CN114288837B - 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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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 CO 2 CO of gas source 2 Introducing 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 reaction 2 Thereby 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 CO 2 The 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.
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). Normally liquid at STPThe molten salt of (a) is referred to as a room temperature ionic liquid. 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) 3 AlF 6 ) 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- 2 And molten steel overflows. The method is not applicable to a halide molten salt system, because the oxygen dissolving amount of the molten salt is greatly increased,even high temperature oxidation reactions occur. Thus, there is a high necessity for a method capable of completely decarburizing a molten halide 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 CO 2 CO of gas source 2 Introducing liquid molten salt below the liquid level through a bubbling pipe to perform high-temperature gas-solid phase decarburization reaction (CO) 2 Gas 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 reaction 2 Thereby realizing decarburization purification.
It should be understood that the solid carbon removed in the high-temperature gas-solid phase decarburization reaction may be a simple substance of carbon contained in the solid halide raw material itself, or a simple substance of carbon generated by pyrolyzing an organic substance under a 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 CO 2 The 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) 2 Or KCl-NaCl-MgCl 2 )。
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 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 tube extending into the reaction kettle is adjusted by welding 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, CO 2 Is introduced in an amount of CO 2 The 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 decarburization 2 And (5) carrying out drying treatment.
Preferably, the chemical decarbonization device also comprises a reaction kettle and CO 2 CO between gas sources 2 A return pipe. It should be understood that CO 2 The return pipe is arranged behind the drying equipment to dry the treated CO 2 By CO 2 Return line to CO 2 Gas source to thereby realize CO 2 Can 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 CO 2 Introducing liquid molten salt below the liquid level via a bubbling pipe to perform high-temperature gas-solid phase decarburization reaction, and stopping introducing CO 2 Thereafter, Ar is introduced below the liquid molten salt surface through a bubbling tube to remove CO 2 Thereby realizing decarburization purification.
Preferably, the carbon content of the halide molten salt before decarburization is between 0.1 and 1wt%, 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 time of the high-temperature gas-solid phase decarburization reaction is between 10 and 72 hours.
Preferably, CO 2 The 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 CO 2 The 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 summary, the present invention provides a halide molten saltThe chemical decarburization method 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 temperature 2 The 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 0.1-1wt% 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 1 2 Photographs 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 disposed 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 CO 2 CO of gas source 2 Introducing the molten salt below the liquid surface through a bubbling pipe 2 to perform high-temperature gas-solid phase decarburization reaction, and stopping introducing CO 2 Thereafter, Ar from an Ar gas source is introduced below the liquid molten salt level through the bubbling tube 2 to remove CO 2 Thereby realizing decarburization purification. In this example, CO 2 Is introduced in an amount of CO 2 The 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 decarbonization apparatus also comprises a drying device for the chemical decarbonizationCO in tail gas after decarburization 2 Drying with CO 2 Return line 8 for returning to CO 2 Gas source to thereby realize CO 2 Can be repeatedly used. The chemical decarbonization device also comprises CO 2 Reflux valve a, CO 2 An inlet valve b, an Ar inlet valve c and an inlet main valve d, wherein CO 2 The reflux valve a is arranged at the CO 2 On the return pipe 8, CO 2 An air inlet valve b is arranged at the CO 2 The 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 1wt% 2 1kg 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-BeF 2 And ensuring that the distance from the bottom of the kettle is 10% of the height of the molten salt liquid column.
Turn on CO 2 And (3) an air source, opening valves b, d and a, and closing a valve c. Setting up CO 2 Introducing gas into the reaction kettle at a flow rate of 500ml/min for bubbling decarburization reaction, closing the valve b after continuously bubbling for 72h, opening the valve c, and setting the Ar flow rate to be 200ml/min for bubbling, blowing and dissolving in LiF-BeF 2 Trace amount of CO in molten salt 2 And after 4 hours of purging, closing valves c, d and a, LiF-BeF 2 Decarburization and purification of the molten salt is completed, LiF-BeF 2 The 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% 2 3kg 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 pipe 2 is inserted into the liquid stateKCl-NaCl-MgCl 2 And ensuring that the distance from the bottom of the kettle is 30% of the height of the molten salt liquid column.
Turn on CO 2 And (3) an air source, opening valves b, d and a, and closing a valve c. Setting up CO 2 Introducing 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-MgCl 2 Trace amount of CO in molten salt 2 And after purging for 2 hours, closing valves c, d and a, KCl-NaCl-MgCl 2 The 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 CO 2 And (3) an air source, opening valves b, d and a, and closing a valve c. Setting up CO 2 Introducing the gas with the total flow of 600ml/min into three bubbling tubes in the reaction kettle for bubbling decarburization reaction, closing the valve b after continuously bubbling for 10 hours, opening the valve c, and bubbling and purging trace CO dissolved in the KBr molten salt by setting the Ar flow at 200ml/min 2 And 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 (9)
1. A chemical decarburization method for a molten halide salt, characterized in that the chemical decarburization method comprises subjecting carbon-containing or carbon-containing molten saltAdding the solid halide raw material of the organic matter into a reaction kettle, heating the reaction kettle to enable the solid halide raw material to form liquid molten salt, and adding CO 2 Introducing liquid molten salt below the liquid level via a bubbling pipe to perform high-temperature gas-solid phase decarburization reaction, and stopping introducing CO 2 Thereafter, Ar is introduced below the liquid molten salt surface through a bubbling tube to remove CO 2 Thereby realizing decarburization purification, and the temperature of the high-temperature gas-solid phase decarburization reaction is between 650-1000 ℃.
2. The chemical decarburization method according to claim 1, wherein the carbon content of the molten halide salt before decarburization is between 0.1 and 1wt%, and the carbon content of the molten halide salt after decarburization is less than 10 ppm.
3. The chemical decarburization method as claimed in claim 1, wherein the high temperature gas-solid phase decarburization reaction is carried out for a period of 10 to 72 hours.
4. The chemical decarburization method of claim 1, wherein CO is 2 The introduction flow rate of (2) is between 100 and 600 ml/min.
5. The chemical decarburization method as claimed in claim 1, wherein the chemical decarburization process is carried out by a chemical decarburization apparatus comprising an electric furnace, a bubbling tube, a feed opening and a reaction vessel, wherein the solid halide raw material containing carbon or organic matter is fed into the reaction vessel through the feed opening, and the electric furnace is arranged around the reaction vessel to heat the solid halide raw material fed into the reaction vessel to form a molten liquid salt, which is derived from CO 2 CO of gas source 2 Introducing 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 reaction 2 Thereby realizing decarburization purification.
6. The chemical decarburization method according to claim 5, wherein the aspect ratio of a molten salt liquid column formed in the reaction vessel is 3 or more.
7. The chemical decarburization method according to claim 5, 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.
8. The chemical decarburization method as claimed in claim 5, wherein the depth of the bubbling tube extending into the reaction vessel is adjusted by welding ferrule boring passages.
9. The chemical decarburization method as claimed in claim 5, wherein the chemical decarburization device further comprises a CO generator disposed in the reaction vessel 2 CO between gas sources 2 A return pipe.
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