CN1329302C - Method for manufacturing sodium aluminium fluoride by pickling aluminium slag - Google Patents
Method for manufacturing sodium aluminium fluoride by pickling aluminium slag Download PDFInfo
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- CN1329302C CN1329302C CNB031040578A CN03104057A CN1329302C CN 1329302 C CN1329302 C CN 1329302C CN B031040578 A CNB031040578 A CN B031040578A CN 03104057 A CN03104057 A CN 03104057A CN 1329302 C CN1329302 C CN 1329302C
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- China
- Prior art keywords
- sodium
- acid
- aluminium slag
- acid etching
- etching aluminium
- Prior art date
- 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.)
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- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 45
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 239000004411 aluminium Substances 0.000 title claims abstract description 41
- 239000011734 sodium Substances 0.000 title claims abstract description 40
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 title claims abstract description 39
- 229910052708 sodium Inorganic materials 0.000 title claims abstract description 39
- 239000002893 slag Substances 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 25
- 238000004519 manufacturing process Methods 0.000 title abstract description 15
- KLZUFWVZNOTSEM-UHFFFAOYSA-K Aluminium flouride Chemical compound F[Al](F)F KLZUFWVZNOTSEM-UHFFFAOYSA-K 0.000 title 2
- 238000005554 pickling Methods 0.000 title 1
- 239000002253 acid Substances 0.000 claims abstract description 38
- 239000002994 raw material Substances 0.000 claims abstract description 10
- 239000007788 liquid Substances 0.000 claims abstract description 9
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims abstract description 7
- 235000011130 ammonium sulphate Nutrition 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000000926 separation method Methods 0.000 claims abstract description 6
- 238000005530 etching Methods 0.000 claims description 26
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 229940056729 sodium sulfate anhydrous Drugs 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 5
- 239000002002 slurry Substances 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 4
- MIMUSZHMZBJBPO-UHFFFAOYSA-N 6-methoxy-8-nitroquinoline Chemical compound N1=CC=CC2=CC(OC)=CC([N+]([O-])=O)=C21 MIMUSZHMZBJBPO-UHFFFAOYSA-N 0.000 claims description 3
- -1 ammonium aluminum fluoride Chemical group 0.000 claims description 3
- 239000001166 ammonium sulphate Substances 0.000 claims description 3
- 239000004615 ingredient Substances 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 2
- 229910052731 fluorine Inorganic materials 0.000 claims description 2
- 239000011737 fluorine Substances 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 claims description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 abstract description 5
- 239000002699 waste material Substances 0.000 abstract description 2
- 238000005260 corrosion Methods 0.000 abstract 3
- 230000007797 corrosion Effects 0.000 abstract 3
- 239000013049 sediment Substances 0.000 abstract 3
- 238000004140 cleaning Methods 0.000 abstract 1
- 229920002521 macromolecule Polymers 0.000 abstract 1
- 239000000047 product Substances 0.000 description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 3
- 229910021502 aluminium hydroxide Inorganic materials 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 239000003929 acidic solution Substances 0.000 description 2
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 238000001125 extrusion Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 229910001388 sodium aluminate Inorganic materials 0.000 description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 description 2
- 235000011152 sodium sulphate Nutrition 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 239000005995 Aluminium silicate Substances 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- DPDMMXDBJGCCQC-UHFFFAOYSA-N [Na].[Cl] Chemical compound [Na].[Cl] DPDMMXDBJGCCQC-UHFFFAOYSA-N 0.000 description 1
- 238000009866 aluminium metallurgy Methods 0.000 description 1
- 235000012211 aluminium silicate Nutrition 0.000 description 1
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 210000003298 dental enamel Anatomy 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 229910001651 emery Inorganic materials 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000003605 opacifier Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 235000017550 sodium carbonate Nutrition 0.000 description 1
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 description 1
- 229960003010 sodium sulfate Drugs 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000006557 surface reaction Methods 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
Landscapes
- Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
- ing And Chemical Polishing (AREA)
Abstract
The present invention relates to a method for manufacturing sodium fluoaluminate by acid corrosion aluminium slag, which mainly solves the problems of high production cost and serious environment pollution of a production process, etc. in the prior art and changes wastes into the valuable synchronously. The method uses the acid corrosion aluminium slag, anhydrous sodium sulfate and hydrofluoaluminic acid as raw materials, and the acid corrosion aluminium slag is reacted with the anhydrous sodium sulfate under certain temperature after milled with water to generate sodium fluoaluminate sediments with a macromolecule ratio and an ammonium sulfate solution; the sodium fluoaluminate sediments and the ammonium sulfate solution are reacted with the hydrofluoaluminic acid after solid-liquid separation and cleaning, and the sodium fluoaluminate sediments and the ammonium sulfate solution are dried to obtain a finished product of the sodium fluoaluminate.
Description
Technical field
The present invention relates to a kind of preparation method of villiaumite, particularly a kind of acid etching aluminium slag is made the method for sodium fluoroaluminate.
Background technology
Sodium fluoroaluminate also is sodium aluminum fluoride, molecular formula Na
3AlF
6, be generally colourless oblique system crystal, but often because of impure canescence, the incarnadine or faint yellow of being.Sodium fluoroaluminate mainly is used to the fusing assistant of aluminium metallurgy, the sterilant of farm crop, the fusion agent and the opacifier of enamel glaze; When making opaque glass, make the glass opalizer, also can be used for the wear-resistant filler of metal flux that aluminium alloy and rimming steel produce and rubber, emery wheel etc.
The production of sodium fluoroaluminate normally adopts hydrofluoric acid, aluminium hydroxide and three kinds of industrial raw material reactions of sodium hydroxide to form, and is in addition, following in addition several by the different production methods of the disclosed sodium fluoroaluminate of Chinese patent literature:
The invention of application number 98118202.X is to adopt raw materials such as Sodium Silicofluoride, industrial ammonia, sodium aluminate to make the method for sodium fluoroaluminate.
The invention of application number 94112436.3 is to adopt kaolin to make Tai-Ace S 150, reacts the method for making sodium fluoroaluminate with hydrofluoric acid, sodium sulfate again.
The invention of application number 99101915.6 is that to adopt hydrofluoric acid, sodium aluminate, Industrial Salt be the method that raw material is made sodium fluoroaluminate.
The invention of application number 90105451.8 is that to adopt hydrochloric acid, clay, Industrial Salt be the method that raw material is made sodium fluoroaluminate.
The invention of application number 94111147.4 is that to adopt hydrofluoric acid, yellow soda ash, aluminium hydroxide be the method that raw material is made sodium fluoroaluminate.
The invention of application number 01123585.3 is that to adopt fluoride waste, sodium hydroxide, aluminium hydroxide be the method that raw material is made sodium fluoroaluminate.
The invention of the patent No. 92111046.4 is to adopt Y zeolite byproduct (NH
4)
2NaAlF
6, sodium-chlor is the method that raw material is made sodium fluoroaluminate.
More than these methods of making sodium fluoroaluminate exist the weak point that production process is long, production cost is higher and environmental pollution is serious.
Summary of the invention
The object of the present invention is to provide a kind of method of making sodium fluoroaluminate with acid etching aluminium slag.Adopt this method manufacturing sodium fluoroaluminate to have and can eliminate acid etching aluminium slag environmental pollution, and the characteristics that production process is short, production cost is low.
The technical scheme that acid etching aluminium slag of the present invention is made the method for sodium fluoroaluminate is: will be made into slurries behind the acid etching aluminium pulp water mill, heating in reactor, insulation are hydrolyzed; Add Sodium sulfate anhydrous.min(99) (anhydrous sodium sulphate) then and react, the sodium fluoroaluminate throw out and the ammoniumsulphate soln that obtain after the reaction are made solid-liquid separation with whizzer, clean solid part; After material that cleaned and hydrofluoaluminic acid reaction, drying is handled and is the finished product sodium fluoroaluminate.
Acid etching aluminium slag of the present invention is made the method for sodium fluoroaluminate, and its concrete steps are as follows:
A, raw material are acid etching aluminium slag, Sodium sulfate anhydrous.min(99) and hydrofluoaluminic acid;
After b, acid etching aluminium pulp water are milled to 100～180 orders, be made into solid-to-liquid ratio and be 1: 1～3 slurries, in reactor, be heated to 95 ℃～110 ℃, be incubated 1～3 hour and be hydrolyzed;
C, add Sodium sulfate anhydrous.min(99) then and react, reacted product is sodium fluoroaluminate throw out and ammoniumsulphate soln, makes solid-liquid separation with whizzer, cleans solid part then;
D, the material that cleaned in the reaction of 75 ℃～95 ℃ temperature and hydrofluoaluminic acid, drying is handled and is the finished product sodium fluoroaluminate again.
The industrial residue that produces when wherein, described acid etching aluminium slag is meant the solution-treated aluminum products surface of preparing with ammonium bifluoride and hydrofluoric acid; The add-on of Sodium sulfate anhydrous.min(99) is 1.05～1.2 times of acid etching aluminium slag butt weight.
Acid etching aluminium slag is a kind of industrial residue, untimely processing meeting serious environment pollution.Acid etching aluminium slag produces in the aluminum products production process, and for example, in architectural aluminum section was produced, the aluminium section bar after the extrusion molding must be done the surface and handle, and could eliminate extrusion machinery line and surface detail microdefect.It is chemical method that aluminium shape surface is handled the most frequently used method, that is: by chemical reaction the mechanical line of aluminium shape surface and defective are removed or covered.At present, the surface treatment method of the common employing of domestic each aluminium section bar plant is the acid etching method: aluminium section bar is immersed in the acidic solution of being prepared by ammonium bifluoride and hydrofluoric acid, produce chemical reaction with aluminium shape surface at a certain temperature, aluminium shape surface is removed one deck, make aluminium shape surface bright and clean soft, fine and smooth attractive in appearance, metalluster arranged.The throw out that acidic solution and aluminium shape surface reaction back produce is exactly an acid etching aluminium slag.Confirm that through chemical analysis the major ingredient of acid etching aluminium slag is ammonium aluminum fluoride (NH
4)
3AlF
6, aluminium element Al content 11～16% wherein, fluorine element F content 50～60%.Adopt method of the present invention, can eliminate of the pollution of acid etching aluminium slag, also can produce the sodium fluoroaluminate product environment.The present invention has that production technique is simple, the characteristics of reduced investment.Adopt can the be up to state standards requirement of GB/T4291.1999 of its quality of sodium fluoroaluminate product of manufacturing of the present invention.
Embodiment
The method of acid etching aluminium slag of the present invention being made sodium fluoroaluminate below by embodiment is described further.
Embodiment
Making in the technology of sodium fluoroaluminate with acid etching aluminium slag, adopting one of 1000L plastics reactor, respectively one of levigator, whizzer, dryer, thermal source adopts 0.6MPa steam.
The concrete steps of making sodium fluoroaluminate with acid etching aluminium slag are as follows:
1, behind dry acid erosion aluminium slag 100kg water mill to 100～180 orders, adding water, to be made into solid-to-liquid ratio be 1: 2 slurries.
2, slurries are added in the reactor,, be incubated 2 hours and be hydrolyzed with being steam heated to 100 ℃.
3, add Sodium sulfate anhydrous.min(99) 120kg then in reactor, keep temperature of reaction at 95 ℃～110 ℃, the reinforced time is 30 minutes.
4, make solid-liquid separation with whizzer, the liquid major ingredient after the separation is an ammonium sulfate, belongs to byproduct; Then the material in the whizzer is added water and clean, add waterside several 3 times.
5, the material that cleaned is reacted with hydrofluoaluminic acid at 85 ℃, and be incubated 2 hours.
6, drying handle finished product sodium fluoroaluminate 102.5kg.
Claims (2)
1, a kind of acid etching aluminium slag is made the method for sodium fluoroaluminate, and acid etching aluminium slag is the industrial residue that produces during with the solution-treated aluminum products surface of ammonium bifluoride and hydrofluoric acid preparation, and major ingredient is ammonium aluminum fluoride (NH
4)
3AlF
6, wherein aluminium element content 11～16%, and fluorine element content 50～60% is characterized in that:
A, raw material are acid etching aluminium slag, Sodium sulfate anhydrous.min(99) and hydrofluoaluminic acid;
After b, acid etching aluminium pulp water are milled to 100～180 orders, be made into solid-to-liquid ratio and be 1: 1～3 slurries, in reactor, be heated to 95 ℃～110 ℃, be incubated 1～3 hour and be hydrolyzed;
C, add Sodium sulfate anhydrous.min(99) then and react, reacted product is sodium fluoroaluminate throw out and ammoniumsulphate soln; Make solid-liquid separation with whizzer, clean solid part then;
D, the material that cleaned in the reaction of 75 ℃～95 ℃ temperature and hydrofluoaluminic acid, drying is handled and is the finished product sodium fluoroaluminate again.
2, acid etching aluminium slag according to claim 1 is made the method for sodium fluoroaluminate, and it is characterized in that: the add-on of Sodium sulfate anhydrous.min(99) is 1.05～1.2 times of acid etching aluminium slag butt weight.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB031040578A CN1329302C (en) | 2003-02-21 | 2003-02-21 | Method for manufacturing sodium aluminium fluoride by pickling aluminium slag |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB031040578A CN1329302C (en) | 2003-02-21 | 2003-02-21 | Method for manufacturing sodium aluminium fluoride by pickling aluminium slag |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1522962A CN1522962A (en) | 2004-08-25 |
| CN1329302C true CN1329302C (en) | 2007-08-01 |
Family
ID=34282168
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB031040578A Expired - Fee Related CN1329302C (en) | 2003-02-21 | 2003-02-21 | Method for manufacturing sodium aluminium fluoride by pickling aluminium slag |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1329302C (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1117944A (en) * | 1994-08-30 | 1996-03-06 | 湘乡铝厂 | Method for production of high-molecular-ratio ice spar |
| CN1332118A (en) * | 2001-08-03 | 2002-01-23 | 刘定忠 | Method for producing cryolite from fluorine-containing wastewater |
-
2003
- 2003-02-21 CN CNB031040578A patent/CN1329302C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1117944A (en) * | 1994-08-30 | 1996-03-06 | 湘乡铝厂 | Method for production of high-molecular-ratio ice spar |
| CN1332118A (en) * | 2001-08-03 | 2002-01-23 | 刘定忠 | Method for producing cryolite from fluorine-containing wastewater |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1522962A (en) | 2004-08-25 |
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Granted publication date: 20070801 Termination date: 20120221 |