CN115852182B - Preparation method of aluminum amalgam for inactive gas bubbling type mercury delivery - Google Patents

Preparation method of aluminum amalgam for inactive gas bubbling type mercury delivery Download PDF

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CN115852182B
CN115852182B CN202211531499.XA CN202211531499A CN115852182B CN 115852182 B CN115852182 B CN 115852182B CN 202211531499 A CN202211531499 A CN 202211531499A CN 115852182 B CN115852182 B CN 115852182B
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mercury
aluminum
pipeline
inert gas
evaporator
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CN115852182A (en
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黄敏杰
陈扬
冯钦忠
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Beihang University
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Beihang University
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Abstract

The invention discloses a preparation method of an aluminum amalgam for mercury conveying by inert gas bubbling, which relates to the technical field of nonferrous metal smelting. Because mercury enters the molten aluminum soup in a vapor form, the whole process is safe and controllable, and the phenomenon of mercury explosion can not occur. Under the dual actions of bubbling and stirring, the aluminum amalgam with uniform components can be obtained.

Description

Preparation method of aluminum amalgam for inactive gas bubbling type mercury delivery
Technical Field
The invention relates to the technical field of nonferrous metal smelting, in particular to a preparation method of an aluminum amalgam for inert gas bubbling type mercury delivery.
Background
The aluminum water hydrogen production technology is a potential hydrogen production technology, and a reaction product is an important precursor for preparing superfine alumina powder which is another important industrial raw material. Since the surface of aluminum is easily formed with a dense oxide film, aluminum water is prevented from continuing to react, and thus metallic aluminum cannot be directly used for the reaction with aluminum. The mercury in the aluminum amalgam can prevent the surface of aluminum from being oxidized to form a compact oxide film, and the mercury is easy to separate in a heating evaporation mode, so that the aluminum amalgam is a good material for producing hydrogen and superfine alumina powder.
Aluminum amalgam is difficult to prepare by conventional methods because the melting point of aluminum is much higher than the boiling point of mercury. The published preparation methods of the aluminum amalgam are chemical methods, and the aluminum amalgam can be only prepared on the surface of aluminum in a small amount, and the aluminum amalgam has no value of large-scale industrial application.
Disclosure of Invention
The invention aims to provide a preparation method of an aluminum amalgam for inert gas bubbling type mercury delivery, which solves the problems existing in the prior art and can prepare a large amount of aluminum amalgam with uniform properties under safe and reliable conditions.
In order to achieve the above object, the present invention provides the following solutions:
the invention provides a preparation method of an aluminum amalgam for inert gas bubbling mercury delivery, which comprises the following steps:
step one, constructing a bubbling type mercury-conveying aluminum amalgam preparation device;
Calculating the quantity of the required mercury raw material according to the mass of aluminum fed into the reaction furnace at one time, and calculating the quantity and flow of the inert gas required by mercury transportation according to the preparation time requirement;
step three, putting the weighed aluminum into a smelting furnace for smelting;
step four, putting the weighed mercury raw materials into an evaporator, and checking the air tightness of the evaporator to a second pipeline of the reaction furnace;
Step five, a valve on a third pipeline of the inert gas through reaction furnace is opened, and the third pipeline of the inert gas through reaction furnace is temporarily closed after air in the third pipeline is blown off;
step six, after aluminum is melted, removing surface oxide slag, and transferring aluminum in a molten state into a reaction furnace;
Step seven, heat preservation is carried out on the aluminum in the molten state transferred in the reaction furnace, so that the internal temperature of a hearth of the reaction furnace is higher than the melting point of the aluminum, a stirring structure of the reaction furnace is started, oxidized slag sinking at the bottom of the hearth of the reaction furnace floats to the surface, and then slag skimming treatment is carried out on the surface;
Step eight, starting a preheater on the first pipeline to heat the first pipeline, starting a heater of the second pipeline to heat and preserve heat of the second pipeline, and starting an evaporator to heat the mercury raw material;
Step nine, after slag skimming is completed and the temperature of the evaporator reaches a rated value, enabling inert gas to sequentially pass through the preheater and the evaporator, and enabling the inert gas with mercury vapor to enter molten aluminum in a hearth of the reaction furnace through a feeding pipe of the reaction furnace;
Step ten, taking a molten aluminum amalgam sample from a sampling port of the reaction furnace after the preset feeding time is reached, and detecting components in the molten aluminum amalgam sample; if the components meet the requirements, stopping heating the evaporator, closing a valve of the first pipeline, opening a valve of the third pipeline, enabling the inert gas to directly enter the feeding pipe, and maintaining the clean and high-temperature inert gas to be conveyed for a period of time;
And step eleven, the aluminum amalgam prepared in the reaction furnace is emptied, cast and molded, and the preparation work of the hydrogen production material is finished.
Preferably, the preparation device of the bubbling type mercury-delivery aluminum amalgam comprises an inactive gas storage structure, a preheater, an evaporator, a smelting furnace and a reaction furnace, wherein the inactive gas storage structure is used for storing inactive gas, the evaporator is used for heating mercury raw materials, the smelting furnace is used for smelting aluminum, the inactive gas storage structure is connected with the preheater through a first pipeline, the preheater is connected with the evaporator through a first pipeline, the evaporator is connected with a feed pipe of the reaction furnace through a second pipeline, the preheater is connected with the feed pipe of the reaction furnace through a third pipeline, and the smelting furnace is connected with a feed inlet of the reaction furnace.
Preferably, the first pipeline, the second pipeline and the third pipeline are all provided with heaters, and the heaters are cast copper heating rings or ceramic heating rings.
Preferably, in the second step, the mercury raw material is pure mercury or mercury-containing amalgam.
Preferably, the inert gas used is a gas which is stable in properties below 700 ℃ and is not easily reacted with aluminum.
Preferably, the inert gas used is nitrogen or an inert gas.
Preferably, rated operating temperatures of the preheater, the evaporator and the heater of the second pipeline are all set above the boiling point of the mercury feed.
Preferably, the second pipeline is a seamless pipe made of 310S or 316L materials.
Preferably, the material passing pipe is made of a material which is resistant to temperature not lower than 700 ℃ and is not easy to be corroded by aluminum water.
Preferably, the lower end of the material passing pipe is provided with an opening, and the side wall of the lower part of the material passing pipe is provided with a plurality of through holes; the lower end of the feeding pipe is positioned below the liquid level of the aluminum soup and is 1cm away from the bottom of the hearth.
Compared with the prior art, the invention has the following technical effects:
1. the invention can safely prepare a large amount of aluminum amalgam with uniform components;
2. the invention is also suitable for preparing the alloy with the melting point higher than that of the other component by a melting method, so that explosion which is extremely easy to occur in the preparation process is avoided;
3. the activity of the reaction of the aluminum amalgam with water can be realized by adjusting the amount of mercury introduced and controlling the mercury content in the alloy;
4. gaseous mercury is conveyed through an inert gas and conveyed through a third heat-preserving pipeline, so that the mercury is ensured not to cause too violent phase change reaction (bumping) due to sudden boiling when contacting aluminum water;
5. The material passing pipe adopts a side wall porous structure, and when high-concentration mercury-containing gas enters aluminum water, the high-concentration mercury-containing gas can be scattered into a plurality of small bubbles, so that the aluminum and mercury elements are mixed more uniformly and the process is milder.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a flow chart of a method for preparing an aluminum amalgam for inactive gas bubbling mercury delivery according to the present invention;
FIG. 2 is a schematic diagram of a bubbling type mercury-transporting aluminum amalgam preparation device according to the present invention;
wherein: 1-inactive gas storage structure, 2-preheater, 3-evaporator, 4-smelting furnace, 5-first pipeline, 6-second pipeline, 7-third pipeline, 8-reaction furnace.
Description of the embodiments
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by a person skilled in the art based on the embodiments of the invention without any inventive effort, are intended to fall within the scope of the invention.
The invention aims to provide a preparation method of an aluminum amalgam for inert gas bubbling type mercury delivery, which solves the problems existing in the prior art and can prepare a large amount of aluminum amalgam with uniform properties under safe and reliable conditions.
In order that the above-recited objects, features and advantages of the present invention will become more readily apparent, a more particular description of the invention will be rendered by reference to the appended drawings and appended detailed description.
As shown in fig. 1: the embodiment provides a preparation method of an aluminum amalgam for inert gas bubbling mercury delivery, which is used for preparing 100kg of hydrogen production material with 0.5% of mercury content and comprises the following steps:
Step one, accounting for material, taking into account losses, requires about 105kg of aluminum and 1kg of mercury raw material; weighing 105kg of aluminum blocks and about 1kg of mercury raw materials for standby, and constructing a bubbling type mercury-transporting aluminum amalgam preparation device according to FIG. 2;
As shown in fig. 2, the preparation device of the bubbling type mercury-delivery aluminum amalgam comprises an inactive gas storage structure 1, a preheater 2, an evaporator 3, a smelting furnace 4 and a reaction furnace 8, wherein the inactive gas storage structure 1 is used for storing inactive gas, the evaporator 3 is used for heating mercury raw materials, the mercury raw materials are pure mercury or mercury-containing amalgam, the smelting furnace 4 is used for smelting aluminum, the inactive gas storage structure 1 is connected with the preheater 2 through a first pipeline 5, the preheater 2 is connected with the evaporator 3 through the first pipeline 5, the evaporator 3 is connected with a material passing pipe of the reaction furnace 8 through a second pipeline 6, the preheater 2 is connected with a material passing pipe of the reaction furnace 8 through a third pipeline 7, and the smelting furnace 4 is connected with a material inlet of the reaction furnace 8;
calculating the quantity of the required mercury raw material according to the mass of aluminum fed into the reaction furnace 8 at one time, and calculating the quantity and flow of the inert gas required by mercury transportation according to the preparation time requirement;
Step three, putting weighed aluminum into a smelting furnace 4 for smelting, starting up a machine according to the time of the predicted temperature rise of the reaction furnace 8 to the rated temperature (for example 695+/-15 ℃), preheating the reaction furnace 8, and heating a second pipeline 6 to 360+/-40 ℃;
step four, putting the weighed mercury raw material into the evaporator 3, and checking the air tightness of the evaporator 3 to a second pipeline 6 of the reaction furnace 8;
Fifthly, turning on heaters of the preheater 2 and the third pipeline 7 according to the predicted aluminum conversion time and the time required for heating; when the temperature of the third pipeline 7 is raised to 400+/-40 ℃, blowing off air in the third pipeline 7 and the hearth of the reaction furnace 8 by using inert gas; starting the evaporator 3 according to the expected feeding time in a machine selecting mode to heat;
Step six, after aluminum is melted, removing surface oxide slag, and transferring aluminum in a molten state into a reaction furnace 8;
Step seven, heat preservation is carried out on the aluminum in the molten state transferred in the reaction furnace 8, so that the internal temperature of a hearth of the reaction furnace 8 is 35+/-15 ℃ higher than the melting point of the aluminum, a stirring structure of the reaction furnace 8 is started, oxide slag sinking at the bottom of the hearth of the reaction furnace 8 floats up to the surface, slag skimming treatment is carried out on the surface, and a valve of a third pipeline 7 is closed after slag skimming;
Step eight, starting a preheater 2 on a first pipeline 5 to heat the first pipeline 5, starting a heater of a second pipeline 6 to heat and preserve heat of the second pipeline 6, and starting an evaporator 3 to heat mercury raw materials;
Step nine, after slag skimming is completed, and the temperature of the evaporator 3 reaches a rated value, a valve of a first pipeline 5 is opened to enable inert gas to sequentially pass through the preheater 2 and the evaporator 3, and the inert gas with mercury vapor enters molten aluminum in a hearth of the reaction furnace 8 through a feed pipe of the reaction furnace 8;
step ten, predicting the casting time of aluminum discharge and the heating time of the aluminum discharge port heating device, and selecting a machine to start heating the aluminum discharge port; when the preset feeding time is reached, taking a molten aluminum amalgam sample from a sampling port of the reaction furnace 8, detecting components in the molten aluminum amalgam sample, and taking a sample at intervals until the mercury content reaches the requirement; if the components meet the requirements, stopping heating the evaporator 3, closing the valve of the first pipeline 5, opening the valve of the third pipeline 7, enabling the inert gas to directly enter the feeding pipe, and maintaining to convey clean and high-temperature inert gas for 3-5 minutes until the liquid level of the aluminum soup is reduced to be out of contact with the feeding pipe;
In the embodiment, the inert gas is always introduced into the hearth through the material introducing pipe in the aluminum discharging process;
And step eleven, when the temperature of the aluminum outlet reaches over 660 ℃, the aluminum amalgam prepared in the reaction furnace 8 is emptied, cast and molded, and the preparation work of the hydrogen production material is finished.
The embodiment discloses a preparation method of an aluminum amalgam for mercury conveying by bubbling inert gas, which adopts inert gas as shielding gas, heats mercury to form mercury vapor through an evaporator 3, and then introduces the mercury vapor into aluminum soup through a second pipeline 6 and a feed-through pipe with the lower end inserted below the liquid level of a reaction furnace 8, and diffuses the carried mercury vapor into the aluminum soup in a bubbling mode to complete the preparation of the aluminum amalgam. Because mercury enters the molten aluminum soup in a vapor form, the whole process is safe and controllable, and the phenomenon of mercury explosion can not occur. In the embodiment, under the dual actions of bubbling and stirring, the aluminum amalgam with relatively uniform components can be obtained.
In this example, the inert gas used was a gas which was stable at 700℃or lower and hardly reacted with aluminum. The inert gas is nitrogen or inert gas.
In this embodiment, the rated operating temperatures of the preheater 2, the evaporator 3 and the heater of the second line 6 are all set above the boiling point of the mercury feed.
In this embodiment, the second pipeline 6 is a seamless pipe made of 310S or 316L material.
In this embodiment, the first pipeline 5, the second pipeline 6 and the third pipeline 7 are all provided with heaters, and the heaters are cast copper heating rings or ceramic heating rings.
In this embodiment, the material pipe is made of a material which is resistant to temperature not lower than 700 ℃ and is not easily corroded by aluminum water, and preferably graphite. The lower end of the feeding pipe is positioned below the liquid level of the aluminum soup and is 1cm away from the bottom of the hearth. The lower extreme of feed-through pipe is provided with the opening, has offered a plurality of through-holes on the lateral wall of the lower part of feed-through pipe.
The principles and embodiments of the present invention have been described in this specification with reference to specific examples, the description of which is only for the purpose of aiding in understanding the method of the present invention and its core ideas; also, it is within the scope of the present invention to be modified by those of ordinary skill in the art in light of the present teachings. In view of the foregoing, this description should not be construed as limiting the invention.

Claims (8)

1.一种不活泼气体鼓泡式输汞的铝汞合金制备方法，其特征在于：包括以下步骤：1. A method for preparing aluminum-mercury alloy by inert gas bubbling mercury infusion, characterized in that it comprises the following steps: 步骤一，搭建鼓泡式输汞铝汞合金制备装置；Step 1: construct a bubbling type mercury-infusion aluminum-mercury alloy preparation device; 步骤二，根据反应炉一次投放铝的质量计算出所需汞原料的量，并根据制备时间要求，计算出输送汞所需不活泼气体的量和流量；Step 2: Calculate the amount of mercury raw material required according to the mass of aluminum put into the reactor at one time, and calculate the amount and flow rate of inactive gas required for transporting mercury according to the preparation time requirement; 步骤三，将称量好的铝投入熔炼炉中进行熔化；Step 3, putting the weighed aluminum into a smelting furnace for melting; 步骤四，将称量好的汞原料投入到蒸发器中，并检查蒸发器到反应炉第二管路的气密性；Step 4, putting the weighed mercury raw material into the evaporator, and checking the air tightness of the second pipeline from the evaporator to the reactor; 步骤五，开启不活泼气体直通反应炉的第三管路上的阀门，吹除第三管路中空气后暂时关闭不活泼气体直通反应炉的第三管路；Step 5, opening the valve on the third pipeline of the inert gas direct-flow reactor, blowing out the air in the third pipeline and temporarily closing the third pipeline of the inert gas direct-flow reactor; 步骤六，铝熔化后，对其去除表面氧化渣后，将熔融状态下的铝转移到反应炉中；Step 6: After the aluminum is melted, the surface oxide slag is removed and the molten aluminum is transferred to a reaction furnace; 步骤七，在反应炉中对转入的熔融状态的铝进行保温，使得反应炉的炉膛内部温度均处于铝的熔点以上，开启反应炉的搅拌结构，使沉在反应炉的炉膛底部的氧化渣上浮至表面，再进行表面的扒渣处理；Step 7: Insulate the molten aluminum in the reactor so that the temperature inside the furnace of the reactor is above the melting point of aluminum, start the stirring mechanism of the reactor to make the slag at the bottom of the furnace float to the surface, and then perform slag removal on the surface; 步骤八，开启第一管路上的预热器对第一管路进行加热，同时开启第二管路的加热器对第二管路进行升温、保温，开启蒸发器对汞原料进行加热；Step eight, turning on the preheater on the first pipeline to heat the first pipeline, turning on the heater on the second pipeline to heat and keep the second pipeline warm, and turning on the evaporator to heat the mercury raw material; 步骤九，完成扒渣，且蒸发器温度达到额定值后，使得不活泼气体依次经过预热器和蒸发器，带有汞蒸汽的不活泼气体经过反应炉的通料管进入反应炉的炉膛的熔融状态的铝中；Step nine, after the slagging is completed and the evaporator temperature reaches the rated value, the inactive gas is passed through the preheater and the evaporator in sequence, and the inactive gas with mercury vapor enters the molten aluminum in the furnace of the reaction furnace through the feed pipe of the reaction furnace; 步骤十，当达到预定投料时间后，从反应炉取样口取熔融铝汞合金样品，检测其中组分；如果组分达到要求，则停止蒸发器加热并将第一管路的阀门关闭，打开第三管路的阀门，使不活泼气体直接进入通料管，维持输送干净、高温的不活泼气体一段时间；Step 10, when the predetermined feeding time is reached, a molten aluminum-mercury alloy sample is taken from the sampling port of the reaction furnace to detect the components therein; if the components meet the requirements, the evaporator heating is stopped and the valve of the first pipeline is closed, and the valve of the third pipeline is opened to allow the inactive gas to directly enter the feed pipe, and the clean, high-temperature inactive gas is transported for a period of time; 步骤十一，将反应炉中制取完成的铝汞合金放空浇铸成型，结束制氢材料的制取工作；Step 11, emptying the aluminum-mercury alloy prepared in the reaction furnace and casting it to complete the preparation of hydrogen production materials; 所述鼓泡式输汞铝汞合金制备装置包括不活泼气体存储结构、预热器、蒸发器、熔炼炉和反应炉，所述不活泼气体存储结构用于存储不活泼气体，所述蒸发器用于加热汞原料，所述熔炼炉用于熔炼铝，所述不活泼气体存储结构通过第一管路与所述预热器连接，所述预热器通过第一管路与所述蒸发器连接，所述蒸发器通过第二管路与所述反应炉的通料管连接，所述预热器通过第三管路与所述反应炉的通料管连接，所述熔炼炉与所述反应炉的进料口连接；The bubbling type mercury-injection aluminum-mercury alloy preparation device comprises an inert gas storage structure, a preheater, an evaporator, a smelting furnace and a reaction furnace, wherein the inert gas storage structure is used to store inert gas, the evaporator is used to heat mercury raw materials, the smelting furnace is used to smelt aluminum, the inert gas storage structure is connected to the preheater through a first pipeline, the preheater is connected to the evaporator through a first pipeline, the evaporator is connected to the feed pipe of the reaction furnace through a second pipeline, the preheater is connected to the feed pipe of the reaction furnace through a third pipeline, and the smelting furnace is connected to the feed inlet of the reaction furnace; 所述第一管路、所述第二管路和所述第三管路上均设置有加热器，所述加热器为铸铜加热圈或陶瓷加热圈。The first pipeline, the second pipeline and the third pipeline are all provided with heaters, and the heaters are cast copper heating coils or ceramic heating coils. 2.根据权利要求1所述的不活泼气体鼓泡式输汞的铝汞合金制备方法，其特征在于：所述步骤二中，所述汞原料为纯汞或含汞汞齐。2. The method for preparing aluminum-mercury alloy by inert gas bubbling mercury injection according to claim 1, characterized in that: in the step 2, the mercury raw material is pure mercury or mercury-containing amalgam. 3.根据权利要求1所述的不活泼气体鼓泡式输汞的铝汞合金制备方法，其特征在于：采用的所述不活泼气体为700℃以下性质稳定且不易与铝反应的气体。3. The method for preparing aluminum-mercury alloy by inert gas bubbling mercury injection according to claim 1, characterized in that the inert gas used is a gas that is stable at a temperature below 700°C and does not easily react with aluminum. 4.根据权利要求3所述的不活泼气体鼓泡式输汞的铝汞合金制备方法，其特征在于：采用的所述不活泼气体为氮气或惰性气体。4. The method for preparing aluminum-mercury alloy by inert gas bubbling mercury infusion according to claim 3, characterized in that the inert gas used is nitrogen or an inert gas. 5.根据权利要求1所述的不活泼气体鼓泡式输汞的铝汞合金制备方法，其特征在于：所述预热器、所述蒸发器以及所述第二管路的加热器的额定工作温度均设置在汞原料的沸点以上。5. The method for preparing aluminum-mercury alloy by inert gas bubbling mercury injection according to claim 1, characterized in that the rated operating temperatures of the preheater, the evaporator and the heater of the second pipeline are all set above the boiling point of the mercury raw material. 6.根据权利要求1所述的不活泼气体鼓泡式输汞的铝汞合金制备方法，其特征在于：所述第二管路为采用310S或为316L材质制成的无缝管。6. The method for preparing aluminum-mercury alloy by inert gas bubbling mercury infusion according to claim 1, characterized in that the second pipeline is a seamless pipe made of 310S or 316L material. 7.根据权利要求1所述的不活泼气体鼓泡式输汞的铝汞合金制备方法，其特征在于：所述通料管采用耐温不低于700℃且不易被铝水侵蚀的材质制成。7. The method for preparing aluminum-mercury alloy by inert gas bubbling mercury infusion according to claim 1, characterized in that the feed pipe is made of a material that can withstand a temperature of not less than 700°C and is not easily corroded by aluminum liquid. 8.根据权利要求1所述的不活泼气体鼓泡式输汞的铝汞合金制备方法，其特征在于：所述通料管的下端设置有开口，所述通料管的下部的侧壁上开设有多个通孔；所述通料管的下端位于铝汤的液面以下且距离炉膛的底部1cm。8. The method for preparing aluminum-mercury alloy by inert gas bubbling mercury infusion according to claim 1 is characterized in that: the lower end of the feed tube is provided with an opening, and a plurality of through holes are opened on the side wall of the lower part of the feed tube; the lower end of the feed tube is located below the liquid level of the aluminum soup and 1 cm away from the bottom of the furnace.
CN202211531499.XA 2022-12-01 2022-12-01 Preparation method of aluminum amalgam for inactive gas bubbling type mercury delivery Expired - Fee Related CN115852182B (en)

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CN108310955A (en) * 2018-01-30 2018-07-24 湖南西林环保材料有限公司 A method of mercury is recycled in situ from non-ferrous metal metallurgy mercury fume

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB757908A (en) * 1952-06-24 1956-09-26 Reynolds Metals Co Process for producing aluminium electrolytically by amalgam metallurgy
CN201140277Y (en) * 2007-12-10 2008-10-29 扬州市邗江天和电子厂 Mercury pellet preparation device
CN106744679A (en) * 2016-12-29 2017-05-31 云南靖创液态金属热控技术研发有限公司 Hydrogen production process and mechanism
CN108310955A (en) * 2018-01-30 2018-07-24 湖南西林环保材料有限公司 A method of mercury is recycled in situ from non-ferrous metal metallurgy mercury fume

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