CN113697835A - Method for extracting aluminum fluoride from silicon dioxide slag - Google Patents

Method for extracting aluminum fluoride from silicon dioxide slag Download PDF

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CN113697835A
CN113697835A CN202110009472.3A CN202110009472A CN113697835A CN 113697835 A CN113697835 A CN 113697835A CN 202110009472 A CN202110009472 A CN 202110009472A CN 113697835 A CN113697835 A CN 113697835A
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aluminum fluoride
silicon dioxide
mother liquor
filter cake
dioxide slag
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蔡从美
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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
    • C01F7/50Fluorides
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/113Silicon oxides; Hydrates thereof
    • C01B33/12Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/10Solid density
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/80Compositional purity

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  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
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  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
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Abstract

The invention discloses a method for extracting aluminum fluoride from silicon dioxide slag, which comprises the following steps: the method comprises the following steps: crystallizing and filtering the aluminum fluoride solution to obtain aluminum fluoride mother liquor; step two: circularly washing the silicon dioxide slag for 8-12 minutes by using aluminum fluoride mother liquor under stirring; step three: filtering the washed silicon dioxide slag and aluminum fluoride mother liquor by using a vacuum filter to obtain 1.15-1.28L of aluminum fluoride filtrate and a silicon dioxide filter cake; step four: crystallizing the aluminum fluoride filtrate at the temperature of 92-98 ℃, and filtering to obtain an aluminum fluoride filter cake; step five: drying the aluminum fluoride filter cake at the temperature of 102-108 ℃, calcining the dried aluminum fluoride filter cake to lose crystal water, and cooling to obtain 74-83 g of aluminum fluoride, wherein the aluminum fluoride filter cake has the advantages that: the loss of aluminum fluoride in the silicon dioxide slag is reduced, the loss is reduced, the pollution to the environment is obviously reduced, and the yield of the aluminum fluoride is improved.

Description

Method for extracting aluminum fluoride from silicon dioxide slag
Technical Field
The invention relates to the technical field of aluminum fluoride extraction methods, in particular to the technical field of a method for extracting aluminum fluoride from silicon dioxide slag generated by fluosilicic acid and aluminum hydroxide.
Background
Aluminum fluoride is mainly used in aluminum production, and has the functions of lowering the melting point and improving the conductivity of electrolyte. At present, the production methods of aluminum fluoride are largely divided into two types: one is the refined acid dry method used by the metallurgical industry till now, the method uses sulfuric acid to decompose fluorite to generate hydrofluoric acid, and then the hydrofluoric acid reacts with aluminum hydroxide to prepare aluminum fluoride; the other is fluorosilicic acid process, which uses fluorosilicic acid as by-product in acid process of phosphate fertilizer industry to react with aluminium hydroxide to obtain aluminium fluoride solution, which is then crystallized, filtered, dried, calcined and cooled to obtain aluminium fluoride product. The production process of the aluminum fluoride by the fluosilicic acid method has the advantages that the used main raw material fluosilicic acid is derived from a byproduct in phosphate fertilizer production, the production cost is very low, and the product quality is good, so that the aluminum fluoride product produced by the fluosilicic acid method has strong competitiveness in the market by virtue of the absolute advantage of the price. In the production process of producing aluminum fluoride by a fluorosilicic acid method, after fluosilicic acid reacts with aluminum hydroxide, solid matters obtained after filtration and liquid-solid separation are silicon dioxide slag, and at present, the silicon dioxide slag generated by the fluorosilicic acid method is directly discarded. However, the water content of the silicon dioxide slag is larger than 50%, so that 5% of aluminum fluoride is lost, the loss is large, and secondary pollution is easily caused.
Disclosure of Invention
The invention aims to solve the defects and provide a method for extracting aluminum fluoride from silicon dioxide slag, which can recover the aluminum fluoride in the silicon dioxide slag, improve the yield of the aluminum fluoride, reduce the production cost and achieve the maximum benefit utilization.
The technical solution adopted by the present invention to solve the above technical problems is as follows:
a method for extracting aluminum fluoride from silicon dioxide slag comprises the following steps:
the method comprises the following steps: filtering a product obtained after reaction of fluosilicic acid and aluminum hydroxide to obtain an aluminum fluoride solution and silicon dioxide slag, and crystallizing and filtering the aluminum fluoride solution to obtain an aluminum fluoride mother liquor;
step two: taking 2.3-2.7 kg of silicon dioxide slag according to the weight ratio, taking 0.8-1.2L of aluminum fluoride mother liquor according to the volume ratio, adding the aluminum fluoride mother liquor into the silicon dioxide slag, and circularly washing the silicon dioxide slag for 8-12 minutes through the aluminum fluoride mother liquor under stirring;
step three: filtering the washed silicon dioxide slag and aluminum fluoride mother liquor by using a vacuum filter to obtain 1.15-1.28L of aluminum fluoride filtrate and a silicon dioxide filter cake;
step four: feeding the aluminum fluoride filtrate obtained in the third step into a crystallization tank, crystallizing at the temperature of 92-98 ℃ for 3.8-4.2 hours, and filtering to obtain 122-136 g of an aluminum fluoride filter cake;
step five: and drying the aluminum fluoride filter cake obtained in the fourth step at the temperature of 102-108 ℃ to reduce the weight of the aluminum fluoride filter cake by 39.3-39.62%, calcining the dried aluminum fluoride filter cake to lose crystal water, and cooling to obtain 74-83 g of aluminum fluoride.
Preferably, in the second step, 2.5kg of silicon dioxide slag is taken according to the weight ratio, 1L of aluminum fluoride mother liquor is taken according to the volume ratio, the aluminum fluoride mother liquor is added into the silicon dioxide slag, and the silicon dioxide slag is circularly washed for 10 minutes through the aluminum fluoride mother liquor under stirring; in the third step, the washed silicon dioxide slag and the aluminum fluoride mother liquor are filtered by a vacuum filter to obtain 1.2L of aluminum fluoride filtrate; in the fourth step, the aluminum fluoride filtrate obtained in the third step is sent into a crystallization tank, crystallized for 4 hours at the temperature of 95 ℃, and then filtered to obtain 127g of an aluminum fluoride filter cake; in the fifth step, the aluminum fluoride filter cake obtained in the fourth step is dried at a temperature of 105 ℃ so that the weight of the aluminum fluoride filter cake is reduced by 39.4%, then the dried aluminum fluoride filter cake is calcined to lose crystal water, and 78.4g of aluminum fluoride is obtained after cooling.
The invention adopts the technical proposal to achieve the following beneficial effects: according to the method, the aluminum fluoride mother liquor is used for washing, filtering, crystallizing, drying, calcining and the like of the silicon dioxide slag, so that high-quality aluminum fluoride is extracted from the silicon dioxide slag, the loss of the aluminum fluoride in the silicon dioxide slag is greatly reduced, the loss is reduced, the pollution to the environment is remarkably reduced, and the yield of the aluminum fluoride is improved; and because the aluminum fluoride mother liquor used for extracting the aluminum fluoride is a byproduct generated in the process of producing the aluminum fluoride by the fluosilicic acid and the aluminum hydroxide, the production cost is extremely low, and the benefit maximization is realized. Meanwhile, the aluminum fluoride mother liquor is used for washing without introducing other impurities, so that the finally extracted aluminum fluoride has low impurity content and high quality. The filtrate of aluminum fluoride after crystallization contains F in comparison with the mother liquor of aluminum fluoride-And Al3+The content is reduced, which indicates that a part of aluminum fluoride in the aluminum fluoride mother liquor is separated out, so the method of the invention also extracts the aluminum fluoride in the aluminum fluoride mother liquor, thereby further improving the yield of the aluminum fluoride, reducing the cost and realizing the maximization of the benefitAnd (4) utilizing.
Detailed Description
Example 1: a method for extracting aluminum fluoride from silicon dioxide slag comprises the following steps:
the method comprises the following steps: filtering a product obtained after reaction of fluosilicic acid and aluminum hydroxide to obtain an aluminum fluoride solution and silicon dioxide slag, and crystallizing and filtering the aluminum fluoride solution to obtain an aluminum fluoride mother liquor;
step two: taking 2.3kg of silicon dioxide slag according to the weight ratio, taking 0.8L of aluminum fluoride mother liquor according to the volume ratio, adding the aluminum fluoride mother liquor into the silicon dioxide slag, and circularly washing the silicon dioxide slag for 8 minutes through the aluminum fluoride mother liquor under stirring;
step three: filtering the washed silicon dioxide slag and aluminum fluoride mother liquor by using a vacuum filter to obtain 1.15L of aluminum fluoride filtrate and a silicon dioxide filter cake;
step four: feeding the aluminum fluoride filtrate obtained in the third step into a crystallization tank, crystallizing at the temperature of 92 ℃ for 3.8 hours, and filtering to obtain 122g of an aluminum fluoride filter cake;
step five: and drying the aluminum fluoride filter cake obtained in the fourth step at the temperature of 102 ℃ to reduce the weight of the aluminum fluoride filter cake by 39.3%, calcining the dried aluminum fluoride filter cake to lose crystal water, and cooling to obtain 74g of aluminum fluoride.
The following table is a comparison table of the content change of some components in this example:
Figure BDA0002884681680000041
as can be seen from the above table, F after washing-The content of Al in the aluminum fluoride mother liquor is changed from 4.28g/L in the aluminum fluoride mother liquor to 7.72g/L in the aluminum fluoride filtrate3+The content of the aluminum fluoride is 31.24g/L in the aluminum fluoride filtrate from 17.56g/L in the aluminum fluoride mother liquor, which shows that aluminum fluoride in the silicon dioxide slag is largely washed out after washing; the filtrate of aluminium fluoride after crystallization is compared with mother liquor of aluminium fluoride, F-The content of Al is reduced from 4.28g/L to 4.16g/L3+The content of (b) is reduced from 17.56g/L to 12.68g/L, which shows that a part of fluorine is also contained in the aluminum fluoride mother liquorAluminum fluoride is precipitated, so that aluminum fluoride in the aluminum fluoride mother liquor is also extracted by the method of the embodiment; the weight of the calcined aluminum fluoride was 74g, and it was demonstrated that 74g of aluminum fluoride was finally extracted from 2.3kg of silica fume by the method of this example, and F was contained in the extracted aluminum fluoride-Up to 64.81% of Al3+Up to 31.75% of SiO2In an amount of as low as 0.12%, P2O5The content of (a) is as low as 0.06%, which shows that the aluminum fluoride extracted by the method of the embodiment has high purity, low impurity content and high quality.
Example 2: a method for extracting aluminum fluoride from silicon dioxide slag comprises the following steps:
the method comprises the following steps: filtering a product obtained after reaction of fluosilicic acid and aluminum hydroxide to obtain an aluminum fluoride solution and silicon dioxide slag, and crystallizing and filtering the aluminum fluoride solution to obtain an aluminum fluoride mother liquor;
step two: taking 2.5kg of silicon dioxide slag according to the weight ratio, taking 1L of aluminum fluoride mother liquor according to the volume ratio, adding the aluminum fluoride mother liquor into the silicon dioxide slag, and circularly washing the silicon dioxide slag for 10 minutes through the aluminum fluoride mother liquor under stirring;
step three: filtering the washed silicon dioxide slag and aluminum fluoride mother liquor by a vacuum filter to obtain 1.2L of silicon dioxide filter cake and aluminum fluoride filtrate;
step four: feeding the aluminum fluoride filtrate obtained in the third step into a crystallization tank, crystallizing at the temperature of 95 ℃ for 4 hours, and filtering to obtain 127g of an aluminum fluoride filter cake;
step five: and drying the aluminum fluoride filter cake obtained in the fourth step at the temperature of 105 ℃ to reduce the weight of the aluminum fluoride filter cake by 39.4%, calcining the dried aluminum fluoride filter cake to lose crystal water, and cooling to obtain 78.4g of aluminum fluoride.
The following table is a comparison table of the content change of some components in this example:
Figure BDA0002884681680000061
as can be seen from the above table, F after washing-The content of Al is 7.59g/L in the aluminum fluoride filtrate from 4.4g/L in the aluminum fluoride mother liquor3+The content of the aluminum fluoride is changed from 17.92g/L in the aluminum fluoride mother liquor to 30.9g/L in the aluminum fluoride filtrate, which shows that aluminum fluoride in the silicon dioxide slag is largely washed out after washing; the filtrate of aluminium fluoride after crystallization is compared with mother liquor of aluminium fluoride, F-The content of Al is reduced from 4.4g/L to 3.95g/L3+The content of (2) is reduced from 17.92g/L to 12.5g/L, which indicates that a part of aluminum fluoride is precipitated in the aluminum fluoride mother liquor, so the aluminum fluoride in the aluminum fluoride mother liquor is also extracted by the method of the embodiment; the weight of the calcined aluminum fluoride was 78.4g, which shows that 78.4g of aluminum fluoride was finally extracted from 2.5kg of silica fume by the method of this example, and F was contained in the extracted aluminum fluoride-Up to 64.4% of Al3+Up to 31.62% of SiO2In an amount of as low as 0.13%, P2O5As low as 0.05%; it is demonstrated that the aluminum fluoride extracted by the method of this example has high purity, low impurity content, and high quality.
Example 3: a method for extracting aluminum fluoride from silicon dioxide slag comprises the following steps:
the method comprises the following steps: filtering a product obtained after reaction of fluosilicic acid and aluminum hydroxide to obtain an aluminum fluoride solution and silicon dioxide slag, and crystallizing and filtering the aluminum fluoride solution to obtain an aluminum fluoride mother liquor;
step two: taking 2.7kg of silicon dioxide slag according to the weight ratio, taking 1.2L of aluminum fluoride mother liquor according to the volume ratio, adding the aluminum fluoride mother liquor into the silicon dioxide slag, and circularly washing the silicon dioxide slag for 12 minutes through the aluminum fluoride mother liquor under stirring;
step three: filtering the washed silicon dioxide slag and aluminum fluoride mother liquor by a vacuum filter to obtain 1.28L of silicon dioxide filter cake and aluminum fluoride filtrate;
step four: feeding the aluminum fluoride filtrate obtained in the third step into a crystallization tank, crystallizing at the temperature of 98 ℃ for 4.2 hours, and filtering to obtain 136g of an aluminum fluoride filter cake;
step five: and C, drying the aluminum fluoride filter cake obtained in the fourth step at 108 ℃ to reduce the weight of the aluminum fluoride filter cake by 39.62%, calcining the dried aluminum fluoride filter cake to lose crystal water, and cooling to obtain 83g of aluminum fluoride.
The following table is a comparison table of the content change of some components in this example:
Figure BDA0002884681680000081
as can be seen from the above table, F after washing-The content of Al is 7.45g/L in the aluminum fluoride filtrate from 4.59g/L in the aluminum fluoride mother liquor3+The content of the aluminum fluoride is 30.82g/L in the aluminum fluoride filtrate from 18.13g/L in the aluminum fluoride mother liquor, which shows that aluminum fluoride in the silicon dioxide slag is largely washed out after washing; the filtrate of aluminium fluoride after crystallization is compared with mother liquor of aluminium fluoride, F-The content of Al is reduced from 4.59g/L to 3.87g/L3+The content of (2) was reduced from 18.13g/L to 12.41g/L, which indicates that a part of aluminum fluoride in the aluminum fluoride mother liquor was also precipitated, so the aluminum fluoride in the aluminum fluoride mother liquor was also extracted by the method of this example; the weight of the calcined aluminum fluoride was 83g, which shows that 83g of aluminum fluoride was finally extracted from 2.7kg of silica fume by the method of this example, and F was contained in the extracted aluminum fluoride-Up to 64.35% of Al3+The content of (A) is up to 31.58 percent, and SiO2In an amount of as low as 0.14%, P2O5As low as 0.04%; it is demonstrated that the aluminum fluoride extracted by the method of this example has high purity, low impurity content, and high quality.
The specific implementation process is experimental data of a lab scale, and the data can be completely suitable for industrial practical production after being amplified in equal proportion.

Claims (2)

1. A method for extracting aluminum fluoride from silicon dioxide slag is characterized by comprising the following steps:
the method comprises the following steps: filtering a product obtained after reaction of fluosilicic acid and aluminum hydroxide to obtain an aluminum fluoride solution and silicon dioxide slag, and crystallizing and filtering the aluminum fluoride solution to obtain an aluminum fluoride mother liquor;
step two: taking 2.3-2.7 kg of silicon dioxide slag according to the weight ratio, taking 0.8-1.2L of aluminum fluoride mother liquor according to the volume ratio, adding the aluminum fluoride mother liquor into the silicon dioxide slag, and circularly washing the silicon dioxide slag for 8-12 minutes through the aluminum fluoride mother liquor under stirring;
step three: filtering the washed silicon dioxide slag and aluminum fluoride mother liquor by using a vacuum filter to obtain 1.15-1.28L of silicon dioxide filter cake and aluminum fluoride filtrate;
step four: feeding the aluminum fluoride filtrate obtained in the third step into a crystallization tank, crystallizing at the temperature of 92-98 ℃ for 3.8-4.2 hours, and filtering to obtain 122-136 g of an aluminum fluoride filter cake;
step five: and drying the aluminum fluoride filter cake obtained in the fourth step at the temperature of 102-108 ℃ to reduce the weight of the aluminum fluoride filter cake by 39.3-39.62%, calcining the dried aluminum fluoride filter cake to lose crystal water, and cooling to obtain 74-83 g of aluminum fluoride.
2. The method for extracting the aluminum fluoride from the silicon dioxide slag as claimed in claim 1, wherein the method comprises the following steps: in the second step, 2.5kg of silicon dioxide slag is taken according to the weight ratio, 1L of aluminum fluoride mother liquor is taken according to the volume ratio, the aluminum fluoride mother liquor is added into the silicon dioxide slag, and the silicon dioxide slag is circularly washed for 10 minutes through the aluminum fluoride mother liquor under stirring; in the third step, the washed silicon dioxide slag and the aluminum fluoride mother liquor are filtered by a vacuum filter to obtain 1.2L of aluminum fluoride filtrate; in the fourth step, the aluminum fluoride filtrate obtained in the third step is sent into a crystallization tank, crystallized for 4 hours at the temperature of 95 ℃, and then filtered to obtain 127g of an aluminum fluoride filter cake; in the fifth step, the aluminum fluoride filter cake obtained in the fourth step is dried at a temperature of 105 ℃ so that the weight of the aluminum fluoride filter cake is reduced by 39.4%, then the dried aluminum fluoride filter cake is calcined to lose crystal water, and 78.4g of aluminum fluoride is obtained after cooling.
CN202110009472.3A 2021-01-05 2021-01-05 Method for extracting aluminum fluoride from silicon dioxide slag Pending CN113697835A (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3738778A1 (en) * 1986-06-11 1989-05-24 Alusuisse Process for preparing aluminium fluoride trihydrate
CN101428805A (en) * 2008-12-03 2009-05-13 湖北天进工贸有限公司 Utilization technology of fluorine-containing silicon slag
CN101913637A (en) * 2010-08-13 2010-12-15 刘德华 Process method for producing fluorine compounds and silicon compounds by cleanly utilizing fluosilicic acid
CN105502451A (en) * 2015-12-29 2016-04-20 湖北祥福化工科技有限公司 Method for producing aluminum fluoride and co-produced high-molecular ratio cryolite
CN105645447A (en) * 2015-12-29 2016-06-08 湖北祥福化工科技有限公司 Method for producing high-molecular ratio cryolite by utilizing low-concentration fluosilicic acid
CN109231247A (en) * 2018-11-28 2019-01-18 达州励志环保科技有限公司 A kind of method that the by-product of fluosilicic acid legal system aluminum fluoride prepares ice crystal

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3738778A1 (en) * 1986-06-11 1989-05-24 Alusuisse Process for preparing aluminium fluoride trihydrate
CN101428805A (en) * 2008-12-03 2009-05-13 湖北天进工贸有限公司 Utilization technology of fluorine-containing silicon slag
CN101913637A (en) * 2010-08-13 2010-12-15 刘德华 Process method for producing fluorine compounds and silicon compounds by cleanly utilizing fluosilicic acid
CN105502451A (en) * 2015-12-29 2016-04-20 湖北祥福化工科技有限公司 Method for producing aluminum fluoride and co-produced high-molecular ratio cryolite
CN105645447A (en) * 2015-12-29 2016-06-08 湖北祥福化工科技有限公司 Method for producing high-molecular ratio cryolite by utilizing low-concentration fluosilicic acid
CN109231247A (en) * 2018-11-28 2019-01-18 达州励志环保科技有限公司 A kind of method that the by-product of fluosilicic acid legal system aluminum fluoride prepares ice crystal

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Application publication date: 20211126