CN100348495C - Method of producing aluminium fluoride - Google Patents

Method of producing aluminium fluoride Download PDF

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Publication number
CN100348495C
CN100348495C CNB2005100174042A CN200510017404A CN100348495C CN 100348495 C CN100348495 C CN 100348495C CN B2005100174042 A CNB2005100174042 A CN B2005100174042A CN 200510017404 A CN200510017404 A CN 200510017404A CN 100348495 C CN100348495 C CN 100348495C
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China
Prior art keywords
aluminum fluoride
montmorillonite
reaction
aluminum
fluoride
Prior art date
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Expired - Fee Related
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CNB2005100174042A
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Chinese (zh)
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CN1830795A (en
Inventor
李世江
侯红军
杨华春
皇甫根利
刘顺兴
刘海霞
张金保
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Duo Fluoride Chemicals Co Ltd
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Duo Fluoride Chemicals Co Ltd
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Priority to CNB2005100174042A priority Critical patent/CN100348495C/en
Publication of CN1830795A publication Critical patent/CN1830795A/en
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Publication of CN100348495C publication Critical patent/CN100348495C/en
Expired - Fee Related legal-status Critical Current
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Abstract

The present invention relates to a method for producing aluminum fluoride. Montmorillonite and hydrofluoric acid are used as raw materials. The montmorillonite is crushed into 100 to 200 meshes, sulfuric acid solution with the concentration of 200 to 300 g/l reacts with the montmorillonite in a pressurized reactor, the reaction temperature is between 130 DEG C and 150 DEG C, and the reaction time is 1 to 2 hours. After the completion of the reaction, aluminum sulfate solution is obtained after filtration. The aluminum sulfate solution reacts with hydrofluoric acid for crystallization, and after the completion of the crystallization, trihydrate aluminum fluoride is obtained through filtration and washing. Then, aluminum fluoride products are prepared after drying and dehydration, and mother liquor of dilute sulfuric acid is returned for use. The raw material of the method for producing aluminum fluoride is the montmorillonite which replaces aluminum hydroxide. China has large reserve of montmorillonite, the exploitation of the montmorillonite is easy, and the price of the montmorillonite is much lower than that of the aluminum hydroxide. Compared with the traditional method, the cost of the method for producing aluminum fluoride is reduced by 1000 to 1200 Yuan per ton. The mother liquor of diluted sulfuric acid can be in cyclic use when the method of the present invention is used for preparing the aluminum fluoride.

Description

A kind of method of producing aluminum fluoride
Technical field
The present invention relates to a kind of method with kaolinite and Acid of Hydrofluoric Acid Production aluminum fluoride.
Background technology
Aluminum fluoride is used as auxiliary agent in Aluminum Electrolysis Production, be used to reduce electrolytical fusing point, improve electrolytical electric conductivity.Wet method that its traditional processing technology is a hydrofluoric acid---dry method and hydrofluoric acid---.Hydrofluoric acid---dry process is to be raw material with hydrogen fluoride and aluminium hydroxide, its production method is for comprising that aluminium hydroxide is carried out pre-treatment removes crystal water, the thorough mixing reaction under 500-600 ℃ temperature condition with powdery aluminium hydroxide and hydrogen fluoride gas then, generate aluminum trifluoride at reactor bottom, aluminum trifluoride is sent into the rotary drum cooling get product.The raw material of hydrofluoric acid---wet processing is hydrofluoric acid and aluminium hydroxide, and production technique is that hydrofluoric acid and aluminum hydroxide slime react, crystallization, gets aluminum fluoride trihydrate, and drying dehydration again makes aluminium fluoride product.Above-mentioned production technique cost of material height, production cost is higher, and the dry process facility investment is big, complex process.
Summary of the invention
The object of the invention is to provide a kind of method of producing aluminum fluoride, to reduce production costs.
To achieve these goals, technical program of the present invention lies in providing a kind of method of producing aluminum fluoride, it is characterized in that: with kaolinite and hydrofluoric acid is raw material, kaolinite is crushed to the 100-200 order, with concentration be the sulphuric acid soln of 200-300g/l in the compressive reaction still with kaolinite reaction, temperature of reaction 130-150 ℃, reaction times 1-2 hour, after reaction finishes, filter and obtain alum liquor; With alum liquor and hydrofluoric acid reactive crystallization, after crystallization was finished, filtration washing obtained aluminum fluoride trihydrate, and drying dehydration more promptly makes aluminium fluoride product, and the mother liquor dilute sulphuric acid returns use.
Described kaolinic alumina content is 35%-50%.
Aluminium composition is 35-60g/l in the described alum liquor.
Reaction formula of the present invention is:
Al 2O 3+3H 2SO 4=Al 2(SO 4) 3+3H 2O
Al 2(SO 4) 3+6HF=2AlF 3+3H 2SO 4
The raw material that this method is produced aluminum fluoride is a kaolinite, has substituted aluminium hydroxide, abundant, the exploitation easily of China's kaolinite reserves, and price is well below aluminium hydroxide.The present invention produces the method for aluminum fluoride, than the traditional method 1000-1200 unit/ton that can reduce cost.And adopt method of the present invention to prepare aluminum fluoride, its mother liquor dilute sulphuric acid can recycle.
The aluminum fluoride finished product of producing with this method is through chemical examination, quality product be up to state standards (GB/T4292-1999).
Chemical index F Al Na SiO 2 Fe 2O 3 SO 4 2- P 2O 5
The aluminium fluoride product of the present invention's preparation 63 32 0.1 0.01 0.03 0.3 0.01
Special one-level ≥61.0 ≥30.0 ≤0.5 ≤0.28 ≤0.10 ≤0.5 ≤0.04
Special secondary ≥60.0 ≥30.0 ≤0.5 ≤0.30 ≤0.13 ≤0.8 ≤0.04
One-level ≥58.0 ≥28.2 ≤3.0 ≤0.30 ≤0.13 ≤1.1 ≤0.04
Secondary ≥57.0 ≥28.0 ≤3.5 ≤0.35 ≤0.15 ≤1.2 ≤0.04
Embodiment
Embodiment 1
The method of the production aluminum fluoride of present embodiment is as follows: the mother liquor (dilute sulphuric acid) and the vitriol oil are mixed with the sulphuric acid soln that concentration is 200g/l, react 135 ℃ of temperature of reaction, 1 hour reaction times with kaolinite in the compressive reaction still; After reaction finishes, filter and obtain the alum liquor that aluminium composition is 42g/l; With alum liquor and hydrofluoric acid reactive crystallization, after crystallization was finished, filtration washing obtained aluminum fluoride trihydrate, and drying dehydration again makes aluminium fluoride product.
Embodiment 2
The method of the production aluminum fluoride of present embodiment is as follows: the mother liquor (dilute sulphuric acid) and the vitriol oil are mixed with the sulphuric acid soln that concentration is 250g/, react 140 ℃ of temperature of reaction, 1.5 hours reaction times with kaolinite in the compressive reaction still; After reaction finishes, filter and obtain the alum liquor that aluminium composition is 55g/l; With alum liquor and hydrofluoric acid reactive crystallization, after crystallization was finished, filtration washing obtained aluminum fluoride trihydrate, and drying dehydration again makes aluminium fluoride product.
Embodiment 3
The method of the production aluminum fluoride of present embodiment is as follows: the mother liquor (dilute sulphuric acid) and the vitriol oil are mixed with the sulphuric acid soln that concentration is 300g/l, react 145 ℃ of temperature of reaction, 2 hours reaction times with kaolinite in the compressive reaction still; After reaction finishes, filter and obtain the alum liquor that aluminium composition is 60g/l; With alum liquor and hydrofluoric acid reactive crystallization, after crystallization was finished, filtration washing obtained aluminum fluoride trihydrate, and drying dehydration again makes aluminium fluoride product.
It should be noted last that: above embodiment is the unrestricted technical scheme of the present invention in order to explanation only, although the present invention is had been described in detail with reference to the foregoing description, those of ordinary skill in the art is to be understood that: still can make amendment or be equal to replacement the present invention, and not breaking away from any modification or partial replacement of the spirit and scope of the present invention, it all should be encompassed in the middle of the claim scope of the present invention.

Claims (3)

1, a kind of method of producing aluminum fluoride, it is characterized in that: with kaolinite and hydrofluoric acid is raw material, kaolinite is crushed to the 100-200 order, the sulphuric acid soln that with concentration is 200-300g/l reacts with kaolinite in the compressive reaction still, temperature of reaction 130-150 ℃, reaction times 1-2 hour, after reaction finishes, filter and obtain alum liquor; With alum liquor and hydrofluoric acid reactive crystallization, after crystallization was finished, filtration washing obtained aluminum fluoride trihydrate, and drying dehydration more promptly makes aluminium fluoride product, and the mother liquor dilute sulphuric acid returns use.
2, the method for production aluminum fluoride according to claim 1 is characterized in that: described kaolinic alumina content is 35%-50%.
3, the method for production aluminum fluoride according to claim 1 is characterized in that: aluminium composition is 35-60g/l in the described alum liquor.
CNB2005100174042A 2005-03-07 2005-03-07 Method of producing aluminium fluoride Expired - Fee Related CN100348495C (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CNB2005100174042A CN100348495C (en) 2005-03-07 2005-03-07 Method of producing aluminium fluoride

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CNB2005100174042A CN100348495C (en) 2005-03-07 2005-03-07 Method of producing aluminium fluoride

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CN1830795A CN1830795A (en) 2006-09-13
CN100348495C true CN100348495C (en) 2007-11-14

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Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103539180B (en) * 2013-10-31 2015-03-18 洛阳氟钾科技股份公司 Technology for removing sodium out of industrial aluminium fluoride
CN111807399A (en) * 2020-07-07 2020-10-23 锦洋高新材料股份有限公司 Production process method of low-density aluminum fluoride

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1116609A (en) * 1994-08-06 1996-02-14 温宝礼 Method for producing aluminium fluoride and cryolite with kaoline

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1116609A (en) * 1994-08-06 1996-02-14 温宝礼 Method for producing aluminium fluoride and cryolite with kaoline

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