CN1868887A - Preparation method of cryolite - Google Patents

Preparation method of cryolite Download PDF

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Publication number
CN1868887A
CN1868887A CN 200510017594 CN200510017594A CN1868887A CN 1868887 A CN1868887 A CN 1868887A CN 200510017594 CN200510017594 CN 200510017594 CN 200510017594 A CN200510017594 A CN 200510017594A CN 1868887 A CN1868887 A CN 1868887A
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China
Prior art keywords
cryolite
reaction
ammonium
aluminum sulfate
fluoroaluminate
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CN 200510017594
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Chinese (zh)
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CN100360415C (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 CNB2005100175948A priority Critical patent/CN100360415C/en
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Abstract

A process for preparing cryolite from ammonium fluoroaluminate, aluminum sulfate and nitrium sulfate includes such steps as preparing slurry of ammonium fluoroaluminate and the aqueous solution of nitrium sulfate, adding aluminum sulfate to said aqueous solution to obtain mixed solution, adding it to said slurry, reaction, filtering, washing, filtering, washing and drying.

Description

Preparation method of cryolite
Technical Field
The invention relates to a preparation method of cryolite, which takes aluminum profile surface treatment waste residue, namely ammonium fluoroaluminate, aluminum sulfate and mirabilite as raw materials.
Background
The cryolite is named sodium fluoroaluminate in chemical name and has the molecular formula of Na3AlF6It is mainly used as fluxing agent for aluminium electrolysis, wear-resisting filler for rubber and grinding wheel, opalescent agent for enamel, light-shading agent for glass and metal flux, etc. The traditional production process of cryolite is a fluoroaluminate soda ash method, and a clay bittern method, a sodium fluosilicate method, a hydrofluoric acid sodium aluminate method and the like are additionally adopted, and the method generally has the problem of relatively high production cost.
Disclosure of Invention
The invention aims to provide a preparation method of cryolite to reduce the production cost of the cryolite.
In order to achieve the purpose, the technical scheme of the invention is that a cryolite preparation method is adopted, ammonium fluoroaluminate,aluminum sulfate and mirabilite are used as raw materials to react in a water phase, during the reaction, the ammonium fluoroaluminate is firstly prepared into slurry with the concentration of 15-45%, the mirabilite is prepared into a sodium sulfate solution with the concentration of 250-300g/l, and the aluminum sulfate is added according to the reaction proportion calculated according to the molecular ratio n of the generated cryolite to prepare an aluminum sulfate and sodium sulfate mixed solution; uniformly adding the prepared aluminum sulfate and sodium sulfate mixed solution into the ammonium fluoroaluminate slurry for reaction; after the feeding is finished, continuously reacting for a period of time; after the reaction is finished, filtering, fully washing the ointment, filtering, drying the washed ointment to obtain the product, wherein the filtered filtrate is ammonium sulfate solution.
The granularity of the ammonium fluoroaluminate is 150-300 meshes.
The whole reaction process can be carried out at the temperature of normal temperature to 100 ℃.
The reaction formula of the invention is as follows:
in the formula, n: the molecular ratio of cryolite is shown, n ranges from 1 to 3, and n is not equal to 3.
Because the method of the invention takes the waste residue of the surface treatment of the aluminum profile, namely the ammonium fluoroaluminate, as the main raw material, the production cost is lower; in addition, the preparation method has the advantages of simple process, easy operation, easily obtained raw materials and low cost; the most important point is that the invention solves the problem of environmental pollution caused by long-term overstock of ammonium fluoroaluminate waste and realizes changingwaste into valuable.
Detailed Description
Example 1
Preparing ammonium fluoroaluminate with the granularity of 150 meshes into 20% slurry, preparing mirabilite into 300g/l sodium sulfate solution, taking the molecular ratio n of generated cryolite as 1, and adding aluminum sulfate according to the reaction proportion to prepare aluminum sulfate and sodium sulfate mixed solution; heating the ammonium fluoroaluminate slurry to 60 ℃, and uniformly adding the prepared aluminum sulfate and sodium sulfate mixed solution into the ammonium fluoroaluminate slurry for reaction; adding the materials for 60 minutes, continuing to react for 30 minutes after the materials are added, keeping the temperature of 80 ℃ in the whole reaction process, filtering after the reaction is finished, fully washing the ointment, and drying the filtered and washed ointment to obtain the product.
Example 2
Preparing 30% slurry of ammonium fluoroaluminate with the granularity of 200 meshes, preparing 250g/l sodium sulfate solution from mirabilite, taking the molecular ratio n of generated cryolite as 1.5, and adding aluminum sulfate according to the reaction proportion to prepare aluminum sulfate and sodium sulfate mixed solution; heating ammonium fluoroaluminate slurry to 100 ℃, and uniformly adding the prepared aluminum sulfate and sodium sulfate mixed solution into the ammonium fluoroaluminate slurry for reaction; adding the materials for 40 minutes, continuing to react for 15 minutes after the materials are added, keeping the temperature at 100 ℃ in the whole reaction process, filtering after the reaction is finished, fully washing the ointment, and drying the filtered and washed ointment to obtain the product.
Example 3
Preparing 45% slurry of ammonium fluoroaluminate with the granularity of 300 meshes, preparing 280g/l sodium sulfate solution from mirabilite, taking the molecular ratio n of generated cryolite as 2, and adding aluminum sulfate according to the proportion to prepare aluminum sulfate and sodium sulfate mixed solution; uniformly adding the prepared aluminum sulfate and sodium sulfate mixed solution into the ammonium fluoroaluminate slurry at normal temperature to react; adding the materials for 90 minutes, continuing to react for 30 minutes after the materials are added, keeping the temperature of the whole reaction process at normal temperature, filtering after the reaction is finished, and fully washing the ointment. Filtering, washing, drying to obtain the final product, and filtering to obtain filtrate as ammonium chloride solution.
Finally, it should be noted that: although the present invention has been described in detail with reference to the above embodiments, it should be understood by those skilled in the art that: modifications and equivalents may be made thereto without departing from the spirit and scope of the invention and it is intended to cover in the claims the invention as defined in the appended claims.

Claims (4)

1. A method for preparing cryolite is characterized in that: the method comprises the steps of taking ammonium fluoroaluminate, aluminum sulfate and mirabilite as raw materials to react in an aqueous phase, preparing the ammonium fluoroaluminate into slurry with the concentration of 15-45% during reaction, preparing the mirabilite into a sodium sulfate solution with the concentration of 300g/l, and adding the aluminum sulfate according to the reaction proportion according to the calculation of the molecular ratio n of generated cryolite to prepare an aluminum sulfate-sodium sulfate mixed solution; uniformly adding the prepared aluminum sulfate and sodium sulfate mixed solution into the ammonium fluoroaluminate slurry for reaction; after the feeding is finished, continuously reacting for a period of time; after the reaction is finished, filtering, fully washing the ointment, filtering, drying the washed ointment to obtain the product, wherein the filtered filtrate is ammonium sulfate solution.
2. A process for the preparation of cryolite according to claim 1, wherein: the granularity of the ammonium fluoroaluminate is 150-300 meshes.
3. A process for the preparation of cryolite according to claim 2, wherein: the whole reaction process is carried out at the temperature of normal temperature to 100 ℃.
4. A process for the preparation of cryolite according to claim 1, wherein: the value of n is between 1 and 3, and n is not equal to 3.
CNB2005100175948A 2005-05-23 2005-05-23 Preparation method of cryolite Expired - Fee Related CN100360415C (en)

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CNB2005100175948A CN100360415C (en) 2005-05-23 2005-05-23 Preparation method of cryolite

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Application Number Priority Date Filing Date Title
CNB2005100175948A CN100360415C (en) 2005-05-23 2005-05-23 Preparation method of cryolite

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CN1868887A true CN1868887A (en) 2006-11-29
CN100360415C CN100360415C (en) 2008-01-09

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101555033B (en) * 2009-03-20 2011-08-24 云南云天化国际化工股份有限公司 Method for preparing cryolite and coproducing soluble glass by using hydrof luorosilicic acid
CN102649577A (en) * 2012-05-23 2012-08-29 深圳市新星轻合金材料股份有限公司 Sodium cryolite for aluminum electrolytic industry and preparation method thereof

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SU431113A1 (en) * 1970-04-20 1974-06-05 В. Г. Морозов, О. С. Игнатьев, И. А. Варлаков , В. Н. Коровин Институт химии , технологии резких элементов , минерального METHOD OF OBTAINING FLUORINE ALUMINUM
US3816591A (en) * 1972-05-05 1974-06-11 Oesterr Stickstoffwerke Ag Process for the recovery of aluminium and fluorine from a dilute aqueous solution
CN1194897C (en) * 2002-05-10 2005-03-30 焦作市多氟多化工有限公司 Method for producing cryolite
CN1203000C (en) * 2002-10-23 2005-05-25 赵小春 Method for producing cryolite
JP2004313657A (en) * 2003-04-21 2004-11-11 Ge Medical Systems Global Technology Co Llc Radiation calculated tomographic image apparatus

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101555033B (en) * 2009-03-20 2011-08-24 云南云天化国际化工股份有限公司 Method for preparing cryolite and coproducing soluble glass by using hydrof luorosilicic acid
CN102649577A (en) * 2012-05-23 2012-08-29 深圳市新星轻合金材料股份有限公司 Sodium cryolite for aluminum electrolytic industry and preparation method thereof
WO2013174066A1 (en) * 2012-05-23 2013-11-28 深圳市新星轻合金材料股份有限公司 Sodium cryolite used in aluminum electrolysis industry and preparation method thereof

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Granted publication date: 20080109

Termination date: 20120523