light intensity at 285.2 nm. MgCl2-related condensation and deposition, particle scattering, contamination of the observation window 110, light source attenuation, and optical path drift all contribute to the attenuation of the transmittance in the 285.2 nm band and the second detection light not covering 285.2 nm. The spectrometer 150 continuously acquires the real-time transmitted spectral signal, and the processing module 160 extracts the characteristic absorption signal at 285.2 nm and simultaneously extracts the absorption signal in the second detection light band.
[0030] As the distillation process proceeds, the volatile Mg and MgCl2-related volatiles in the distillation vessel 210 gradually decrease, and the concentration of Mg gaseous volatiles in the connecting pipe 230 decreases, resulting in a weakening of the characteristic absorption signal in the 285.2nm band. The processing module 160 determines correction parameters by comparing the absorption signal of the second detection light band with the baseline signal of the second detection light band. These correction parameters reflect the effects of contamination of the observation window 110, particle scattering, MgCl2-related condensation and deposition, light source attenuation, and optical path drift on the band absorption signal. Then, based on these correction parameters, the characteristic absorption signal of 285.2nm collected by the processing module 160 is corrected. Comparing the corrected 285.2nm band absorption intensity with the 285.2nm band baseline signal allows for determination of whether the distillation has reached its endpoint. Specifically, after determining that the distillation has reached its endpoint, the processing module 160 can output a distillation endpoint prompt signal, such as by using an alarm device, to facilitate intuitive and accurate determination of the distillation endpoint by the operator.
[0031] Therefore, this embodiment transforms the determination of the distillation endpoint from subjective experience into objective data, ensuring accuracy and reliability. It achieves automatic and real-time determination of the distillation endpoint in the sponge titanium distillation system 200. Compared to related technologies that rely on manual determination of the distillation endpoint, this method is more objective and allows for real-time determination, improving the accuracy, timeliness, and objectivity of endpoint determination. This benefits product quality, distillation efficiency, and energy consumption, while also reducing the workload of operators and enhancing the automation level of sponge titanium production. Furthermore, the sponge titanium distillation gas-phase magnesium spectral absorption detection device 100 provided in this embodiment can directly measure the concentration of Mg gas-phase volatiles. The detection object is closer to the change in volatile concentration itself during distillation, which improves detection accuracy. It also reduces the impact of contamination of the observation window 110, particle scattering, MgCl2-related condensation deposition, light source attenuation, and optical path drift on detection accuracy, further enhancing the accuracy of distillation endpoint determination.
[0032] Furthermore, the wavelength of the first detection light can be from 280nm to 290nm, etc. The wavelength of the second detection light can avoid 285.2nm and other characteristic absorption bands of volatiles. For example, the wavelength of the second detection light can be from 325nm to 328nm, 340nm to 345nm, 665nm to 675nm, or other bands.
[0033] like Figure 1 As shown, in some possible embodiments provided by this utility model, the light source assembly 120 includes: a first light source 121 for emitting a first detection light; a second light source 122 for emitting a second detection light; and an optical path combining unit 123 located on the outgoing optical path of the first light source 121 and the second light source 122. The optical path combining unit 123 is configured to combine the first detection light and the second detection light into a coaxial beam before entering the optical processing assembly 130.
[0034] In this embodiment, the light source assembly 120 adopts a dual-channel light source assembly. The dual-channel light source assembly includes a first light source 121 for outputting a first detection light, a second light source 122 for outputting a second detection light, and an optical path combining unit 123. The first and second detection lights are combined into a coaxial beam by the optical path combining unit 123 and then enter the optical processing assembly 130. This facilitates the subsequent unified processing of the first and second detection lights by the optical processing assembly 130, ensuring that they pass through the interior of the connecting pipe 230 more vertically and centrally, thereby reducing light energy loss, lowering detection errors, and improving detection accuracy. At the same time, this arrangement simplifies the optical path structure, makes the layout of the light source assembly 120 compact, and helps to reduce the space occupied by the light source assembly 120.
[0035] In some possible embodiments provided by this utility model, the first light source 121 includes one of a magnesium hollow cathode lamp, an LED lamp, and a deuterium lamp with a wavelength selector.
[0036] Specifically, the magnesium hollow cathode lamp is used to emit the characteristic spectral lines of magnesium (dominant wavelength 285.2 nm); the LED lamp can be a deep ultraviolet LED lamp with a wavelength range of 280 nm to 290 nm; the deuterium lamp with a wavelength selector can use the wavelength selector to make its emitted light cover the 285.2 nm wavelength range, such as the 280 nm to 290 nm band. Specifically, the wavelength selector can be a narrowband filter, a bandpass filter, or a monochromator.
[0037] The second light source 122 includes one of an LED lamp or a deuterium lamp with a wavelength selector. Specifically, the wavelength of the second detection light can be 325nm to 328nm, 340nm to 345nm, 665nm to 675nm, or other wavelengths. The second light source 122 can be a deuterium lamp with a wavelength selector, such as the output light source of a deuterium lamp after wavelength selection by a bandpass filter or monochromator, or the second light source 122 can be an LED lamp, such as an LED light source with a peak wavelength located near 326.5nm, 342.5nm, or 670nm. The second detection light output by the second light source 122 can be a wavelength light with stable transmittance that avoids the characteristic absorption or emission regions of Mg, MgCl2, and other volatiles, such as the second detection light not covering the 285.2nm wavelength band.
[0038] The second detection light may not cover the 285.2nm band; that is, the second detection light should avoid the stable reference band characteristic of Mg, MgCl2, and other volatile compounds. The second detection light can reflect changes in the overall transmittance, deposition, scattering, and optical path drift of the beam, and is used to correct the effects of contamination, scattering, and intensity drift on the transmittance of the first detection light. It can be selected based on the response of the light source, window, optical fiber, and spectrometer 150. The second detection light can also serve as a non-characteristic reference band for reference compensation and stability assessment.
[0039] Specifically, the second detection light can be a stable non-characteristic sub-band in the visible or near-infrared light, that is, the second detection light can be a visible or near-infrared band that does not cover the 285.2nm band.
[0040] Furthermore, the spectrometer 150 is connected to the processing module 160 via signal, and the processing module 160 performs characteristic band extraction, reference band correction, and distillation endpoint determination on the spectral data or light intensity data.
[0041] like Figure 2 and Figure 3As shown, in some possible embodiments provided by this utility model, the observation window 110 includes a first observation window 111 and a second observation window 112. The first observation window 111 and the optical processing component 130 are located on the same side of the connecting pipe 230, and the second observation window 112 and the optical receiving component 140 are located on the same side of the connecting pipe 230. The optical processing component 130, the first observation window 111, the second observation window 112, and the optical receiving component 140 are located on the same detection optical axis, which passes through the connecting pipe 230 and intersects the migration direction of the volatiles within the connecting pipe 230. This allows the detection light to pass through the connecting pipe 230 in a transmission manner, enabling spectral absorption detection of volatiles such as magnesium and magnesium chloride flowing through the connecting pipe 230, thereby determining the distillation endpoint.
[0042] Specifically, such as Figures 1 to 3 As shown, the dotted line in the figure can be interpreted as the detection optical axis shared by the optical processing component 130, the first observation window 111, the second observation window 112, and the optical receiving component 140. The first observation window 111 and the optical processing component 130 are located above the connecting pipe 230, and the second observation window 112 and the optical receiving component 140 are located below the connecting pipe 230.
[0043] like Figure 3 As shown, in some possible embodiments provided by this utility model, the optical processing component 130 includes: a photomask 131, a photofiber 132, and a collimating lens 133 located inside the photomask 131. The first end of the photomask 131 is connected to the connecting pipe 230 and covers the outside of the observation window 110. The second end of the photomask 131 is provided with a first fiber optic interface. The photofiber 132 is installed at the first fiber optic interface and connected to the light source component 120.
[0044] This embodiment provides the specific structure of the optical processing component 130. The emitting photomask 131 is connected to the connecting pipe 230. The emitting photomask 131 can limit the divergence range of the detection light, suppress stray light and diffuse reflection light, allowing the detection light to pass smoothly through the first observation window 111 and be transmitted into the connecting pipe 230. The emitting optical fiber 132 can efficiently conduct and directionally deliver the detection light into the emitting photomask 131, with low light loss, stable transmission, and flexible optical path layout. The collimating lens 133 can shape the divergent detection light into a parallel beam, keeping the beam coaxial and stable during transmission, which is beneficial for improving the utilization rate and detection accuracy of the detection light.
[0045] like Figure 3 As shown, in some possible embodiments provided by this utility model, the optical processing component 130 further includes an aperture 134 located within the emitting photomask 131, the aperture 134 being arranged between the collimating lens 133 and the observation window 110.
[0046] Among them, the aperture 134 is used to limit the aperture of the detection beam, cut off stray light and scattered light at the edge, constrain the effective field of view of the optical path, regulate the beam transmission aperture, suppress scattering and background stray light interference, and improve the coaxial consistency of the detection optical path and the signal-to-noise ratio of the spectral signal.
[0047] like Figure 2 and Figure 3 As shown, in some possible embodiments provided by this utility model, the optical receiving assembly 140 includes: a receiving mask 141, a receiving optical fiber 142, and a receiving lens 143 located inside the receiving mask 141. The first end of the receiving mask 141 is connected to the connecting pipe 230 and covers the outside of the observation window 110. The second end of the receiving mask 141 is provided with a second optical fiber interface. The receiving optical fiber 142 is installed at the second optical fiber interface and connected to the spectrometer 150.
[0048] This embodiment provides a specific structure for the optical receiving assembly 140. The receiving mask 141 is connected to the connecting pipe 230. The receiving mask 141 can directionally receive the transmitted light beam through the connecting pipe 230 and the second observation window 112, limiting the receiving field of view and shielding lateral stray light. The receiving optical fiber 142 can stably transmit the detection light transmitted through the second observation window 112, stabilizing the light receiving aperture and directionally delivering it to the spectrometer 150. It features low light loss, stable transmission, and flexible optical path layout. The receiving lens 143 can converge and shape the detection light projected through the second observation window 112 and couple it into the receiving optical fiber 142, regulating the beam transmission angle and coaxiality, suppressing large-angle scattered stray light, and improving light energy utilization and detection stability.
[0049] In some embodiments, during assembly, the optical processing component 130 and the optical receiving component 140 can be fixed to the outside of the connecting pipe 230 via adjustable mounting bases. That is, the emitting photomask 131 and the receiving photomask 141 can be adjusted and fixed to the connecting pipe 230, such that the outgoing optical axis of the optical processing component 130, the geometric center of the two observation windows 110, and the receiving optical axis of the optical receiving component 140 are substantially coincident. The adjustable mounting base can be used to adjust the position and angle of the emitting and receiving optical axes, allowing the detection light to pass through the gas phase region of the connecting pipe 230 relatively vertically and concentratedly, thus penetrating to the volatiles such as magnesium and magnesium chloride flowing through the connecting pipe 230. Therefore, online spectral detection of changes in volatile concentration during distillation can be achieved without damaging the original distillation vessel 210, condenser 220, and the main structure of the connecting pipe 230.
[0050] In some possible embodiments provided by this utility model, the observation window 110 is made of fused silica or sapphire, and the observation window 110 is sealed and installed on the pipe wall of the connecting pipe 230.
[0051] In this embodiment, since the 285.2nm band belongs to the ultraviolet band, ordinary glass has low transmittance in this band. Therefore, setting the observation window 110 to be made of fused silica or sapphire ensures that the detection light in the 285.2nm band has high transmittance, which is beneficial to improving detection accuracy and thus improving the accuracy of determining the distillation endpoint. Specifically, the observation window 110 is made of ultraviolet-grade fused silica that has transmittance to ultraviolet detection light near 285.2nm, or it is made of synthetic sapphire that has transmittance to ultraviolet detection light near 285.2nm.
[0052] The observation window 110 can be sealed and embedded in the wall of the connecting pipe 230, which can ensure the vacuum and pressure sealing of the connecting pipe 230.
[0053] In some possible embodiments provided by this utility model, the sponge titanium distillation gas phase magnesium spectral absorption detection device 100 further includes: a mounting base, an observation window 110 mounted on the mounting base, and the mounting base being sealed to the connecting pipe 230. That is, the observation window 110 is sealed to the connecting pipe 230 via the mounting base. Specifically, the connecting pipe 230 has a window in its wall, the mounting base is connected to the window of the connecting pipe 230, and the observation window 110 is fixed inside the mounting base by a clamping flange.
[0054] Furthermore, such as Figure 1 and Figure 3 As shown, the mounting base includes a first mounting base 170 and a second mounting base 180. A first observation window 111 is sealed and mounted to the connecting pipe 230 via the first mounting base 170, and a second observation window 112 is sealed and mounted to the connecting pipe 230 via the second mounting base 180. Specifically, the first mounting base 170 supports the optical processing component 130; that is, the first observation window 111 and the optical processing component 130 can be simultaneously mounted on the connecting pipe 230 via the first mounting base 170. Similarly, the second observation window 112 and the optical receiving component 140 can be simultaneously mounted on the connecting pipe 230 via the second mounting base 180. This simplifies the installation structure, reduces manufacturing costs, and meets the design requirements of the sponge titanium distillation gas-phase magnesium spectral absorption detection device 100 for its compact structure and small size.
[0055] Furthermore, the sponge titanium distillation gas phase magnesium spectral absorption detection device 100 also includes a sealing element located between the mounting base and the observation window 110 to seal the gap between the mounting base and the observation window 110, thereby meeting the vacuum sealing requirements under high temperature and low pressure distillation conditions.
[0056] Furthermore, a seal can be installed between the mounting base and the window of the connecting pipe 230 to seal the gap between the mounting base and the window, so as to meet the vacuum sealing requirements under high temperature and low pressure distillation environment.
[0057] Specifically, the sealing element can be a sealing ring, a sealing gasket, etc.
[0058] In some embodiments provided by this utility model, the sponge titanium distillation gas phase magnesium spectral absorption detection device 100 further includes a heat insulation component and / or a heating component. The heat insulation component is located outside the connecting pipe 230 and surrounds the outer wall of the mounting base. The heat insulation component can reduce the possibility of heat in the connecting pipe 230 being transferred to the outside of the connecting pipe 230 through the mounting base, thereby reducing heat loss in the observation window 110 area. This is beneficial to reducing the deposition of Mg, MgCl2-related condensates or particles on the surface of the observation window 110 and improving detection accuracy.
[0059] The heating element is located outside the connecting pipe 230 and is configured to heat the mounting base. The heating element is used to increase the temperature of the mounting base, thereby increasing the temperature near the observation window 110. This helps to reduce the deposition of Mg, MgCl2-related condensates or particles on the surface of the observation window 110 and improves the detection accuracy.
[0060] It is understood that the sponge titanium distillation gas phase magnesium spectral absorption detection device 100 may include a heat insulation element or a heating element, or may include both a heat insulation element and a heating element.
[0061] Specifically, the insulation component can be an insulation coating, which at least covers the first mounting base located outside the connecting pipe 230. The heating component can be a heating element or a heating rod, etc.
[0062] An embodiment of this utility model also provides a sponge titanium distillation system 200, including: the sponge titanium distillation gas-phase magnesium spectral absorption detection device 100 of any of the foregoing embodiments. Since the sponge titanium distillation system 200 includes the aforementioned sponge titanium distillation gas-phase magnesium spectral absorption detection device 100, it has all the technical effects of the aforementioned sponge titanium distillation gas-phase magnesium spectral absorption detection device 100, which will not be described in detail here.
[0063] Furthermore, the sponge titanium distillation system 200 also includes a vacuum pump 240, which can be located on the side of the condenser 220 away from the distillation vessel 210 and connected to the condenser 220 or the connecting pipe 230 through a vacuum line to maintain the vacuum environment required inside the distillation production system.
[0064] Compared with the prior art, the embodiments of this utility model have at least the following beneficial effects: First, in this embodiment, the Mg gas phase volatiles in the connecting pipe 230 are detected by transmission spectral absorption in the 285.2nm band. The detection object is closer to the change in volatile concentration itself during the distillation process, which is beneficial to improving the detection accuracy.
[0065] Secondly, the light source assembly 120, the optical processing assembly 130, the observation window 110, the internal area of the connecting pipe 230, the optical receiving assembly 140 and the spectrometer 150 are used to form a transmission detection optical path. The detection optical path does not require the probe to extend into the connecting pipe 230, which helps to maintain the vacuum seal of the system and reduce the risk of contamination.
[0066] Third, the light source assembly 120 emits a first detection light covering the 285.2nm wavelength band through the first light source 121 and a second detection light not covering the 285.2nm wavelength band through the second light source 122. The detection light is formed by the optical path beam combining unit and transmitted to the connecting pipe 230. In this way, the processing module 160 corrects the received 285.2nm characteristic absorption signal according to the characteristic signal of the second detection light received by the spectrometer 150. The corrected 285.2nm characteristic absorption signal is used to determine whether the distillation has reached the end point. This can reduce the common light intensity attenuation caused by contamination of the observation window 110, particle scattering, MgCl2 related condensation deposition, light source attenuation and optical path drift, which is conducive to improving the detection accuracy and thus improving the accuracy of the distillation end point determination.
[0067] Fourth, the observation window 110 adopts an ultraviolet-grade fused silica window or a synthetic sapphire window, and is equipped with heating elements and / or heat preservation elements, which helps to improve the long-term stability of the detection light under high temperature and low pressure distillation environment.
[0068] Fifth, it can provide spectral absorption data for monitoring the concentration changes of Mg gas phase volatiles and determining the distillation endpoint during the vacuum distillation of sponge titanium.
[0069] It should be noted that, in this document, the terms "comprising," "including," or any other variations thereof are intended to cover non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements includes not only those elements but also other elements not expressly listed, or elements inherent to such a process, method, article, or apparatus. Without further limitations, an element defined by the phrase "comprising one..." does not exclude the presence of other identical elements in the process, method, article, or apparatus that includes that element. Furthermore, it should be noted that the scope of the methods and apparatuses in the embodiments of this utility model is not limited to performing functions in the order shown or discussed, but may also include performing functions substantially simultaneously or in the reverse order, depending on the functions involved. For example, the described methods may be performed in a different order than described, and various steps may be added, omitted, or combined. Additionally, features described with reference to certain examples may be combined in other examples.
[0070] The embodiments of the present invention have been described above with reference to the accompanying drawings. However, the present invention is not limited to the specific embodiments described above. The specific embodiments described above are merely illustrative and not restrictive. Those skilled in the art can make many other forms under the guidance of the present invention without departing from the spirit and scope of the present invention, and all of these forms are within the protection scope of the present invention.
Claims
1. A sponge titanium distillation gas-phase magnesium spectral absorption detection device, characterized in that, For use in a sponge titanium distillation system, the sponge titanium distillation gas-phase magnesium spectral absorption detection device includes: The observation window of the sponge titanium distillation system includes a distillation container, a condenser container, and a connecting pipe connecting the distillation container and the condenser container. The pair of observation windows are arranged in a direction perpendicular to the flow direction of the connecting pipe and are respectively set on the pipe wall on opposite sides of the connecting pipe. A light source assembly is disposed outside the connecting pipe for emitting detection light. The detection light includes a first detection light and a second detection light. The first detection light covers at least a first preset wavelength band, and the second detection light does not cover the first preset wavelength band. The first preset wavelength band is 285.2 nm. An optical processing component is disposed on one side of the connecting pipe, opposite to the observation window, and connected to the light source component. The detection light is transmitted into the connecting pipe through the optical processing component and the observation window. An optical receiving component is disposed on the other side of the connecting pipe, opposite to the observation window, and is used to receive the detection light passing through the connecting pipe and the observation window; A spectrometer is disposed outside the connecting pipe and connected to the optical receiving assembly; A processing module, which is connected to the spectrometer signal, is configured to determine the distillation endpoint based on the analytical information from the spectrometer.
2. The sponge titanium distillation gas-phase magnesium spectral absorption detection device according to claim 1, characterized in that, The light source assembly includes: A first light source is used to emit the first detection light; The second light source is used to emit the second detection light; An optical path combining unit is located on the outgoing optical path of the first light source and the second light source. The optical path combining unit is configured to combine the first detection light and the second detection light into a coaxial beam before entering the optical processing component.
3. The sponge titanium distillation gas-phase magnesium spectral absorption detection device according to claim 2, characterized in that, The first light source includes one of a magnesium hollow cathode lamp, an LED lamp, and a deuterium lamp with a wavelength selector; The second light source includes one of an LED lamp and a deuterium lamp with a wavelength selector.
4. The sponge titanium distillation gas-phase magnesium spectral absorption detection device according to claim 1, characterized in that, The optical processing component includes: The light emitter includes a light emitter cover, a light emitter fiber, and a collimating lens located inside the light emitter cover. The first end of the light emitter cover is connected to the connecting pipe and covers the outside of the observation window. The second end of the light emitter cover is provided with a first fiber optic interface. The light emitter fiber is installed at the first fiber optic interface and connected to the light source assembly.
5. The sponge titanium distillation gas-phase magnesium spectral absorption detection device according to claim 4, characterized in that, The optical processing component further includes: An aperture stop is located within the emitting photomask, and the aperture stop is arranged between the collimating lens and the observation window.
6. The sponge titanium distillation gas-phase magnesium spectral absorption detection device according to claim 1, characterized in that, The optical receiving component includes: The instrument comprises a receiving photomask, a receiving optical fiber, and a receiving lens located inside the receiving photomask. The first end of the receiving photomask is connected to the connecting pipe and covers the outside of the observation window. The second end of the receiving photomask is provided with a second optical fiber interface. The receiving optical fiber is installed at the second optical fiber interface and connected to the spectrometer.
7. The sponge titanium distillation gas-phase magnesium spectral absorption detection device according to any one of claims 1 to 6, characterized in that, The observation window is made of fused silica or sapphire and is sealed to the wall of the connecting pipe.
8. The sponge titanium distillation gas-phase magnesium spectral absorption detection device according to any one of claims 1 to 6, characterized in that, Also includes: Mounting base, the observation window is mounted on the mounting base, and the mounting base is sealed to the connecting pipe; A sealing element is disposed between the mounting base and the observation window; Insulation and / or heating elements, wherein the insulation element is located outside the connecting pipe and surrounds the outer wall of the mounting base, and the heating element is disposed outside the connecting pipe and configured to heat the mounting base.
9. The sponge titanium distillation gas-phase magnesium spectral absorption detection device according to any one of claims 1 to 6, characterized in that, The observation window includes a first observation window and a second observation window. The first observation window and the optical processing component are located on the same side of the connecting pipe, and the second observation window and the optical receiving component are located on the same side of the connecting pipe. The optical processing component, the first observation window, the second observation window, and the optical receiving component are located on the same detection optical axis, which passes through the connecting pipe and intersects the migration direction of the volatiles in the connecting pipe.
10. A sponge titanium distillation system, characterized in that, include: The sponge titanium distillation gas phase magnesium spectral absorption detection device as described in any one of claims 1 to 9.