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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aluminum
mercury
pipeline
inert gas
reaction furnace
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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. The preparation method of the aluminum amalgam for the inert gas bubbling type mercury delivery is characterized by comprising the following steps of: the method 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;
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;
The bubbling type mercury-conveying aluminum amalgam preparation device 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 material passing pipe of the reaction furnace through a second pipeline, the preheater is connected with a material passing pipe of the reaction furnace through a third pipeline, and the smelting furnace is connected with a material feeding port of the reaction furnace;
heaters are arranged on the first pipeline, the second pipeline and the third pipeline, and the heaters are cast copper heating rings or ceramic heating rings.
2. The method for preparing the aluminum amalgam for inert gas bubbling mercury delivery according to claim 1, wherein the method comprises the following steps: in the second step, the mercury raw material is pure mercury or mercury-containing amalgam.
3. The method for preparing the aluminum amalgam for inert gas bubbling mercury delivery according to claim 1, wherein the method comprises the following steps: the inert gas used is a gas which is stable in properties below 700 ℃ and is not easy to react with aluminum.
4. The method for preparing the aluminum amalgam for inert gas bubbling mercury delivery according to claim 3, wherein the method comprises the following steps: the inert gas is nitrogen or inert gas.
5. The method for preparing the aluminum amalgam for inert gas bubbling mercury delivery according to claim 1, wherein the method comprises the following steps: 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. The method for preparing the aluminum amalgam for inert gas bubbling mercury delivery according to claim 1, wherein the method comprises the following steps: the second pipeline is a seamless pipe made of 310S or 316L materials.
7. The method for preparing the aluminum amalgam for inert gas bubbling mercury delivery according to claim 1, wherein the method comprises the following steps: 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 molten aluminum.
8. The method for preparing the aluminum amalgam for inert gas bubbling mercury delivery according to claim 1, wherein the method comprises the following steps: 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.
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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 Apparatus for producing blue pills
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

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 Apparatus for producing blue pills
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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