CN110589860A - Full-automatic preparation process of anhydrous aluminum trichloride - Google Patents

Full-automatic preparation process of anhydrous aluminum trichloride Download PDF

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Publication number
CN110589860A
CN110589860A CN201910971462.0A CN201910971462A CN110589860A CN 110589860 A CN110589860 A CN 110589860A CN 201910971462 A CN201910971462 A CN 201910971462A CN 110589860 A CN110589860 A CN 110589860A
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China
Prior art keywords
aluminum
anhydrous
trichloride
chlorine
aluminum trichloride
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CN201910971462.0A
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Chinese (zh)
Inventor
安小晖
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Jiangsu Sea Chemical Co Ltd
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Jiangsu Sea Chemical Co Ltd
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Priority to CN201910971462.0A priority Critical patent/CN110589860A/en
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00Compounds of aluminium
    • C01F7/48Halides, with or without other cations besides aluminium
    • C01F7/56Chlorides
    • C01F7/58Preparation of anhydrous aluminium chloride

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

The invention discloses a full-automatic anhydrous aluminum trichloride preparation process, relates to the technical field of anhydrous aluminum trichloride preparation, and aims to solve the problems that the conventional aluminum ingot method for producing anhydrous aluminum trichloride adopts metallic aluminum as a raw material, the production cost is relatively high, and mixed aluminum is adopted as the raw material, so that the cost can be reduced, but impurities in the raw material can reduce the product quality. Step 1: pouring the recovered aluminum scraps into cleaning equipment, and intensively cleaning to remove impurities on the surfaces of the aluminum scraps; step 2: the waste aluminum after cleaning and oil removal is classified into three types, namely pure aluminum, aluminum alloy and mixture according to the properties of the waste aluminum; and step 3: crushing the aluminum alloy and the mixture by using a crusher and then purifying; and 4, step 4: preheating the purified aluminum material, adding the aluminum material into a closed chlorination reaction furnace, introducing chlorine, and reacting the chlorine and the aluminum material at 800 ℃ to generate anhydrous aluminum trichloride gas.

Description

Full-automatic preparation process of anhydrous aluminum trichloride
Technical Field
The invention relates to the technical field of anhydrous aluminum trichloride preparation, in particular to a full-automatic anhydrous aluminum trichloride preparation process.
Background
Anhydrous aluminum trichloride is an important inorganic chemical raw material, and is mainly used for preparing alkylating agents of detergents, synthetic drugs, synthetic dyes, synthetic rubbers, detergents, plastics, spices and the like. At the same time, the anhydrous aluminum trichloride is also an important catalyst, and is particularly widely applied as a catalyst of the Friedel-crafts reaction. In addition, the anhydrous aluminum trichloride is expected to be used for producing metal aluminum, and has great potential in the aspects of energy conservation, emission reduction and greenhouse gas emission reduction if the anhydrous aluminum trichloride is used as a raw material for aluminum electrolysis.
However, the conventional aluminum ingot method for producing anhydrous aluminum trichloride adopts metal aluminum as a raw material, so that the production cost is relatively high, while the mixed aluminum is adopted as the raw material, although the cost can be reduced, impurities in the raw material can reduce the product quality; therefore, the existing requirements are not met, and a full-automatic anhydrous aluminum trichloride preparation process is provided for the requirements.
Disclosure of Invention
The invention aims to provide a full-automatic preparation process of anhydrous aluminum trichloride, which aims to solve the problems that the existing aluminum ingot method for producing anhydrous aluminum trichloride in the background art adopts metallic aluminum as a raw material, the production cost is relatively high, and mixed aluminum is adopted as the raw material, although the cost can be reduced, the impurity in the raw material can reduce the product quality.
In order to achieve the purpose, the invention provides the following technical scheme: a full-automatic preparation process of anhydrous aluminum trichloride comprises the following steps:
step 1: pouring the recovered aluminum scraps into cleaning equipment, and intensively cleaning to remove impurities on the surfaces of the aluminum scraps;
step 2: the waste aluminum after cleaning and oil removal is classified into three types, namely pure aluminum, aluminum alloy and mixture according to the properties of the waste aluminum;
and step 3: crushing the aluminum alloy and the mixture by using a crusher and then purifying;
and 4, step 4: preheating the purified aluminum material, adding the aluminum material into a closed chlorination reaction furnace, introducing chlorine, and reacting the chlorine and the aluminum material at 800 ℃ to generate anhydrous aluminum trichloride gas;
and 5: when the temperature of the gas-phase product anhydrous aluminum trichloride reaches 400 ℃, a condenser is used for capturing the anhydrous aluminum trichloride to obtain anhydrous aluminum trichloride;
step 6: and (3) washing and absorbing the residual tail gas by using dilute alkali or lime milk, and then emptying.
Preferably, the cleaning step in the step 1 can effectively remove oil stains on the surface of the waste aluminum impurities, so that the cleanliness of the surface of the filter material is ensured, twenty percent of impurities can enter slag in the waste aluminum impurities which are not completely removed, and the purity of the anhydrous aluminum trichloride production is influenced.
Preferably, in the step 2, the pure aluminum is aluminum with the purity of 98.8-99.7%; the aluminum alloy is an alloy of which the melting point of a fusant is larger than that of aluminum, such as iron-aluminum alloy and copper-aluminum alloy; the mixture is an aluminum workpiece or connecting piece which is connected by other materials and is difficult to normally remove.
Preferably, the aluminum alloy in the step 3 is crushed into fine particles by a crusher, and then melted by a melting furnace, and the melting temperature of the melting furnace is controlled to be 650 ℃ to 700 ℃, because the melting point of aluminum is 660 ℃, which is low in metals, and the melting points of metals such as iron and copper are above 1000 ℃, only aluminum in the alloy is melted after temperature control, so that the aluminum can be collected.
Preferably, after the mixture in the step 3 is crushed into fine particles by a crusher, an aluminum magnetic separator needs to be used for magnetic separation to extract the aluminum material therein.
Preferably, the chlorine gas in the step 4 is formed by heating and gasifying chlorine liquid, and is metered by a buffer and a flow tube and then added into the chlorination reaction furnace.
Preferably, the introduction amount of chlorine in the step 4 is difficult to control, the content of chlorine tail gas affects the color of the product, and as the content of the tail gas is reduced, the anhydrous aluminum trichloride can form a color change process of orange, withered yellow, light yellow, white and light gray, wherein the yellow, light yellow and white are fine products, so that the introduction amount of chlorine only needs to control the anhydrous aluminum trichloride in the three color states.
Preferably, the reaction equation of the chlorine gas and the aluminum material in the step 4 is 2AL +3CL2=2ALCL3
Compared with the prior art, the invention has the beneficial effects that:
1. according to the invention, the recovered aluminum scraps are cleaned, classified, crushed and purified, the oil stains on the surface of the aluminum scraps can be effectively removed through cleaning, the cleanliness of the surface of the aluminum materials is ensured, the quality of finished products is improved, the cleaned aluminum materials are classified and then purified by adopting two modes of melting or magnetic absorption according to the properties of the aluminum materials, the anhydrous aluminum trichloride is prepared by adopting the purified aluminum materials, the impurities are few, the quality of products can be ensured, the crusher, the magnetic separator and the smelting furnace used in the purification process are disposable, the anhydrous aluminum trichloride can be used for a long time, high aluminum metal is not required to be purchased as a production raw material of the anhydrous aluminum trichloride, and the recovered aluminum scraps can be used for preparing the anhydrous aluminum trichloride with qualified quality.
2. The anhydrous aluminum trichloride is prepared by adopting a closed chlorination reaction furnace and a condenser, the purified aluminum material is preheated and then added into the closed chlorination reaction furnace, chlorine is introduced to directly react, the chlorine is formed by heating chlorine liquid through a gasifier, the chlorine is measured through a buffer and a flow tube and then added into the chlorination reaction furnace, and the aluminum trichloride gas after the reaction is collected by the condenser, so that the anhydrous aluminum trichloride is obtained.
Drawings
FIG. 1 is a flow chart of the present invention;
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
Referring to fig. 1, an embodiment of the present invention: a full-automatic preparation process of anhydrous aluminum trichloride comprises the following steps:
step 1: pouring the recovered aluminum scraps into cleaning equipment, and intensively cleaning to remove impurities on the surfaces of the aluminum scraps;
step 2: the waste aluminum after cleaning and oil removal is classified into three types, namely pure aluminum, aluminum alloy and mixture according to the properties of the waste aluminum;
and step 3: crushing the aluminum alloy and the mixture by using a crusher and then purifying;
and 4, step 4: preheating the purified aluminum material, adding the aluminum material into a closed chlorination reaction furnace, introducing chlorine, and reacting the chlorine and the aluminum material at 800 ℃ to generate anhydrous aluminum trichloride gas;
and 5: when the temperature of the gas-phase product anhydrous aluminum trichloride reaches 400 ℃, a condenser is used for capturing the anhydrous aluminum trichloride to obtain anhydrous aluminum trichloride;
step 6: and (3) washing and absorbing the residual tail gas by using dilute alkali or lime milk, and then emptying.
Furthermore, the cleaning step in the step 1 can effectively remove oil stains on the surface of the waste aluminum impurities, the cleanliness of the surface of the filter material is ensured, twenty percent of impurities can enter slag at most when the waste aluminum impurities are not completely removed, and therefore the purity of the anhydrous aluminum trichloride production is influenced.
Further, in the step 2, the pure aluminum is aluminum with the purity of 98.8-99.7%; the aluminum alloy is an alloy of which the melting point of a fusant is larger than that of aluminum, such as iron-aluminum alloy and copper-aluminum alloy; the mixture is an aluminum workpiece or connecting piece which is connected by other materials and is difficult to normally remove.
Further, after the aluminum alloy in the step 3 is crushed into fine particles by the crusher, the aluminum alloy needs to be melted by a melting furnace, the temperature of the melting furnace is controlled to be 650 ℃ to 700 ℃, the melting point of the aluminum is 660 ℃, the melting point of the aluminum is low in the metal, and the melting points of the metals such as iron and copper are all above 1000 ℃, so that only the aluminum in the alloy can be melted after temperature control, and the aluminum can be collected.
Further, after the mixture in the step 3 is crushed into fine particles by a crusher, an aluminum material in the mixture needs to be extracted by a magnetic separation mode of an aluminum magnetic separator.
Further, the chlorine gas in the step 4 is formed by heating chlorine liquid and then gasifying the chlorine liquid, and the chlorine gas is metered by a buffer and a flow tube and then added into a chlorination reaction furnace.
Furthermore, the introduction amount of chlorine in the step 4 is difficult to control, the content of chlorine tail gas influences the color of the product, and as the content of the tail gas is reduced, the anhydrous aluminum trichloride can form a color change process of orange, withered yellow, light yellow, white and light gray, wherein the yellow, light yellow and white are fine products, so that the introduction amount of the chlorine only needs to control the anhydrous aluminum trichloride in the three color states.
Further, the reaction equation of the chlorine gas and the aluminum material in the step 4 is as follows: 2AL +3CL2=2ALCL3
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.

Claims (8)

1. A full-automatic preparation anhydrous aluminum trichloride process is characterized in that: the method comprises the following steps:
step 1: pouring the recovered aluminum scraps into cleaning equipment, and intensively cleaning to remove impurities on the surfaces of the aluminum scraps;
step 2: the waste aluminum after cleaning and oil removal is classified into three types, namely pure aluminum, aluminum alloy and mixture according to the properties of the waste aluminum;
and step 3: crushing the aluminum alloy and the mixture by using a crusher and then purifying;
and 4, step 4: preheating the purified aluminum material, adding the aluminum material into a closed chlorination reaction furnace, introducing chlorine, and reacting the chlorine and the aluminum material at 800 ℃ to generate anhydrous aluminum trichloride gas;
and 5: when the temperature of the gas-phase product anhydrous aluminum trichloride reaches 400 ℃, a condenser is used for capturing the anhydrous aluminum trichloride to obtain anhydrous aluminum trichloride;
step 6: and (3) washing and absorbing the residual tail gas by using dilute alkali or lime milk, and then emptying.
2. The full-automatic preparation process of anhydrous aluminum trichloride as claimed in claim 1, which is characterized in that: the cleaning step in the step 1 can effectively remove oil stains on the surface of the waste aluminum impurities, the cleanliness of the surface of the filter material is ensured, twenty percent of impurities can enter slag at most when the waste aluminum impurities are not completely removed, and therefore the purity of the anhydrous aluminum trichloride production is influenced.
3. The full-automatic preparation process of anhydrous aluminum trichloride as claimed in claim 1, which is characterized in that: in the step 2, the pure aluminum is aluminum with the purity of 98.8-99.7%; the aluminum alloy is an alloy of which the melting point of a fusant is larger than that of aluminum, such as iron-aluminum alloy and copper-aluminum alloy; the mixture is an aluminum workpiece or connecting piece which is connected by other materials and is difficult to normally remove.
4. The full-automatic preparation process of anhydrous aluminum trichloride as claimed in claim 1, which is characterized in that: after the aluminum alloy in the step 3 is crushed into fine particles by the crusher, the aluminum alloy needs to be melted by a melting furnace, the temperature of the melting furnace is controlled to be 650-700 ℃, the melting point of the aluminum is 660 ℃, so that the aluminum is low in the metal, the melting points of the iron, copper and other metals are above 1000 ℃, and only the aluminum in the alloy is melted after temperature control, so that the aluminum can be collected.
5. The full-automatic preparation process of anhydrous aluminum trichloride as claimed in claim 1, which is characterized in that: after the mixture in the step 3 is crushed into fine particles by the crusher, an aluminum material in the mixture needs to be extracted by a magnetic separation mode of an aluminum magnetic separator.
6. The full-automatic preparation process of anhydrous aluminum trichloride as claimed in claim 1, which is characterized in that: and (4) heating the chlorine liquid and then gasifying the chlorine gas to form chlorine gas, metering the chlorine gas by a buffer and a flow tube, and adding the chlorine gas into the chlorination reaction furnace.
7. The full-automatic preparation process of anhydrous aluminum trichloride as claimed in claim 1, which is characterized in that: in the step 4, the introduction amount of chlorine is difficult to control, the content of chlorine tail gas influences the color of the product, and as the content of the tail gas is reduced, the anhydrous aluminum trichloride can form a color change process of orange, withered yellow, light yellow, white and light gray, wherein the yellow, light yellow and white are fine products, so that the introduction amount of the chlorine only needs to control the anhydrous aluminum trichloride in the three color states.
8. The method of claim 1A full-automatic preparation anhydrous aluminum trichloride process is characterized in that: the reaction equation of the chlorine gas and the aluminum material in the step 4 is 2AL +3CL2=2ALCL3
CN201910971462.0A 2019-10-14 2019-10-14 Full-automatic preparation process of anhydrous aluminum trichloride Pending CN110589860A (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102352439A (en) * 2011-07-18 2012-02-15 株洲冶炼集团股份有限公司 Method of producing zinc chloride and aluminum chloride by using waste zinc-aluminum alloy
CN104402032A (en) * 2014-11-17 2015-03-11 宁夏中远天宇科技有限公司 Production method for novel anhydrous aluminum trichloride

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102352439A (en) * 2011-07-18 2012-02-15 株洲冶炼集团股份有限公司 Method of producing zinc chloride and aluminum chloride by using waste zinc-aluminum alloy
CN104402032A (en) * 2014-11-17 2015-03-11 宁夏中远天宇科技有限公司 Production method for novel anhydrous aluminum trichloride

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
J.A.奥里蒙等: "《逸散性工业粉尘控制技术》", 31 December 1989 *
闫曙光等: "工业无水三氯化铝的制备及其产品质量的控制", 《内蒙古石油化工》 *

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Application publication date: 20191220