CN101289213B - Process for preparing cryolite - Google Patents

Process for preparing cryolite Download PDF

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Publication number
CN101289213B
CN101289213B CN2007100542522A CN200710054252A CN101289213B CN 101289213 B CN101289213 B CN 101289213B CN 2007100542522 A CN2007100542522 A CN 2007100542522A CN 200710054252 A CN200710054252 A CN 200710054252A CN 101289213 B CN101289213 B CN 101289213B
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China
Prior art keywords
aluminum fluoride
aluminium
electrolyte
sodium aluminum
raw materials
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Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Fee Related
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CN2007100542522A
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Chinese (zh)
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CN101289213A (en
Inventor
李世江
侯红军
杨华春
皇甫根利
张金保
张梅
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Duo Fluoride Chemicals Co Ltd
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Duo Fluoride Chemicals Co Ltd
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Publication date
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Priority to CN2007100542522A priority Critical patent/CN101289213B/en
Publication of CN101289213A publication Critical patent/CN101289213A/en
Application granted granted Critical
Publication of CN101289213B publication Critical patent/CN101289213B/en
Expired - Fee Related legal-status Critical Current
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  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)

Abstract

The invention relates to a method for preparing cryolite which is prepared in a solid phase reaction by taking electrolyte blocks in an aluminum factory and fluoaluminic acid ammonium as raw materials. The raw materials of the invention are a large amount of residues in electrolytic aluminum factories, namely the electrolyte blocks, and the residues in section aluminum industry, namely the fluoaluminic acid ammonium, thus opening up the resources of raw materials for producing villiaumite, reducing dependency on fluorite, saving a large amount of valuable resources, greatly reducing production cost and relieving the problem of the pollution to surrounding environment and having low cost. In addition, the products in the reaction process of the invention can be circularly utilized, which greatly reduces the production cost to a certain degree, therefore the method has good social and economic value, which is easy for popularization and application.

Description

A kind of method for preparing sodium aluminum fluoride
Technical field
The present invention relates to a kind of method for preparing sodium aluminum fluoride, this method is a raw material with the ionogen and the ammonium aluminum fluoride of aluminum electrolysis industry.
Background technology
Sodium aluminum fluoride is a kind of alkali-metal fluoaluminate, also claims sodium fluoroaluminate, and its molecular formula is Na 3AlF 6Natural cryolite is monoclinic prismatic crystallization, and is colourless, because the influence of impurity often is canescence, faint yellow or incarnadine, is black sometimes.The indivisible compact block of normal one-tenth has vitreous luster.Be slightly soluble in water, react acid, meet sulfuric acid and promptly decompose.Sodium aluminum fluoride is as a kind of Chemicals, be mainly used in the fusing assistant of metal smelting aluminium, also can make the sterilant of farm crop, the enamel opacifier, the opalizer and the fusing assistant of glass and enamel production usefulness, the wear-resistant filler of resin rubber also can be used for the production of iron alloy and rimming steel, about 100,000 tons of domestic annual requirement.Along with the fast development of aluminium industry, its potential market share progressively increases, and is also more and more higher to the requirement of quality.
The traditional processing technology of sodium aluminum fluoride is a hydrofluoaluminic acid soda ash method, also have clay bittern method, Sodium Silicofluoride method and hydrofluoric acid sodium aluminate method etc., these methods all need take certain fluorine resource, and production cost is higher, and all there is the different problem of environmental pollution of degree in current technology.
Summary of the invention
The object of the invention is to provide a kind of method for preparing sodium aluminum fluoride, to reduce production costs, saves resource.
To achieve these goals, technical program of the present invention lies in adopting a kind of method for preparing sodium aluminum fluoride, it is that raw material reacts in solid phase with aluminium manufacturer's electrolyte block and ammonium aluminum fluoride.
Described aluminium manufacturer electrolyte block is the waste residue of aluminum electrolysis industry.
Described ammonium aluminum fluoride is that aluminium shape surface is handled waste residue.
Concrete production method is: earlier with the high temperature melting of impure more aluminium manufacturer's electrolyte block through 900 ℃-1200 ℃, fusing point difference according to various compositions in the ionogen, separate, remove infusibility impurity---pitch carbon granule, carbon element of graphite, aluminium carbide, prussiate and ferrosilicon oxide compound, solid electrolyte after will purifying again and ammonium aluminum fluoride pulverize, press mass ratio 3-5: 1 mixed, the high-temperature calcination through 400 ℃~600 ℃ promptly gets the sodium aluminum fluoride product.
Reaction formula of the present invention is:
2(NH 4) 3AlF 6+Al 2O 3→4AlF 3+6NH 3↑+3H 2O
Raw material of the present invention is that ammonium aluminum fluoride is a raw material to the employing a large amount of waste residue of electrolytic aluminium factory---electrolyte block and aluminium section bar industry waste residue---, opened up the source of villiaumite raw materials for production, alleviated dependence to fluorite, saved a large amount of precious resources, with low cost, greatly reduce production cost, and the problem of environmental pollution around also having alleviated.In addition, the product in the reaction process of the present invention can recycle, greatly reduces production cost to a certain extent, and the present invention has favorable social and economic worth, is easy to apply.
This technology sodium aluminum fluoride quality contrast table
Electrolytical composition analysis
The sodium aluminum fluoride national standard
Embodiment
Embodiment 1
Preparation method of the present invention is: with the solid electrolyte piece, be broken into the fritter of 30mm with jaw crusher or hammer mill, it is standby to be stored in feed bin; With electrolyte block after the fragmentation, add in 950 ℃ molten the coming out of the stove of high temperature, generate the melting electrolyte solution; With vacuum withdraw device electrolyte solution is extracted, solid waste is wherein separated with purified electrolyte solution; Electrolyte solution becomes electrolyte block after cooling off; Electrolyte block and ammonium aluminum fluoride after Raymond mill is levigate, are mixed by 3.5: 1 amount of mass ratio, add in the high-temperature calcination stove and under 450 ℃ temperature, carry out calcination reaction, generate sodium aluminum fluoride.
Embodiment 2
Preparation method of the present invention is: with the solid electrolyte piece, be broken into the fritter of 40mm with jaw crusher or hammer mill, it is standby to be stored in feed bin; With electrolyte block after the fragmentation, add in 1000 ℃ molten the coming out of the stove of high temperature, generate the melting electrolyte solution; With vacuum withdraw device electrolyte solution is extracted, solid waste is wherein separated with purified electrolyte solution; Electrolyte solution becomes electrolyte block after cooling off; After Raymond mill was levigate, it was even to press 4: 1 mixed of mass ratio, adds in the high-temperature calcination stove and carry out calcination reaction under 500 ℃ temperature, generates sodium aluminum fluoride with electrolyte block and ammonium aluminum fluoride.
Embodiment 3
Preparation method of the present invention is: with the solid electrolyte piece, be broken into the fritter of 50mrn with jaw crusher or hammer mill, it is standby to be stored in feed bin; With electrolyte block after the fragmentation, add in 1100 ℃ molten the coming out of the stove of high temperature, generate the melting electrolyte solution; With vacuum withdraw device electrolyte solution is extracted, solid waste is wherein separated with purified electrolyte solution; Electrolyte solution becomes electrolyte block after cooling off; After Raymond mill is levigate, is that 4.5: 1 amount mix by mass ratio with electrolyte block and ammonium aluminum fluoride, adds and carry out the calcination reaction in the high-temperature calcination stove under 600 ℃ temperature, generates sodium aluminum fluoride.
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 (2)

1. method for preparing sodium aluminum fluoride, it is characterized in that: with aluminium manufacturer's electrolyte block and ammonium aluminum fluoride is that raw material reacts in solid phase and makes, concrete production method is: earlier with the high temperature melting of impure more aluminium manufacturer's electrolyte block through 900 ℃-1200 ℃, fusing point difference according to various compositions in the ionogen, separate, remove infusibility impurity---the pitch carbon granule, carbon element of graphite, aluminium carbide, prussiate and ferrosilicon oxide compound, solid electrolyte after will purifying again and ammonium aluminum fluoride pulverize, press mass ratio 3-5: 1 mixed is even, add in the high-temperature calcination stove and under 400 ℃-600 ℃ temperature, carry out calcination reaction, promptly get the sodium aluminum fluoride product.
2. the method for preparing sodium aluminum fluoride according to claim 1 is characterized in that: described ammonium aluminum fluoride is that aluminium shape surface is handled waste residue.
CN2007100542522A 2007-04-19 2007-04-19 Process for preparing cryolite Expired - Fee Related CN101289213B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN2007100542522A CN101289213B (en) 2007-04-19 2007-04-19 Process for preparing cryolite

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN2007100542522A CN101289213B (en) 2007-04-19 2007-04-19 Process for preparing cryolite

Publications (2)

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CN101289213A CN101289213A (en) 2008-10-22
CN101289213B true CN101289213B (en) 2011-07-20

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1119300A (en) * 1966-05-26 1968-07-10 Ver Kunstmestf Mekog Albatros A process for the preparation of anhydrous aluminium fluoride
US4070447A (en) * 1975-06-16 1978-01-24 Central Glass Company, Limited Process for preparing anhydrous aluminum fluoride
CN1736875A (en) * 2004-08-19 2006-02-22 焦作市多氟多化工有限公司 Cryolite production method

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1119300A (en) * 1966-05-26 1968-07-10 Ver Kunstmestf Mekog Albatros A process for the preparation of anhydrous aluminium fluoride
US4070447A (en) * 1975-06-16 1978-01-24 Central Glass Company, Limited Process for preparing anhydrous aluminum fluoride
CN1736875A (en) * 2004-08-19 2006-02-22 焦作市多氟多化工有限公司 Cryolite production method

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
刘建良.用铵冰渣制取氟化铝.化工生产与技术.2005,12(4),6-7. *
石泓然.火法熔炼分离固废料中电解质与碳技术的研究.轻金属.1997,(5),36-39. *

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Granted publication date: 20110720

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