WO2019044917A1 - Dispositif d'analyse de concentration de chlore, procédé d'analyse de concentration de chlore, dispositif de production de tétrachlorure de titane et procédé de production d'éponge de titane - Google Patents

Dispositif d'analyse de concentration de chlore, procédé d'analyse de concentration de chlore, dispositif de production de tétrachlorure de titane et procédé de production d'éponge de titane Download PDF

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Publication number
WO2019044917A1
WO2019044917A1 PCT/JP2018/031991 JP2018031991W WO2019044917A1 WO 2019044917 A1 WO2019044917 A1 WO 2019044917A1 JP 2018031991 W JP2018031991 W JP 2018031991W WO 2019044917 A1 WO2019044917 A1 WO 2019044917A1
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WO
WIPO (PCT)
Prior art keywords
chlorine
containing gas
chlorine concentration
titanium
concentration
Prior art date
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PCT/JP2018/031991
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English (en)
Japanese (ja)
Inventor
山本　仁
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東邦チタニウム株式会社
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Publication date
Application filed by 東邦チタニウム株式会社 filed Critical 東邦チタニウム株式会社
Priority to JP2019539592A priority Critical patent/JP6816293B2/ja
Publication of WO2019044917A1 publication Critical patent/WO2019044917A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00—Compounds of titanium
    • C01G23/02—Halides of titanium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B34/00—Obtaining refractory metals
    • C22B34/10—Obtaining titanium, zirconium or hafnium
    • C22B34/12—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light

Definitions

  • the present invention relates to a chlorine concentration analyzer, a chlorine concentration analyzer, a titanium tetrachloride manufacturing apparatus, and a sponge titanium manufacturing method using the same.
  • a process of producing titanium tetrachloride by reacting titanium oxide in raw material ore with chlorine using a chlorination furnace is known.
  • a chlorine source supplied into the chlorination furnace for example, a chlorine-containing gas generated in a manufacturing process of titanium oxide, a chlorine-containing gas generated in an electrolysis process of magnesium chloride of sponge titanium, and a purchased chlorine gas can be used.
  • the chlorine-containing gas generated in the manufacturing plant the amount of chlorine gas purchased can be reduced as much as possible, and economics and productivity can be improved.
  • the chlorine-containing gas generated in the manufacturing process of titanium oxide contains more impurities than the purchased chlorine gas etc., and the chlorine concentration in the generated gas may fluctuate depending on the type of titanium oxide to be manufactured. It is preferable to constantly monitor the chlorine concentration in the chlorine-containing gas supplied to the chlorination furnace. The current situation is that gas supply control is being performed based on assumptions and empirical rules.
  • JP-A-2006-519156 proposes a method of performing on-line analysis of chlorine gas concentration in chlorinator exhaust gas or burner exhaust gas with an ultraviolet chlorine analyzer in the production process of titanium dioxide.
  • Patent Document 1 the ultraviolet chlorine analyzer as exemplified in Patent Document 1 is very expensive itself. Therefore, by introducing an expensive analyzer into the feed gas analysis of the chlorination furnace, the profitability of sponge titanium may be reduced and the economy may be impaired.
  • the present invention provides a chlorine concentration analyzer capable of always and inexpensively analyzing the chlorine concentration in a chlorine-containing gas containing a high concentration of chlorine, a chlorine concentration analysis method, a titanium tetrachloride manufacturing apparatus and Provided is a method of producing sponge titanium.
  • the present inventor has found that it is effective to perform chlorine concentration analysis using an absorptiometric method using an LED light source capable of irradiating ultraviolet light.
  • the present invention completed on the basis of the above findings, in one aspect, includes a measuring cell for containing a chlorine-containing gas, a light emitting unit including an LED light source for irradiating ultraviolet light to the chlorine-containing gas flowing in the measuring cell, and a measuring cell
  • the chlorine concentration analyzer includes the light receiving unit that receives the ultraviolet light that has passed through and the calculating unit that calculates the chlorine concentration in the chlorine-containing gas based on the output signal from the light receiving unit.
  • the chlorine concentration analyzer according to the present invention comprises the LED light source emitting ultraviolet light having a wavelength of 200 to 350 nm.
  • the light receiving unit includes a solar cell.
  • the chlorine concentration of the chlorine-containing gas is 1% by mass or more.
  • a chlorine-containing gas is allowed to flow into the measurement cell, and the chlorine-containing gas flowing in the measurement cell is irradiated with ultraviolet light from a light emitting unit including an LED light source capable of irradiating ultraviolet light.
  • a chlorine concentration analysis method is provided that includes: receiving the ultraviolet light transmitted through the measurement cell in the light receiving unit; and calculating the chlorine concentration in the chlorine-containing gas based on the output signal from the light receiving unit.
  • the chlorine concentration analysis method according to the present invention includes, in one embodiment, irradiating a chlorine-containing gas with ultraviolet light having a wavelength of 200 nm to 350 nm.
  • the chlorine concentration analysis method according to the present invention includes, in another embodiment, using a solar cell in the light receiving unit.
  • the method for analyzing chlorine concentration according to the present invention includes, in yet another embodiment, analyzing a chlorine-containing gas having a chlorine concentration of 1% by mass or more.
  • the chlorine-containing gas includes at least one of a chlorine-containing gas generated in a manufacturing process of titanium oxide and a chlorine-containing gas generated in an electrolysis process of magnesium chloride. .
  • a chlorination furnace for producing titanium tetrachloride by contacting a raw material ore containing titanium oxide with a chlorine-containing gas, a supply pipe for supplying the chlorine-containing gas into the chlorination furnace, and a supply pipe And a chlorine concentration analyzer for continuously analyzing the concentration of chlorine in the chlorine-containing gas flowing in the supply pipe.
  • the chlorine-containing gas is at least one of a chlorine-containing gas generated in a titanium oxide manufacturing process and a chlorine-containing gas generated in an electrolysis process of magnesium chloride. including.
  • the apparatus for producing titanium tetrachloride according to the present invention further includes, in another embodiment, a mechanism for adjusting the supply amount of the chlorine-containing gas supplied to the chlorination furnace based on the analysis result of the chlorine concentration by the chlorine concentration analyzer. .
  • a method for producing sponge titanium comprising producing titanium sponge using the titanium tetrachloride obtained by the above-mentioned apparatus for producing titanium tetrachloride.
  • a chlorine concentration analyzer capable of always and inexpensively analyzing the chlorine concentration in a chlorine-containing gas containing a high concentration of chlorine, a chlorine concentration analysis method, a titanium tetrachloride production apparatus and a sponge titanium A manufacturing method can be provided.
  • FIG. 1 is explanatory drawing which shows an example of the manufacturing process of sponge titanium which used the Kroll method.
  • the manufacturing process of sponge titanium includes a chlorination process (S1), a distillation process (S2), a reduction separation process (S3), a crushing process (S4), and an electrolysis process (S5).
  • the raw material ore containing titanium oxide is supplied to the chlorination furnace 101 and is brought into contact with a chlorine-containing gas in the chlorination furnace 101 to generate titanium tetrachloride.
  • the generated titanium tetrachloride is cooled by a condenser 102 connected to a chlorination furnace 101 and recovered to obtain a crude titanium tetrachloride solution.
  • the crude titanium tetrachloride solution is pumped by a pump (not shown) and sent to the pretreatment tank 103, hydrogen sulfide is added in the pretreatment tank 103, and the crude titanium tetrachloride is subjected to sulfurization treatment to obtain vanadium chloride etc. Impurities are removed.
  • the crude titanium tetrachloride solution pretreated in the pretreatment tank 103 is heated in the evaporation vessel 104 and then distilled in the distillation column 105 to obtain purified titanium tetrachloride (distillation step S2).
  • a raw material of sponge titanium can be obtained by subjecting this purified titanium tetrachloride to reduction separation processing in the reduction separation step S3.
  • the reduction separation step S3 titanium tetrachloride is reduced with magnesium in a reduction furnace formed of a stainless steel or iron container under an argon atmosphere, and sponge titanium is generated while intermittently extracting magnesium chloride as a by-product.
  • the sponge titanium produced in the reduction furnace is transferred to the separation furnace, and the separation furnace and the condenser connected to the separation furnace are evacuated to perform vacuum separation processing.
  • the sponge titanium after vacuum separation processing is crushed to a predetermined size in the crushing step S4, and then stored in a closed container for product shipment.
  • the titanium sponge produced in this step can be used to produce a desired product such as titanium ingot or titanium alloy.
  • magnesium chloride produced as a by-product in the reduction separation step S3 is carried to the electrolysis step S5 and accommodated in the electrolytic cell 106, and is separated into metallic magnesium and chlorine gas (chlorine-containing gas) by molten salt electrolysis.
  • the chlorine-containing gas obtained in the electrolysis step can be supplied from the electrolytic cell 106 into the chlorination furnace 101 through the supply pipe 107 connected to the chlorination furnace 101.
  • a supply line (not shown) for supplying the chlorine-containing gas recovered in the titanium oxide production process or the chlorine gas purchased from the outside is connected. That is, the supply pipe 107 connected to the chlorination furnace 101 contains at least one of the chlorine-containing gas generated in the manufacturing process of titanium oxide and the chlorine-containing gas generated in the electrolysis process of magnesium chloride of sponge titanium.
  • the chlorine concentration in the chlorine-containing gas recovered in the titanium oxide production step is lower in chlorine concentration than the chlorine-containing gas obtained in the electrolysis step S5. Therefore, by supplying the chlorine-containing gas recovered in the titanium oxide production process to the chlorination furnace 101, the chlorine concentration in the chlorination furnace 101 may be lower than expected.
  • a chlorine concentration analyzer 1 is connected to a supply pipe 107 for supplying a chlorine-containing gas to the chlorination furnace 101, and can continuously analyze the concentration of chlorine supplied into the chlorination furnace 101;
  • the adjustment mechanism 2 which controls supply_amount
  • the installation position of the chlorine concentration analyzer 1 is not particularly limited, and it may be disposed at any position where the chlorine concentration in the chlorine-containing gas flowing into the chlorination furnace 101 can be analyzed.
  • the chlorine concentration analyzer 1 includes a measurement cell 10 that contains a chlorine-containing gas, and a light emitting unit 20 that includes an LED light source 21 that emits ultraviolet light to the chlorine-containing gas flowing in the measurement cell 10.
  • the light receiving unit 30 receives the ultraviolet light transmitted through the measurement cell 10, and the operation unit 50 calculates the chlorine concentration in the chlorine-containing gas based on the output signal from the light receiving unit 30.
  • the chlorine-containing gas can be circulated continuously inside the measuring cell 10.
  • a pair of transmission plates 11 for transmitting the light from the light emitting unit 20 to the light receiving unit 30 via the measurement cell 10 is disposed in a portion facing the light emitting unit 20 and the light receiving unit 30 of the measurement cell 10 .
  • the material of the transmission plate 11 is not particularly limited, but can be made of, for example, quartz glass.
  • the light emitting unit 20 can include an LED light source 21, a constant current driver for driving the LED light source 21, and an AC / DC converter 23 that converts a DC voltage supplied to the constant current driver from an AC voltage.
  • an LED light source 21 of the light emitting unit 20 since it is not necessary to use an expensive xenon lamp or a power source as in the prior art, the chlorine concentration in the chlorine containing gas can be analyzed more simply and economically.
  • the LED light source 21 used it is preferable to use a deep ultraviolet LED which emits ultraviolet light having a wavelength of 200 to 350 nm, preferably 250 to 300 nm.
  • a deep ultraviolet LED that emits ultraviolet light having a wavelength of 200 to 350 nm, preferably 250 to 300 nm, as the LED light source 21 chlorine molecules contained in the chlorine-containing gas can be more appropriately It can be detected.
  • the LED light source 21 emits ultraviolet light including 254 nm, which is a chlorine molecule absorption wavelength, by using the LED light source 21 having an emission center wavelength of 260 to 270 nm and a half width of 15 nm. Therefore, the absorption by chlorine can be properly analyzed.
  • the conventional expensive chlorine concentration analyzer emits a very wide range of wavelengths, and from among them, only the target wavelength is dispersed and analyzed from the absorption wavelength and absorbance of the substance.
  • the chlorine concentration analyzer 1 according to the present embodiment, by selectively irradiating light of a wavelength suitable for detection of chlorine molecules from the LED light source 21, there is no need to install a spectroscope or the like on the light receiving unit 30 side. It is possible to obtain a simpler chlorine concentration analyzer 1 suitable for analysis of chlorine concentration.
  • the use of a surface-mounted deep ultraviolet LED as the LED light source 21 can miniaturize the device.
  • the light receiving unit 30 is not particularly limited as long as it includes an element that converts light into an electrical signal.
  • a photodiode, an amorphous solar cell, or the like can be used.
  • a solar cell By using a solar cell, a cheaper and simpler chlorine concentration analyzer 1 can be obtained.
  • the LED light source 21 is used for the light emitting unit 20, and the light emitting unit 20 emits light of a wavelength necessary for chlorine concentration analysis.
  • the apparatus can be simplified using a solar cell or the like.
  • a display meter 40 and an operation unit 50 are connected to the light receiving unit 30. Based on the calibration curve data prepared in advance from the relationship between the chlorine concentration of the measurement gas determined by the existing Orsat method and the display meter voltage output from the light receiving unit 30 and displayed on the display meter 40, the calculation unit 50 The chlorine concentration in the chlorine-containing gas that has flowed into the measurement cell 10 can be calculated.
  • the light emitting unit 20 it is preferable to shield light around the measurement cell 10, the light emitting unit 20, and the light receiving unit 30. Thereby, the light reception accuracy of the light receiving unit 30 can be improved, and the density analysis accuracy can be further improved.
  • the chlorine-containing gas is circulated in the measuring cell 10, and the light emitting unit 20 includes the LED light source 21 capable of irradiating ultraviolet light. Then, the ultraviolet light is irradiated to the chlorine-containing gas flowing in the measuring cell 10. Then, the ultraviolet light transmitted through the measurement cell 10 is received by the light receiving unit 30, and the chlorine concentration in the chlorine-containing gas is calculated by the calculating unit 50 based on the output signal from the light receiving unit 30.
  • the chlorine concentration in the chlorine-containing gas flowing in the measuring cell 10 specifically 1% by mass to 100% by mass, more specifically
  • the chlorination furnace 101 is further provided with the adjustment mechanism 2 for adjusting the supply amount of the chlorine-containing gas supplied to the chlorination furnace 101 based on the analysis result of the chlorine concentration by the chlorine concentration analyzer 1. Since it is possible to manually or automatically adjust the concentration of chlorine gas supplied to the inside to a more appropriate range, titanium tetrachloride can be stably produced in the chlorination furnace 101.

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Abstract

La présente invention concerne un dispositif d'analyse de concentration de chlore, comprenant : une cellule de mesure 10 pour contenir un gaz contenant du chlore ; une unité d'émission de lumière 20 pourvue d'une source de lumière à LED 21 pour irradier le gaz contenant du chlore s'écoulant à travers la cellule de mesure 10 avec des rayons UV ; une unité de réception de lumière 30 pour recevoir les rayons UV transmis à travers la cellule de mesure 10 ; et une unité de calcul 50 pour calculer la concentration de chlore dans le gaz contenant du chlore sur la base d'un signal de sortie provenant de l'unité de réception de lumière 30.
PCT/JP2018/031991 2017-09-01 2018-08-29 Dispositif d'analyse de concentration de chlore, procédé d'analyse de concentration de chlore, dispositif de production de tétrachlorure de titane et procédé de production d'éponge de titane WO2019044917A1 (fr)

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JP2019539592A JP6816293B2 (ja) 2017-09-01 2018-08-29 塩素濃度分析装置、塩素濃度分析方法、四塩化チタンの製造装置及びスポンジチタンの製造方法

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JP2017-168772 2017-09-01

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Cited By (2)

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Publication number Priority date Publication date Assignee Title
JP2021021714A (ja) * 2019-07-30 2021-02-18 株式会社フジキン 異常検知方法
WO2022024407A1 (fr) * 2020-07-28 2022-02-03 株式会社トラステック愛知 Dispositif de détection de concentration de gaz

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113184900B (zh) * 2021-05-12 2022-08-12 攀钢集团钒钛资源股份有限公司 四氯化钛生产方法、系统及原料配比调整方法

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JPS52113786A (en) * 1976-03-18 1977-09-24 Cerberus Ag Apparatus for detecting fine particle such as smoke
JPH06508443A (ja) * 1992-04-06 1994-09-22 ローズマウント　アナリティカル　インコーポレイテッド 光度計
JP2006519156A (ja) * 2003-02-25 2006-08-24 トロノックス エルエルシー 二酸化チタンを製造するための改善方法
US20100208239A1 (en) * 2009-02-18 2010-08-19 Nicholas Materer Chlorine dioxide sensor
JP2015081830A (ja) * 2013-10-22 2015-04-27 日機装株式会社 分析装置
WO2017146109A1 (fr) * 2016-02-23 2017-08-31 東邦チタニウム株式会社 Récipient ou tube métallique, procédé de production de titane spongieux et procédé de production de produit traité de titane ou de produit de coulée de titane

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JPH0843302A (ja) * 1994-07-30 1996-02-16 Horiba Ltd 紫外線分析計

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS52113786A (en) * 1976-03-18 1977-09-24 Cerberus Ag Apparatus for detecting fine particle such as smoke
JPH06508443A (ja) * 1992-04-06 1994-09-22 ローズマウント　アナリティカル　インコーポレイテッド 光度計
JP2006519156A (ja) * 2003-02-25 2006-08-24 トロノックス エルエルシー 二酸化チタンを製造するための改善方法
US20100208239A1 (en) * 2009-02-18 2010-08-19 Nicholas Materer Chlorine dioxide sensor
JP2015081830A (ja) * 2013-10-22 2015-04-27 日機装株式会社 分析装置
WO2017146109A1 (fr) * 2016-02-23 2017-08-31 東邦チタニウム株式会社 Récipient ou tube métallique, procédé de production de titane spongieux et procédé de production de produit traité de titane ou de produit de coulée de titane

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2021021714A (ja) * 2019-07-30 2021-02-18 株式会社フジキン 異常検知方法
JP7249031B2 (ja) 2019-07-30 2023-03-30 株式会社フジキン 異常検知方法
WO2022024407A1 (fr) * 2020-07-28 2022-02-03 株式会社トラステック愛知 Dispositif de détection de concentration de gaz
JP2022024437A (ja) * 2020-07-28 2022-02-09 株式会社トラステック愛知 ガス濃度検知装置

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