CN114288837A - Chemical decarburization device and chemical decarburization method for halide molten salt - Google Patents
Chemical decarburization device and chemical decarburization method for halide molten salt Download PDFInfo
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- CN114288837A CN114288837A CN202111522711.1A CN202111522711A CN114288837A CN 114288837 A CN114288837 A CN 114288837A CN 202111522711 A CN202111522711 A CN 202111522711A CN 114288837 A CN114288837 A CN 114288837A
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
- Y02C20/00—Capture or disposal of greenhouse gases
- Y02C20/40—Capture or disposal of greenhouse gases of CO2
Abstract
The invention relates to a chemical decarbonization device of halide fused salt, which comprises an electric heating furnace, a bubbling pipe, a feed inlet and a reaction kettle, wherein a solid halide raw material containing carbon or organic matters is added into the reaction kettle through the feed inlet, the electric heating furnace is arranged around the reaction kettle to heat the solid halide raw material added into the reaction kettle to form liquid fused salt, and the liquid fused salt is obtained from CO2CO of gas source2Introducing Ar from Ar gas source below the liquid surface of the liquid molten salt through the bubbling pipe to remove CO after the high-temperature gas-solid phase decarburization reaction2Thereby realizing decarburization purification. The invention also relates to a chemical decarburization method of the halide molten salt. According to the method for the chemical decarbonization of a molten halide salt according to the invention, by means of CO2The carbon in the halide molten salt is subjected to gas-solid phase reaction to generate CO gas which overflows the molten saltThereby achieving the purpose of chemical decarburization of the molten salt.
Description
Technical Field
The invention relates to inorganic chemical separation and purification, in particular to a chemical decarburization device and a chemical decarburization method for halide molten salt.
Background
Molten salt refers to a liquid phase salt that is normally solid at Standard Temperature and Pressure (STP) (i.e., solid at normal temperature, liquid at elevated temperature, and liquid at elevated temperature is normally used). Molten salts that are normally liquid at STP are referred to as room temperature ionic liquids. The halide fused salt is mainly a metal compound or a mixture melt of metal compounds formed by VIIA elements (F, Cl, Br and I), and the chloride fused salt and the fluoride fused salt are generally widely applied. Molten chloride-molten salt mixtures are commonly used as a medium for heat treatment of various alloys, such as annealing and abrasive grain tempering of steel; the chloride molten salt mixture is used for surface modification of alloys, such as carburization and nitrocarburizing of steel; the multi-element chloride molten salt is an excellent heat transfer and storage medium due to excellent physicochemical properties, and can be used for a focusing solar thermal power generation system. Cryolite (Na)3AlF6) As a solvent for alumina in the production of aluminum; the multi-element fluoride molten salt can be used as a heat transfer medium of a molten salt reactor and a main component of liquid fuel salt.
Since the metal halide usually contains crystal water or is prone to moisture absorption, a high-temperature hydrolysis reaction occurs after the metal halide is melted at a high temperature to generate a second-phase oxide (which refers to a metal oxide or a metal hydroxide, and is mainly a metal oxide), and therefore dehydration, deoxidation and purification of the halide molten salt are required. However, the metal halide raw material usually contains organic impurities (such as engine oil, extractant and the like), or the dehydration and drying of the anhydrous metal halide raw material are carried out in a graphite crucible, which causes that the molten salt prepared from the halide raw material at high temperature contains carbon simple substance which floats on the surface of the molten salt and affects the deoxidation and purification of the halide molten salt, or adversely affects the quality of the product after the molten salt treatment, for example, in the halide molten salt electrolysis or electroplating process, the existence of a surface carbon layer not only easily causes short circuit of a cathode and an anode, but also can cause carbon inclusion in the electrolysis product or the coating, and seriously deteriorates the product quality.
Currently, as for the high-temperature decarburization method, bubbling entrainment decarburization is the most common method, but the method has a limited effect and complete decarburization is difficult to achieve. For example, CN104099445A discloses a method for deep decarburization of ultra-low carbon steel, which is to blow oxygen gas at the temperature range of 1610-2And molten steel overflows. The method is not suitable for a halide molten salt system, because the oxygen dissolving amount of the molten salt is greatly increased, and even high-temperature oxidation reaction occurs. Thus, there is a high necessity for a method capable of completely decarburizing a molten halide molten salt, which is a problem to be solved by the present invention.
Disclosure of Invention
In order to fill the technical blank of removing impurity carbon in molten halide molten salt in the prior art, the invention provides a chemical decarburization device and a chemical decarburization method for the halide molten salt.
The chemical decarbonization device of the halide molten salt comprises an electric heating furnace, a bubbling pipe, a feed inlet and a reaction kettle, wherein the solid halide raw material containing carbon or organic matters is added into the reaction kettle through the feed inlet, the electric heating furnace is arranged around the reaction kettle to heat the solid halide raw material added into the reaction kettle to form liquid molten salt, and the liquid molten salt is obtained from CO2CO of gas source2Introducing liquid molten salt below the liquid level through a bubbling pipe to perform high-temperature gas-solid phase decarburization reaction (CO)2Gas and solid carbon react to generate CO gas), Ar from an Ar gas source is introduced below the liquid level of the liquid molten salt through a bubbling tube to remove CO after the high-temperature gas-solid phase decarburization reaction2Thereby realizing decarburization purification.
It should be understood that the solid carbon removed in the high-temperature gas-solid phase decarburization reaction may be the carbon element contained in the solid halide raw material itself,or the carbon simple substance generated by the pyrolysis of the organic matter under the high-temperature melting condition. It should be appreciated that the electric furnace heats the solid halide feed above 650 c. It is understood that the introduction of Ar is carried out after the high-temperature gas-solid phase decarburization reaction, that is, after a certain period of time of CO2The bubbling treatment is performed.
Preferably, the halide molten salt is a single molten salt (e.g., KBr) or a multi-component molten salt (e.g., LiF-BeF)2Or KCl-NaCl-MgCl2)。
Preferably, the length-diameter ratio of a molten salt liquid column formed by the liquid molten salt in the reaction kettle is more than or equal to 3.
Preferably, the distance between the bottom of the bubbling tube and the bottom of the reaction vessel is less than 60% of the height of the molten salt liquid column. It should be understood that the specific values are determined based on the amount of second phase oxide impurities of the molten salt. If the second phase oxide is contaminated with a large amount of impurities, it is deposited on the bottom of the vessel in a large amount, and the bubble tube is easily clogged as it is inserted deeper, but if it is inserted too shallowly, the decarburization effect is not good, so that the insertion depth of the bubble tube is selected appropriately. When the length-diameter ratio of the molten salt liquid column is more than or equal to 3, the content of the second-phase oxide is less than 5 percent, and the height of the bottom of the bubbling pipe is 10 percent of that of the liquid column; if the content of the second-phase oxide is 5-20%, the height of the bubbling pipe from the bottom is 30% of that of the liquid column; if the content of the second phase oxide is more than 20 percent, the height of the bubbling pipe from the bottom is 50 to 60 percent of the liquid column.
Preferably, the depth of the bubbling pipe extending into the reaction kettle is adjusted by welding a ferrule boring through.
Preferably, the bubbler tube is a pure nickel tube. In particular, the material of the bubbling pipe portion that protrudes below the liquid molten salt level is pure nickel.
Preferably, the chemical decarburization device includes a plurality of bubbling pipes to improve the decarburization efficiency. In a preferred embodiment, three bubble tubes are in a regular triangular arrangement. It should be understood that a single bubble tube is also possible.
Preferably, the reaction kettle is a pure nickel kettle. In particular, the material of the part of the reactor in contact with the liquid molten salt is pure nickel.
Preferably, CO2Is introduced intoIn an amount of CO2The flow meter is adjusted.
Preferably, the amount of Ar introduced is adjusted by an Ar flow meter.
Preferably, the chemical decarbonization device also comprises a multi-stage CO absorption tank communicated with the reaction kettle through a CO tail gas pipe. In a preferred embodiment, each CO absorption tank contains an ammonia water solution of CuCl, so as to absorb CO in the tail gas after decarburization.
Preferably, the interface of the CO tail gas pipe and the reaction kettle is in welded seal or threaded clamping sleeve seal connection.
Preferably, the chemical decarburization device further comprises a drying facility for removing CO from the offgas after decarburization2And (5) carrying out drying treatment.
Preferably, the chemical decarbonization device also comprises a reaction kettle and CO2CO between gas sources2A return pipe. It should be understood that CO2The return pipe is arranged behind the drying equipment to dry the treated CO2By CO2Return line to CO2Gas source to thereby realize CO2Can be repeatedly used.
The chemical decarburization method of the halide molten salt comprises the steps of adding a solid halide raw material containing carbon or organic matters into a reaction kettle, heating the reaction kettle to enable the solid halide raw material to form liquid molten salt, and adding CO2Introducing liquid molten salt below the liquid level via a bubbling pipe to perform high-temperature gas-solid phase decarburization reaction, and stopping introducing CO2Thereafter, Ar is introduced below the liquid molten salt surface through a bubbling tube to remove CO2Thereby realizing decarburization purification.
Preferably, the carbon content of the halide molten salt before decarburization is between 0.1 and 1 wt%, and the carbon content of the halide molten salt after decarburization is less than 10 ppm.
Preferably, the distance between the bottom of the bubbling tube and the bottom of the reaction kettle is set according to the height of a molten salt liquid column formed by the liquid molten salt in the reaction kettle.
Preferably, the temperature of the high-temperature gas-solid phase decarburization reaction is between 650-1000 ℃. The total oxygen content of the halide molten salt subjected to decarburization at the temperature cannot be increased, and meanwhile, the vapor pressure of most of the halide molten salt is increased sharply after the temperature is higher than 1000 ℃, so that the molten salt system is unstable.
Preferably, the high-temperature gas-solid phase decarburization reaction time is between 10 and 72 hours.
Preferably, CO2The introduction flow rate of (2) is between 100 and 600 ml/min.
According to the method for the chemical decarbonization of a molten halide salt according to the invention, by means of CO2The carbon gas-solid phase reaction is carried out with the carbon simple substance in the halide fused salt to generate CO gas which overflows a fused salt system, thereby achieving the purpose of chemical decarburization of the fused salt. The specific reaction equation is
In conclusion, the chemical decarburization method of the halide molten salt provided by the invention can realize the chemical decarburization of the molten single halide molten salt or the molten mixed halide molten salt, and can avoid blowing O at high temperature2The oxygen content of the molten salt is improved due to decarburization, simple substance carbon in the molten salt can be completely removed without increasing the total oxygen content of the molten salt, the carbon content in the molten salt can be reduced from 0.1-1 wt% to less than 10ppm, and the method has important significance for purification and refining of commercial halide molten salt.
Drawings
FIG. 1 is a schematic structural view of a chemical decarburization device of a halide molten salt according to a preferred embodiment of the present invention;
FIG. 2 is CO of example 12Photographs of the surface carbon layer before and after the treatment.
Detailed Description
The preferred embodiments of the present invention will be described in detail below with reference to the accompanying drawings.
The chemical decarbonizing apparatus used in the following examples is constructed as shown in FIG. 1, and comprises an electric heating furnace 1, a bubbling pipe 2, a charging port 3 and a reaction vessel 10, wherein the solid halide raw material is charged into the reaction vessel 10 through the charging port 3, the electric heating furnace 1 is arranged around the reaction vessel 10 to heat the solid halide raw material charged into the reaction vessel 10 to form a liquid molten salt, which is derived from CO2CO of gas source2Through drumThe bubble tube 2 is introduced below the liquid level of the liquid molten salt to perform a high-temperature gas-solid phase decarburization reaction, and the introduction of CO is stopped2Thereafter, Ar from an Ar gas source is introduced below the liquid molten salt level through the bubbling tube 2 to remove CO2Thereby realizing decarburization purification. In this example, CO2Is introduced in an amount of CO2The flow meter 6 is used for adjusting, the introduction amount of Ar is adjusted through the Ar flow meter 7, and the depth of the bubbling pipe 2 extending into the reaction kettle 10 is adjusted through the welding of the ferrule boring through 9. The chemical decarburization device further comprises a multistage CO absorption tank 4 which is communicated with the reaction kettle 10 through a CO tail gas pipe 5, and CuCl ammonia water solution is filled in the multistage CO absorption tank, so that CO in tail gas after decarburization is absorbed. In this embodiment, the interface between the CO off-gas pipe 5 and the reaction kettle 10 is a welded seal or a threaded ferrule seal. The chemical decarburization device also comprises a drying device which is used for removing CO in the tail gas after decarburization2Drying with CO2Return line 8 for returning to CO2Gas source to thereby realize CO2Can be repeatedly used. The chemical decarbonization apparatus further comprises CO2Reflux valve a, CO2An inlet valve b, an Ar inlet valve c and an inlet main valve d, wherein CO2The reflux valve a is arranged at the CO2On the return pipe 8, CO2An air inlet valve b is arranged at the CO2The air inlet valve d is arranged on the bubbling tube 2, and the Ar air inlet valve c is arranged between the Ar air source and the bubbling tube 2.
Example 1
Taking LiF-BeF with carbon content of about 1 wt%21kg of binary molten salt is fed from a feed inlet 3, then the reaction kettle 10 is sealed and heated to melt until the temperature of the molten salt reaches 750 ℃, the length-diameter ratio of a molten salt liquid column is 3, and a black carbon layer floats on the surface after melting at 750 ℃, as shown in (a) of figure 2, the carbon content of the molten salt after melting is about 0.5 wt%. Since the content of solid particles of the second phase oxide in the molten salt is less than 5 wt%, the bubbling tube 2 is inserted into the liquid LiF-BeF2And ensuring that the distance from the bottom of the kettle is 10% of the height of the molten salt liquid column.
Turn on CO2And (3) an air source, opening valves b, d and a, and closing a valve c. Setting up CO2Introducing the gas into the reaction kettle at a flow rate of 500ml/min for bubbling decarburization reaction, and closing the reaction kettle after continuously bubbling for 72 hoursOpening the valve b, bubbling and blowing the solution in LiF-BeF by setting the Ar flow at 200ml/min2Trace amount of CO in molten salt2And after purging for 4 hours, closing valves c, d and a, LiF-BeF2Decarburization and purification of the molten salt is completed, LiF-BeF2The carbon content of the molten salt is less than 10ppm, and as shown in (b) of fig. 2, the black carbon layer on the surface of the molten salt is almost completely removed after melting at 750 ℃.
Example 2
Taking KCl-NaCl-MgCl with carbon content of about 0.1 wt%23kg of ternary molten salt is fed from a feed inlet 3, then the reaction kettle 10 is sealed, heated and melted until the temperature of the molten salt reaches 650 ℃, and the length-diameter ratio of a molten salt liquid column is ensured to be 4, and the carbon content of the molten salt after melting is about 0.1 wt%. Since the content of solid particles of the second phase oxide in the molten salt is about 5 wt% to 20 wt%, the bubbling tube 2 is inserted into the liquid KCl-NaCl-MgCl2And ensuring that the distance from the bottom of the kettle is 30% of the height of the molten salt liquid column.
Turn on CO2And (3) an air source, opening valves b, d and a, and closing a valve c. Setting up CO2Introducing gas into the reaction kettle at a flow rate of 100ml/min for bubbling decarburization reaction, continuously bubbling for 60h, closing the valve b, opening the valve c, and setting Ar flow rate to be 200ml/min for bubbling, purging and dissolving in KCl-NaCl-MgCl2Trace amount of CO in molten salt2And after purging for 2 hours, closing valves c, d and a, KCl-NaCl-MgCl2The carbon content of the molten salt is less than 10 ppm.
Example 3
3kg of KBr molten salt with the carbon content of about 0.5 wt% is taken and fed from a feed inlet 3, then the reaction kettle 10 is sealed and heated to be molten until the temperature of the molten salt reaches 1000 ℃, the length-diameter ratio of a molten salt liquid column is ensured to be 5, and the carbon content of the molten salt after the molten salt is about 1 wt%. Because the content of solid particles of the second-phase oxide in the molten salt is more than 20 wt%, the bubble tubes 2 can be inserted into the liquid KBr molten salt in an equilateral triangle arrangement mode by adopting three bubble tubes, and the distance from the bottom of the kettle is ensured to be 60% of the height of a molten salt liquid column.
Turn on CO2And (3) an air source, opening valves b, d and a, and closing a valve c. Setting up CO2Introducing the gas into three bubbling tubes in the reaction kettle at a total gas flow of 600ml/min for bubbling decarburization reaction, closing the valve b after continuously bubbling for 10 hours,opening a valve c, setting the Ar flow at 200ml/min, bubbling and purging trace CO dissolved in the KBr molten salt2And after purging for 4 hours, closing valves c, d and a, wherein the carbon content of the KBr molten salt is less than 10 ppm.
The above embodiments are merely preferred embodiments of the present invention, which are not intended to limit the scope of the present invention, and various changes may be made in the above embodiments of the present invention. All simple and equivalent changes and modifications made according to the claims and the content of the specification of the present application fall within the scope of the claims of the present patent application. The invention has not been described in detail in order to avoid obscuring the invention.
Claims (10)
1. The chemical decarbonization device of the halide fused salt is characterized by comprising an electric heating furnace, a bubbling pipe, a feed inlet and a reaction kettle, wherein a solid halide raw material containing carbon or organic matters is added into the reaction kettle through the feed inlet, the electric heating furnace is arranged around the reaction kettle to heat the solid halide raw material added into the reaction kettle to form liquid fused salt, and the liquid fused salt comes from CO2CO of gas source2Introducing Ar from Ar gas source below the liquid surface of the liquid molten salt through the bubbling pipe to remove CO after the high-temperature gas-solid phase decarburization reaction2Thereby realizing decarburization purification.
2. The chemical decarburization device of claim 1, wherein the aspect ratio of a molten salt liquid column formed in the reaction vessel by the liquid molten salt is 3 or more.
3. The chemical decarburization apparatus according to claim 2, wherein the distance between the bottom of the bubbling tube and the bottom of the reaction vessel is less than 60% of the height of the molten salt liquid column.
4. The chemical decarburization device of claim 1, wherein the depth of the bubbling tube extending into the reaction vessel is adjusted by welding ferrule boring passages.
5. The chemical decarburization apparatus of claim 1, further comprising a CO generator disposed in the reaction vessel2CO between gas sources2A return pipe.
6. The chemical decarbonization method of halide molten salt is characterized by comprising the steps of adding a solid halide raw material containing carbon or organic matters into a reaction kettle, heating the reaction kettle to enable the solid halide raw material to form liquid molten salt, and adding CO2Introducing liquid molten salt below the liquid level via a bubbling pipe to perform high-temperature gas-solid phase decarburization reaction, and stopping introducing CO2Thereafter, Ar is introduced below the liquid molten salt surface through a bubbling tube to remove CO2Thereby realizing decarburization purification.
7. The chemical decarburization method according to claim 6, wherein the carbon content of the molten halide salt before decarburization is between 0.1 and 1 wt%, and the carbon content of the molten halide salt after decarburization is less than 10 ppm.
8. The chemical decarburization method as claimed in claim 6, wherein the high temperature gas-solid decarburization reaction is carried out at a temperature of 650-1000 ℃.
9. The chemical decarburization method as claimed in claim 6, wherein the high temperature gas-solid phase decarburization reaction is carried out for a period of 10 to 72 hours.
10. The chemical decarburization method of claim 6, wherein CO is2The introduction flow rate of (2) is between 100 and 600 ml/min.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US11931763B2 (en) | 2019-11-08 | 2024-03-19 | Abilene Christian University | Identifying and quantifying components in a high-melting-point liquid |
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