CN109518247A - A kind of anodic oxidation device and method using device aluminium powder anodic oxidation in acid condition - Google Patents
A kind of anodic oxidation device and method using device aluminium powder anodic oxidation in acid condition Download PDFInfo
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- CN109518247A CN109518247A CN201710840182.7A CN201710840182A CN109518247A CN 109518247 A CN109518247 A CN 109518247A CN 201710840182 A CN201710840182 A CN 201710840182A CN 109518247 A CN109518247 A CN 109518247A
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- Prior art keywords
- aluminium powder
- electrolysis bath
- anodic oxidation
- acidic electrolysis
- acid
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 164
- 239000000843 powder Substances 0.000 title claims abstract description 163
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 160
- 239000004411 aluminium Substances 0.000 title claims abstract description 150
- 230000003647 oxidation Effects 0.000 title claims abstract description 70
- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 70
- 238000000034 method Methods 0.000 title claims abstract description 49
- 239000002253 acid Substances 0.000 title claims abstract description 25
- 230000002378 acidificating effect Effects 0.000 claims abstract description 95
- 238000005868 electrolysis reaction Methods 0.000 claims abstract description 95
- 229910052751 metal Inorganic materials 0.000 claims abstract description 42
- 239000002184 metal Substances 0.000 claims abstract description 42
- 238000000926 separation method Methods 0.000 claims abstract description 41
- 239000001257 hydrogen Substances 0.000 claims abstract description 26
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000003780 insertion Methods 0.000 claims abstract description 6
- 230000037431 insertion Effects 0.000 claims abstract description 6
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 claims description 30
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 claims description 26
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 claims description 25
- 235000019837 monoammonium phosphate Nutrition 0.000 claims description 25
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 claims description 24
- BDJRBEYXGGNYIS-UHFFFAOYSA-N nonanedioic acid Chemical compound OC(=O)CCCCCCCC(O)=O BDJRBEYXGGNYIS-UHFFFAOYSA-N 0.000 claims description 24
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 claims description 20
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 17
- 239000004327 boric acid Substances 0.000 claims description 17
- 239000001361 adipic acid Substances 0.000 claims description 15
- 235000011037 adipic acid Nutrition 0.000 claims description 15
- 239000006012 monoammonium phosphate Substances 0.000 claims description 14
- RTBFRGCFXZNCOE-UHFFFAOYSA-N 1-methylsulfonylpiperidin-4-one Chemical compound CS(=O)(=O)N1CCC(=O)CC1 RTBFRGCFXZNCOE-UHFFFAOYSA-N 0.000 claims description 12
- JFCQEDHGNNZCLN-UHFFFAOYSA-N anhydrous glutaric acid Natural products OC(=O)CCCC(O)=O JFCQEDHGNNZCLN-UHFFFAOYSA-N 0.000 claims description 12
- 239000001530 fumaric acid Substances 0.000 claims description 10
- 229910001220 stainless steel Inorganic materials 0.000 claims description 10
- 239000010935 stainless steel Substances 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims description 10
- 230000036961 partial effect Effects 0.000 claims description 9
- 239000007864 aqueous solution Substances 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 8
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 6
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 6
- 239000010931 gold Substances 0.000 claims description 6
- 229910052737 gold Inorganic materials 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 4
- 235000010338 boric acid Nutrition 0.000 claims description 4
- 229910002804 graphite Inorganic materials 0.000 claims description 4
- 239000010439 graphite Substances 0.000 claims description 4
- 229910052697 platinum Inorganic materials 0.000 claims description 4
- 229910052719 titanium Inorganic materials 0.000 claims description 4
- 239000010936 titanium Substances 0.000 claims description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 2
- SEGLCEQVOFDUPX-UHFFFAOYSA-N di-(2-ethylhexyl)phosphoric acid Chemical compound CCCCC(CC)COP(O)(=O)OCC(CC)CCCC SEGLCEQVOFDUPX-UHFFFAOYSA-N 0.000 claims 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims 1
- 230000001788 irregular Effects 0.000 claims 1
- 125000001400 nonyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 26
- 230000000694 effects Effects 0.000 abstract description 8
- 239000003973 paint Substances 0.000 abstract description 6
- 238000002485 combustion reaction Methods 0.000 abstract description 4
- 238000004880 explosion Methods 0.000 abstract description 4
- 238000005260 corrosion Methods 0.000 description 33
- 230000007797 corrosion Effects 0.000 description 33
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 12
- 239000003792 electrolyte Substances 0.000 description 12
- 230000005764 inhibitory process Effects 0.000 description 11
- 238000006243 chemical reaction Methods 0.000 description 9
- 239000000203 mixture Substances 0.000 description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 6
- 238000002156 mixing Methods 0.000 description 6
- 239000001301 oxygen Substances 0.000 description 6
- 229910052760 oxygen Inorganic materials 0.000 description 6
- 239000010405 anode material Substances 0.000 description 5
- 239000010406 cathode material Substances 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 4
- 239000002932 luster Substances 0.000 description 4
- 239000000049 pigment Substances 0.000 description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 229910017604 nitric acid Inorganic materials 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 2
- 239000005711 Benzoic acid Substances 0.000 description 2
- 235000010233 benzoic acid Nutrition 0.000 description 2
- 238000005253 cladding Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical compound OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 description 2
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 description 1
- 235000010323 ascorbic acid Nutrition 0.000 description 1
- 229960005070 ascorbic acid Drugs 0.000 description 1
- 239000011668 ascorbic acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 231100000315 carcinogenic Toxicity 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 239000006115 industrial coating Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000003447 ipsilateral effect Effects 0.000 description 1
- 230000000670 limiting effect Effects 0.000 description 1
- 239000001630 malic acid Substances 0.000 description 1
- 235000011090 malic acid Nutrition 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- FJKROLUGYXJWQN-UHFFFAOYSA-N papa-hydroxy-benzoic acid Natural products OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229960004889 salicylic acid Drugs 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 239000011975 tartaric acid Substances 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
- B22F1/145—Chemical treatment, e.g. passivation or decarburisation
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/005—Apparatus specially adapted for electrolytic conversion coating
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Water Treatment By Electricity Or Magnetism (AREA)
Abstract
The invention discloses a kind of anodic oxidation device and using the method for device aluminium powder anodic oxidation in acid condition.The anodic oxidation device includes cathode groove body, separation bag and anode, and acidic electrolysis bath is held in cathode groove body, and the separation bag immersed in acidic electrolysis bath contacts metal-powder with cathode groove body；At least metal agitating paddle component insertion of anode is dipped in the separation bag of acidic electrolysis bath.The anodic oxidation device structure novel, avoids the short circuit of anode and cathode, improve the dispersibility of aluminium powder, it is ensured that it is contacted with acidic electrolysis bath at any time with anode, improves aluminium powder anodic oxidation effect.The present invention carries out anodic oxidation to aluminium powder under specific solutions of weak acidity using the anodic oxidation device, control voltage, anodic current density, temperature, the pH value of acidic electrolysis bath and conductivity etc., stability of the aluminium powder in water paint is effectively increased, avoids aluminium from reacting the hydrogen generated with water and induces combustion/explosion.
Description
Technical field
The present invention relates to the field of surface treatment of metal-powder, it is related to a kind of anodic oxidation device and using the device in acid
The method of aluminium powder anodic oxidation under the conditions of property.
Background technique
Metallic pigments can make the article being coated bright and colourful as a kind of important decorative pigment, with what is become clear
Metallic luster and metallic travel are widely used in industrial production and life.Coating is important metallic pigments with aluminium powder
One of, it can be used as industrial coating, car paint, printing ink and Plastics Processing Industry.
That there are dispersion stabilizations is poor for water paint for aluminium pigment, the problems such as being easily corroded and gradually lose metallic luster,
Even there is also being reacted because of aluminium with water caused by combustion/explosion problem.Current surface modifying method mainly has addition corrosion inhibiter
Method and cladding embrane method, however, there are still following problems:
1. passivator used in aluminium powder surface passivating treatment containing the Cr VI harmful and carcinogenic to environment, has limited mostly
System uses；
2. cladding process handles the complex process of aluminium powder, higher cost, it is difficult to form fine and close protective layer on aluminium powder surface；
3. additive is since suction-operated is weaker, extremely limited to the effect for inhibiting aluminium powder corrosion.
Summary of the invention
For the above-mentioned problems in the prior art, the purpose of the present invention is to provide a kind of anodic oxidation device and adopt
With the method for device aluminium powder anodic oxidation in acid condition.Anodic oxidation device structure novel of the invention, not only avoids
The short circuit of anode and cathode, also substantially increases the dispersibility of aluminium powder, and ensure that it is at any time connect with acidic electrolysis bath with anode
Touching, improves aluminium powder anodic oxidation effect.The present invention is using the anodic oxidation device in specific non-volatile faintly acid
Under the conditions of to aluminium powder carry out anodic oxidation, control voltage, anodic current density, temperature, the pH value of acidic electrolysis bath and acidity electricity
The conductivity etc. for solving liquid, can effectively improve stability of the aluminium powder in water paint, and aluminium is avoided to react the hydrogen generated with water
Induce combustion/explosion.
In order to achieve the above object, the invention adopts the following technical scheme:
In a first aspect, the present invention provides a kind of anodic oxidation device, the anodic oxidation device includes cathode groove body, separation
Bag and anode hold acidic electrolysis bath in cathode groove body, and separation bag immerses in acidic electrolysis bath, and separation bag wraps up metal-powder
Contact metal-powder with cathode groove body；
The anode includes metal agitating paddle component, and at least metal agitating paddle component insertion of anode is dipped in acidic electrolysis
In the separation bag of liquid.
In the present invention, " the cathode groove body " refers to: holding the groove body of acidic electrolysis bath as cathode.
Anode in the present invention is the anode with metal agitating paddle, that is to say, that metal agitating paddle is also the one of anode
Part, i.e. building block.
In the present invention, " at least metal agitating paddle component " refers to: can there was only metal agitating paddle component；It can also be existing
Metal agitating paddle component has the other parts of anode again.
As the optimal technical scheme of anodic oxidation device of the present invention, the separation bag is filter bag or diaphragm bag, institute
The aperture for stating separation bag is preferably smaller than the partial size of metal powder, and the purpose being arranged in this way is: on the one hand, make metal powder not with cathode can
Body contact；On the other hand, since the aperture of separation bag is less than the partial size of metal powder, metal powder can not be pierced by from separation bag, with gold
Belong to agitating paddle and be located at ipsilateral, mixing effect is good, good with the contact of anode, is conducive to the anodic oxidation of metal powder.
Preferably, the material of the cathode groove body includes any one in Titanium, platinum, gold, stainless steel or graphite, but
It is not limited to the above-mentioned material enumerated, other cathode materials that can reach same effect commonly used in the art can also be used for this hair
It is bright.
Preferably, the material of the anode includes any one in Titanium, platinum, gold or stainless steel, but is not limited to
The above-mentioned material enumerated, other anode materials that can reach same effect commonly used in the art can also be used for the present invention.
Second aspect carries out aluminium powder anodic oxygen using anodic oxidation device described in first aspect the present invention provides a kind of
The method of change, the described method comprises the following steps:
(1) aluminium powder is wrapped up with separation bag, contacts aluminium powder with cathode groove body, and by at least metal agitating paddle portion of anode
Part is inserted into separation bag, is then placed in the cathode groove body containing acidic electrolysis bath；
(2) the metal agitating paddle of starting cathode is stirred, and connects DC power supply, carries out aluminium powder anodic oxidation；
(3) it is detached from anode and separation bag, gained aluminium powder is taken out with separation bag then, obtains the aluminium powder of anodic oxidation；
Wherein, the acidic electrolysis bath is the acidic electrolysis bath of non-performance property, and pH value is 3~7 and is free of 7；
The non-volatile acidic electrolysis bath is boric acid, ammonium dihydrogen phosphate, monoammonium phosphate, adipic acid, glutaric acid, richness
In horse acid, azelaic acid or hexadecylic acid any one or at least two aqueous solution.
In method of the invention, the acidic electrolysis bath is non-volatile faintly acid, and pH is 3~7 and without 7, such as
It is 3,3.5,4,4.5,5,5.2,5.5,6 or 6.5 etc..
In non-volatile acidic electrolysis bath of the invention, described at least two aqueous solution is typical but non-limiting example
Have: the aqueous solution of the aqueous solution of boric acid and ammonium dihydrogen phosphate, boric acid and adipic acid, the water of boric acid, monoammonium phosphate and glutaric acid
The aqueous solution of solution, ammonium dihydrogen phosphate and monoammonium phosphate, adipic acid, glutaric acid, fumaric acid and azelaic acid aqueous solution, boron
Acid, azelaic acid and aqueous solution of hexadecylic acid etc..
In the present invention, aluminium powder is wrapped up by using the separation bag (such as filter bag or diaphragm bag) of suitable mesh number, aluminium is isolated
Then the insertion at least filter bag of the metal agitating paddle of anode or diaphragm bag are immersed in acidic electrolysis bath, start band by powder and cathode
The anode of stirring action, makes aluminium powder contact anode at any time, the anodic oxidation of aluminium powder is realized after powering on, thus in the table of aluminium powder
Face forms the adjustable oxide film of high quality of thickness, and then improves stability of the aluminium powder in application in water paint, avoids
The metallic luster of aluminium powder is destroyed, and is efficiently solved aluminium powder and is easy to react with water, cause generate hydrogen induce burning/it is quick-fried
Fried problem.
As the optimal technical scheme of the method for the invention, the solvent of the acidic electrolysis bath is water, and each component
Content are as follows: 5~100g/L of boric acid, ammonium dihydrogen phosphate 0.1-10g/L, monoammonium phosphate 0.1-10g/L g/L, adipic acid 0.1-
20g/L g/L, glutaric acid 0.1-20g/L, fumaric acid 0.1-20g/L, azelaic acid 0.1-20g/L and hexadecylic acid 0.1-20g/L.
In this optimal technical scheme, the content of boric acid is 5~100g/L, for example, 5g/L, 10g/L, 15g/L, 20g/L,
30g/L, 35g/L, 40g/L, 50g/L, 60g/L, 75g/L, 85g/L, 90g/L or 100g/L etc..
In this optimal technical scheme, the content of ammonium dihydrogen phosphate is 0.1-10g/L, for example, 0.1g/L, 1g/L, 2g/L,
2.5g/L, 3g/L, 4g/L, 5g/L, 6g/L, 7g/L, 8g/L, 9g/L or 10g/L etc..
In this optimal technical scheme, the content of monoammonium phosphate is 0.1-10g/L, for example, 0.1g/L, 1g/L, 2g/L,
2.5g/L, 3g/L, 3.5g/L, 4g/L, 5g/L, 6g/L, 6.5g/L, 7g/L, 8g/L, 9g/L or 10g/L etc..
In this optimal technical scheme, the content of adipic acid is 0.1-20g/L, for example, 0.1g/L, 0.5g/L, 1g/L, 3g/L,
5g/L、6g/L、7g/L、8g/L、9g/L、9.5g/L、10g/L、11g/L、11.5g/L、12.5g/L、13g/L、15g/L、16g/
L, 17g/L, 18.5g/L or 20g/L etc..
In this optimal technical scheme, the content of glutaric acid is 0.1-20g/L, for example, 0.1g/L, 0.5g/L, 1g/L, 3g/L,
4g/L、6g/L、6.5g/L、8g/L、9g/L、10g/L、11g/L、12.5g/L、13g/L、13.5g/L、15g/L、16g/L、17g/
L, 18.5g/L or 20g/L etc..
In this optimal technical scheme, the content of fumaric acid is 0.1-20g/L, for example, 0.1g/L, 0.5g/L, 1g/L, 3g/L,
4g/L, 6g/L, 8g/L, 9g/L, 10g/L, 11g/L, 12.5g/L, 13g/L, 15g/L, 16g/L, 17g/L, 18g/L or 20g/L
Deng.
In this optimal technical scheme, the content of azelaic acid is 0.1-20g/L, for example, 0.1g/L, 0.5g/L, 1g/L, 3g/L,
4g/L, 6g/L, 8g/L, 9g/L, 10g/L, 11g/L, 12.5g/L, 14g/L, 15g/L, 16g/L, 17g/L, 18g/L or 20g/L
Deng.
In this optimal technical scheme, the content of hexadecylic acid is 0.1-20g/L, for example, 0.1g/L, 0.5g/L, 1g/L, 3g/L,
4g/L, 6g/L, 8.5g/L, 9g/L, 10g/L, 11g/L, 12.5g/L, 13g/L, 15g/L, 16g/L, 17g/L, 18g/L or 20g/
L etc..
In this optimal technical scheme, " g/L " refers to: content of each component relative to 1L acidic electrolysis bath.
It is highly preferred that the solvent of the acidic electrolysis bath is water, and the content of each component are as follows: 30~80g/L of boric acid, phosphoric acid
Ammonium dihydrogen 1-5g/L, monoammonium phosphate 0.5-5g/L, adipic acid 0.5-10g/L, glutaric acid 0.5-10g/L, fumaric acid 0.5-
10g/L, azelaic acid 0.5-10g/L and hexadecylic acid 0.5-10g/L.
In the present invention, the pattern of aluminium powder is not especially limited, for example, can be ball aluminum powder, flake aluminum or other not
In regular aluminium powder any one or at least two combination, preferably flake aluminum.
Preferably, the partial size of the aluminium powder be 1~100 μm, such as 1 μm, 5 μm, 10 μm, 12 μm, 14 μm, 20 μm, 25 μm,
30 μm, 40 μm, 45 μm, 50 μm, 60 μm, 70 μm, 80 μm or 100 μm etc..
Preferably, the thickness of the flake aluminum is preferably 50~500nm, for example, 50nm, 100nm, 150nm, 200nm,
220nm, 260nm, 300nm, 350nm, 400nm, 450nm or 500nm etc..
As the optimal technical scheme of the method for the invention, the aluminium powder accounts for the 5~50% of acidic electrolysis bath total weight,
Such as 5%, 10%, 15%, 18%, 20%, 25%, 30%, 35%, 40%, 45% or 50% etc..If mass ratio less than 5%,
The inefficiency of aluminium powder anodic oxidation will lead to the slurry system of acidic electrolysis bath and aluminium powder composition if mass ratio is greater than 50%
Viscosity is excessively high, is unfavorable for the abundant anodic oxidation of aluminium powder.
Preferably, the rate of the stirring in 1000rpm hereinafter, such as 950rpm, 900rpm, 850rpm, 800rpm,
750rpm, 700rpm, 600rpm, 500rpm, 400rpm, 300rpm, 200rpm or 100rpm etc., preferably 400~700rpm,
In this preferred scope, it can both guarantee that aluminium powder was sufficiently mixed in acidic electrolysis bath, and come into full contact with anode, and can be to avoid
Because mixing speed it is too fast caused by whirlpool is too deep that acidic electrolysis bath or aluminium powder overflow is caused to go out groove body.
As the optimal technical scheme of the method for the invention, during the aluminium powder anodic oxidation, control voltage exists
10~240V, anodic current density are 0.5~6A/100cm2, temperature is 30~55 DEG C, the pH value of acidic electrolysis bath 3~7 and
Without 7, the conductivity of acidic electrolysis bath is 100 μ s/cm~10ms/cm.
In this optimal technical scheme, control voltage in 10~240V, such as 10V, 20V, 35V, 50V, 65V, 80V, 100V,
120V, 150V, 170V, 200V, 220V, 230V or 240V etc..
In this optimal technical scheme, anodic current density is 0.5~6A/100cm2, such as 0.5A/100cm2、1A/
100cm2、2A/100cm2、2.5A/100cm2、3A/100cm2、3.5A/100cm2、4A/100cm2、5A/100cm2Or 6A/
100cm2Deng.If anodic current density is lower than 0.5A/100cm2, then the efficiency of anodic oxidation is too low；If anodic current density is higher than
6A/100cm2, then will lead to the quality decline of oxidation film.
In this optimal technical scheme, temperature be 30~55 DEG C, such as 30 DEG C, 35 DEG C, 40 DEG C, 45 DEG C, 50 DEG C, 52.5 DEG C or
55 DEG C etc..
In this optimal technical scheme, the pH value of acidic electrolysis bath 3~7 and be free of 7, such as 3,3.5,4,4.5,5,6,
6.5 or 6.7 etc..
In this optimal technical scheme, the conductivity of acidic electrolysis bath is 100 μ s/cm~10ms/cm, such as 100 μ s/cm,
500μs/cm、800μs/cm、1ms/cm、2ms/cm、3ms/cm、5ms/cm、6ms/cm、7ms/cm、8ms/cm、8.5ms/cm、
9ms/cm or 10ms/cm.If conductivity is lower than 100 μ s/cm, the partial pressure that will lead to acidic electrolysis bath is excessively high, and calorific value increases, energy
Consumption increases；If conductivity is higher than 10ms/cm, it may occur that the oxidation film of scintillation phenomenon, aluminium powder surface is breakdown, destroys oxidation
The integrality of film.
It is highly preferred that controlling voltage in 20~180V, anodic current density 1 during the aluminium powder anodic oxidation
~5A/100cm2, temperature is 35-45 DEG C, and the pH value of acidic electrolysis bath 3~7 and is being free of 7, and the conductivity of acidic electrolysis bath is
1ms/cm~9ms/cm.
Preferably, the time of the aluminium powder anodic oxidation be 10~50min, such as 10min, 15min, 20min, 25min,
30min, 35min, 40min or 50min etc..
As the optimal technical scheme of the method for the invention, the method also includes taking out aluminium powder with separation bag, directly
Tap into the step of row centrifugal filtration, washing and drying.
Preferably, it is washed using pure water, the number of washing is preferably 3~5 times.
Preferably, the temperature of the drying is 45~80 DEG C, such as 45 DEG C, 50 DEG C, 55 DEG C, 60 DEG C, 65 DEG C, 70 DEG C or 80
DEG C etc..
As the further preferred technical solution of the method for the invention, the described method comprises the following steps:
(1) aluminium powder is wrapped up with filter bag or diaphragm bag, contacts aluminium powder with cathode groove body, and by the metal agitating paddle of anode
Component is inserted into filter bag or diaphragm bag, is then placed in the cathode groove body containing acidic electrolysis bath；
(2) the metal agitating paddle of starting cathode is stirred, stirring rate in 1000rpm hereinafter, and connect DC power supply,
Voltage is controlled in 10~240V, anodic current density is 0.5~6A/100cm2, temperature is 30~55 DEG C, the pH of acidic electrolysis bath
Value 3~7 and is being free of 7, and the conductivity of acidic electrolysis bath is 100 μ s/cm~10ms/cm, carry out aluminium powder anodic oxidation 10~
50min；
(3) metal agitating paddle component is taken out from filter bag or diaphragm bag, separates anode with filter bag or diaphragm bag, then
Gained aluminium powder is taken out with filter bag or diaphragm bag, directly progress centrifugal filtration, washing and drying obtains the aluminium powder of anodic oxidation.
The acidic electrolysis bath is non-volatile acidic electrolysis bath, and the pH value of the acidic electrolysis bath is 3~7 and is free of
7；
The solvent of the non-volatile acidic electrolysis bath is water, and the content of each component are as follows: 5~100g/L of boric acid, phosphorus
Acid dihydride ammonium 0.1-10g/L, monoammonium phosphate 0.1-10g/L g/L, adipic acid 0.1-20g/L g/L, glutaric acid 0.1-20g/
L, fumaric acid 0.1-20g/L, azelaic acid 0.1-20g/L or hexadecylic acid 0.1-20g/L.
Compared with the prior art, the invention has the following beneficial effects:
(1) the invention proposes a kind of easy devices that can be used for aluminium powder anodic oxidation, including cathode groove body, separation bag
(such as filter bag or diaphragm bag) and anode hold acidic electrolysis bath in cathode groove body, and separation bag immerses in acidic electrolysis bath, and point
Metal-powder is contacted with cathode groove body from bag package metal-powder；The anode includes metal agitating paddle component, and anode
At least metal agitating paddle component insertion be dipped in the separation bag of acidic electrolysis bath.Anodic oxidation device structure provided by the invention
Uniqueness, anode and aluminium powder with metal agitating paddle are located at the side of separation bag；And cathode is located at the other side, it is this unique to set
On the one hand meter avoids anode and cathode and contacted by aluminium powder occurs short circuit, on the other hand improves the dispersibility of aluminium powder and can protect
It demonstrate,proves it and is contacted at any time with acidic electrolysis bath with anode, improve aluminium powder anodic oxidation effect.
(2) it is carried out under non-volatile solutions of weak acidity the present invention also provides a kind of using the anodic oxidation device
The method of aluminium powder anodic oxidation, the method wrap up aluminium by introducing the separation bag (such as filter bag or diaphragm bag) of suitable mesh number
Powder, is on the one hand isolated aluminium powder and cathode avoids anode and cathode and short circuit occurs (because filter bag or diaphragm bag etc. separate by aluminium powder
Pocket gap is less than aluminium powder partial size, that is, can guarantee aluminium powder not Contact cathod, avoids cathode, anode that short circuit occurs), on the other hand make aluminium
The agitating paddle component of powder and the anode with agitating paddle is located on the inside of the separation bags such as filter bag or diaphragm bag, suitable stirring bar
Preferably dispersibility and the contact with anode and acidic electrolysis bath may be implemented in part.
(3) anodic oxidation device of the invention is utilized, aluminium powder is carried out using specific non-volatile faintly acid electrolyte
Anodic oxidation, control voltage, anodic current density, temperature, the pH value of acidic electrolysis bath and conductivity of acidic electrolysis bath etc., can
Quality is high, defect is few and the adjustable oxidation film of thickness to obtain on aluminium powder surface, inhibits liberation of hydrogen effect obvious, can effectively improve
Stability of the aluminium powder in water paint, avoids the metallic luster of aluminium powder from being destroyed, and solves aluminium powder and is easy to react with water
The problem of, avoid the hydrogen generated from inducing combustion/explosion.
(4) method of the invention can handle the aluminium powder of different-shape, for example, irregularly, sheet or ball aluminum powder, can basis
The aluminium powder of different-grain diameter is adjusted flexibly, replaces filter bag or diaphragm bag, not only avoids short circuit, but facilitate aluminium powder go out slot, separation and
Washing and cleaning operation, non-volatile weak acid environment are conducive to the formation of aluminium powder surface oxide film of high quality, and to operator,
The harm of equipment and environment is small, is suitble to continuous industrialized production.
Detailed description of the invention
Fig. 1 is the anodic oxidation device schematic diagram of embodiment 1, wherein 1- acidic electrolysis bath, 2- cathode groove body, 3- metal
Powder, 4- separation bag, 5- anode, the metal agitating paddle component of 51- anode.
Specific embodiment
To further illustrate the technical scheme of the present invention below with reference to the accompanying drawings and specific embodiments.
In the embodiment of the present invention, in the component of acidic electrolysis bath, " g/L " is contained relative to each component of 1L acidic electrolysis bath
Amount.
The calculating reference literature of collecting gas method and corrosion inhibition rate: Chen Yuqiong, Ye Hongqi, Liu Hui surfactant are located in advance
Dispersion and corrosion resisting property [J] material protection after managing coated aluminum powder polymer, 2010,43 (6): 16-18.
Embodiment 1
The present embodiment provides a kind of anodic oxidation device (its schematic diagram is referring to Fig. 1), the anodic oxidation device includes yin
Pole groove body 2, separation bag 4 and anode 5 hold acidic electrolysis bath 1 in cathode groove body 2, and separation bag 4 immerses in acidic electrolysis bath 1, and
Separation bag 4, which wraps up metal-powder 3, contacts metal-powder 3 with cathode groove body 2；
The anode 5 includes metal agitating paddle component 51, and the insertion of at least metal agitating paddle component 51 of anode 5 is dipped in acid
In the separation bag 4 of property electrolyte 1.
Embodiment 2
Aluminium powder anodic oxygen is carried out using anodic oxidation device described in embodiment 1 in acid condition the present embodiment provides a kind of
The method of change, the described method comprises the following steps:
The first step selects the filter bag of 200 mesh to be placed in the cathode groove body equipped with acidic electrolysis bath, and filter bag hole is less than aluminium powder
Partial size can guarantee aluminium powder not Contact cathod, avoid cathode, anode that short circuit occurs, will account for the aluminium of acidic electrolysis bath quality 35%
Powder is scattered in filter bag, and the metal agitating paddle component of anode is inserted into filter bag；
Second step starts the anode (anode i.e. with metal agitating paddle component) with stirring action, and mixing speed is
450rpm connects DC power supply, controls voltage in 140V, anodic current density 5A/100cm2, temperature 45 C, acidic electrolysis bath
PH value be 4.2, the conductivity of acidic electrolysis bath is 5.02ms/cm, and after 15min is handled, aluminium powder can go out with filter bag
Slot；
The resulting aluminium powder of second step is directly carried out centrifugal filtration with filter bag, and is washed 5 repeatedly with pure water by third step
Time, it is dry in 60 DEG C of baking oven, obtain the aluminium powder of anodic oxidation.
The flake aluminum that selected aluminium powder is 80-85 μm in the present embodiment, with a thickness of 400~450nm；Acidic electrolysis bath
For non-volatile faintly acid electrolyte, form as follows: boric acid 50g/L；Monoammonium phosphate 1g/L；Adipic acid 1g/L；Glutaric acid
1g/L；Selected anode material is stainless steel, and cathode material is graphite.
Aluminium powder after above-mentioned anodized has preferable corrosion resistance, collects aluminium powder and corrosion using drainage
The hydrogen that medium reaction is released, liberation of hydrogen corrosion inhibition rate have reached 96%.
Embodiment 3
Aluminium powder anodic oxygen is carried out using anodic oxidation device described in embodiment 1 in acid condition the present embodiment provides a kind of
The method of change, the described method comprises the following steps:
The first step selects the filter bag of 500 mesh to be placed in the cathode groove body equipped with acidic electrolysis bath, and filter bag hole is less than aluminium powder
Partial size can guarantee aluminium powder not Contact cathod, avoid cathode, anode that short circuit occurs, and will account for the aluminium powder point of electrolyte quality 15%
It dissipates in filter bag, and the metal agitating paddle component of anode is inserted into filter bag；
Second step starts the anode with stirring action, and (anode i.e. with metal agitating paddle component), mixing speed is
500rpm connects DC power supply, controls voltage in 80V, anodic current density 1A/100cm2, 40 DEG C of temperature, acidic electrolysis bath
PH value is 4.0, and the conductivity of acidic electrolysis bath is 6.19ms/cm, and after 20min is handled, aluminium powder can go out slot with filter bag；
The resulting aluminium powder of second step is directly carried out centrifugal filtration with filter bag, and is washed 4 repeatedly with pure water by third step
Time, it is dry in 70 DEG C of baking oven, obtain the aluminium powder of anodic oxidation.
The flake aluminum that selected aluminium powder is 30-36 μm in the present embodiment, with a thickness of 300~350nm；Acidic electrolysis bath
For non-volatile faintly acid electrolyte, form as follows: boric acid 60g/L；Ammonium dihydrogen phosphate 2g/L；Fumaric acid 0.5g/L；It is selected
Anode material is stainless steel, and cathode material is stainless steel.
Aluminium powder after above-mentioned anodized has preferable corrosion resistance, collects aluminium powder and corrosion using drainage
The hydrogen that medium reaction is released, liberation of hydrogen corrosion inhibition rate have reached 94%.
Embodiment 4
Aluminium powder anodic oxygen is carried out using anodic oxidation device described in embodiment 1 in acid condition the present embodiment provides a kind of
The method of change, the described method comprises the following steps:
The first step selects the filter bag of 2000 mesh to be placed in the cathode groove body equipped with acidic electrolysis bath, and filter bag hole is less than aluminium
Powder diameter can guarantee aluminium powder not Contact cathod, avoid cathode, anode that short circuit occurs, will account for the aluminium powder of electrolyte quality 45%
It is scattered in filter bag, and the metal agitating paddle component of anode is inserted into filter bag；
Second step starts the anode (anode i.e. with metal agitating paddle) with stirring action, and mixing speed 600rpm connects
Logical DC power supply controls voltage in 60V, anodic current density 4A/100cm2, 40 DEG C of temperature, the pH value of acidic electrolysis bath is
3.9, the conductivity of acidic electrolysis bath is 5.82ms/cm, and after 45min is handled, aluminium powder can go out slot with filter bag；
The resulting aluminium powder of second step is directly carried out centrifugal filtration with filter bag, and is washed 5 repeatedly with pure water by third step
Time, it is dry in 65 DEG C of baking oven, obtain the aluminium powder of anodic oxidation.
The flake aluminum that selected aluminium powder is 9-12 μm in the present embodiment, with a thickness of 200~250nm；Acidic electrolysis bath
For non-volatile faintly acid electrolyte, form as follows: boric acid 60g/L；Monoammonium phosphate 1g/L；Ammonium dihydrogen phosphate 1g/L；Penta
Diacid 2g/L；Hexadecylic acid 2g/L；Selected anode material is stainless steel, and cathode material is graphite.
Aluminium powder after above-mentioned anodized has preferable corrosion resistance, collects aluminium powder and corrosion using drainage
The hydrogen that medium reaction is released, liberation of hydrogen corrosion inhibition rate have reached 93%.
Embodiment 5
Aluminium powder anodic oxygen is carried out using anodic oxidation device described in embodiment 1 in acid condition the present embodiment provides a kind of
The method of change, the described method comprises the following steps:
The first step selects the filter bag of 15000 mesh to be placed in the cathode groove body equipped with acidic electrolysis bath, and filter bag hole is less than aluminium
Powder diameter can guarantee aluminium powder not Contact cathod, avoid cathode, anode that short circuit occurs, and will account for the aluminium powder point of electrolyte quality 5%
It dissipates in filter bag, and the metal agitating paddle component of anode is inserted into filter bag；
Second step starts the anode (anode i.e. with metal agitating paddle component) with stirring action, and mixing speed is
600rpm connects DC power supply, controls voltage in 20V, anodic current density 1.5A/100cm2, 30 DEG C of temperature, acidic electrolysis bath
PH value 3.5 be that the conductivity of acidic electrolysis bath is 5.91ms/cm, and after 10min is handled, aluminium powder can go out with filter bag
Slot；
The resulting aluminium powder of second step is directly carried out centrifugal filtration with filter bag, and is washed 5 repeatedly with pure water by third step
Time, it is dry in 75 DEG C of baking oven, obtain the aluminium powder of anodic oxidation.
The flake aluminum that selected aluminium powder is 2-6 μm in the present embodiment, with a thickness of 100~150nm；Acidic electrolysis bath is
Non-volatile faintly acid electrolyte forms as follows: boric acid 80g/L；Ammonium dihydrogen phosphate 3g/L；Adipic acid 2g/L；Azelaic acid 1g/
L；Selected anode material is stainless steel, and cathode material is stainless steel.
Aluminium powder after above-mentioned anodized has preferable corrosion resistance, collects aluminium powder and corrosion using drainage
The hydrogen that medium reaction is released, liberation of hydrogen corrosion inhibition rate have reached 93%.
Embodiment 6
The present embodiment the difference from example 2 is that:
In the first step, disperse the aluminium powder for accounting for acidic electrolysis bath quality 10% in filter bag；
In second step, voltage is controlled in 100V, current density 3A/100cm2, temperature is 45 DEG C.
Aluminium powder after above-mentioned anodized has preferable corrosion resistance, collects aluminium powder and corrosion using drainage
The hydrogen that medium reaction is released, liberation of hydrogen corrosion inhibition rate have reached 95%.
Embodiment 7
The present embodiment and the difference of embodiment 3 are:
Acidic electrolysis bath is non-volatile faintly acid electrolyte, is formed as follows: boric acid 60g/L；Adipic acid 10g/L, ten
Six acid 0.5g/L；Fumaric acid 2g/L；
In the first step, disperse the aluminium powder for accounting for acidic electrolysis bath quality 20% in filter bag；
In second step, voltage is controlled in 75V, current density 3A/100cm2, temperature is 35 DEG C.
Aluminium powder after above-mentioned anodized has preferable corrosion resistance, collects aluminium powder and corrosion using drainage
The hydrogen that medium reaction is released, liberation of hydrogen corrosion inhibition rate have reached 94%.
Embodiment 8
The present embodiment the difference from example 2 is that:
Acidic electrolysis bath is non-volatile faintly acid electrolyte, is formed as follows: monoammonium phosphate 5g/L；Adipic acid 15g/
L, azelaic acid 0.5g/L；Hexadecylic acid 10g/L；Fumaric acid 3.5g/L；
In the first step, disperse the aluminium powder for accounting for electrolyte quality 17% in filter bag；
In second step, voltage is controlled in 160V, current density 2.5A/100cm2, temperature is 36 DEG C.Through above-mentioned anodic oxygen
Changing treated aluminium powder has preferable corrosion resistance, collects the hydrogen that aluminium powder reacts with corrosive medium releasing using drainage,
Its liberation of hydrogen corrosion inhibition rate has reached 96%.
Comparative example 1
In addition to the composition of acidic electrolysis bath, other methods and condition are same as Example 2, concrete composition are as follows:
Nitric acid 20g/L；Sulfuric acid 15g/L；Hydrochloric acid 8g/L；Tartaric acid 4g/L；Benzoic acid 0.2g/L；Salicylic acid 6g/L；Coffee
Sour 0.3g/L.
Aluminium powder after above-mentioned anodized has preferable corrosion resistance, collects aluminium powder and corrosion using drainage
The hydrogen that medium reaction is released, liberation of hydrogen corrosion inhibition rate are 83%.
Comparative example 2
In addition to the composition of acidic electrolysis bath, other methods and condition are same as Example 3, concrete composition are as follows:
Nitric acid 25g/L；Sulfuric acid 20g/L；Oxalic acid 8g/L；Citric acid (citric acid) 4g/L；Benzoic acid 0.4g/L.
Aluminium powder after above-mentioned anodized has preferable corrosion resistance, collects aluminium powder and corrosion using drainage
The hydrogen that medium reaction is released, liberation of hydrogen corrosion inhibition rate are 82%.
Comparative example 3
In addition to the composition of acidic electrolysis bath, other methods and condition are same as Example 4, concrete composition are as follows:
Nitric acid 40g/L；Hydrochloric acid 10g/L；Malic acid 3g/L；Citric acid (citric acid) 4g/L；Ascorbic acid 2g/L.
Aluminium powder after above-mentioned anodized has preferable corrosion resistance, collects aluminium powder and corrosion using drainage
The hydrogen that medium reaction is released, liberation of hydrogen corrosion inhibition rate are 80%.
The Applicant declares that the present invention is explained by the above embodiments method detailed of the invention, but the present invention not office
Be limited to above-mentioned method detailed, that is, do not mean that the invention must rely on the above detailed methods to implement.Technical field
Technical staff it will be clearly understood that any improvement in the present invention, equivalence replacement and auxiliary element to each raw material of product of the present invention
Addition, selection of concrete mode etc., all of which fall within the scope of protection and disclosure of the present invention.
Claims (10)
1. a kind of use anodic oxidation device, which is characterized in that the anodic oxidation device includes:
Cathode groove body, separation bag and anode hold acidic electrolysis bath in cathode groove body, and separation bag immerses in acidic electrolysis bath, and
Separation bag package metal-powder contacts metal-powder with cathode groove body；
The anode includes metal agitating paddle component, and at least metal agitating paddle component insertion of anode is dipped in acidic electrolysis bath
In separation bag.
2. anodic oxidation device according to claim 1, which is characterized in that the separation bag is filter bag or diaphragm bag；
Preferably, the aperture of the separation bag is less than the partial size of metal powder.
3. anodic oxidation device according to claim 1 or 2, which is characterized in that the material of the cathode groove body includes gold
Belong to any one in titanium, platinum, gold, stainless steel or graphite；
Preferably, the material of the anode includes any one in Titanium, platinum, gold or stainless steel.
4. a kind of method for carrying out aluminium powder anodic oxidation using the described in any item anodic oxidation devices of claim 1-3, special
Sign is, the described method comprises the following steps:
(1) aluminium powder is wrapped up with separation bag, contacts aluminium powder with cathode groove body, and at least metal agitating paddle component of anode is inserted
Enter in separation bag, is then placed in the cathode groove body containing acidic electrolysis bath；
(2) the metal agitating paddle of starting cathode is stirred, and connects DC power supply, carries out aluminium powder anodic oxidation；
(3) it is detached from anode and separation bag, gained aluminium powder is taken out with separation bag then, obtains the aluminium powder of anodic oxidation；
Wherein, the acidic electrolysis bath is non-volatile acidic electrolysis bath, and pH value is 3~7 and is free of 7；
The non-volatile acidic electrolysis bath is boric acid, ammonium dihydrogen phosphate, monoammonium phosphate, adipic acid, glutaric acid, rich horse
In acid, azelaic acid or hexadecylic acid any one or at least two aqueous solution.
5. according to the method described in claim 4, it is characterized in that, the solvent of the acidic electrolysis bath is water, and each component
Content are as follows: 5~100g/L of boric acid, ammonium dihydrogen phosphate 0.1-10g/L, monoammonium phosphate 0.1-10g/L g/L, adipic acid 0.1-
20g/L, glutaric acid 0.1-20g/L, fumaric acid 0.1-20g/L, azelaic acid 0.1-20g/L and hexadecylic acid 0.1-20g/L；
Preferably, the solvent of the acidic electrolysis bath is water, and the content of each component are as follows: 30~80g/L of boric acid, ammonium dihydrogen phosphate
1-5g/L, monoammonium phosphate 0.5-5g/L, adipic acid 0.5-10g/L, glutaric acid 0.5-10g/L, fumaric acid 0.5-10g/L, nonyl
Diacid 0.5-10g/L and hexadecylic acid 0.5-10g/L.
6. method according to claim 4 or 5, which is characterized in that the separation bag is filter bag or diaphragm bag；
Preferably, the aluminium powder be ball aluminum powder, flake aluminum or irregular aluminium powder in any one or at least two group
It closes, preferably flake aluminum；
Preferably, the partial size of the aluminium powder is 1~100 μm；
Preferably, the thickness of the flake aluminum is preferably 50~500nm.
7. according to the described in any item methods of claim 4-6, which is characterized in that the aluminium powder accounts for acidic electrolysis bath total weight
5~50%；
Preferably, the rate of the stirring is in 1000rpm hereinafter, it is preferred that 400~700rpm.
8. according to the described in any item methods of claim 4-7, which is characterized in that during the aluminium powder anodic oxidation, control
For voltage processed in 10~240V, anodic current density is 0.5~6A/100cm2, temperature is 30~55 DEG C, the pH value of acidic electrolysis bath
3~7 and be free of 7, the conductivity of acidic electrolysis bath is 100 μ s/cm~10ms/cm；
Preferably, during the aluminium powder anodic oxidation, for control voltage in 20~180V, anodic current density is 1~5A/
100cm2, temperature is 35~45 DEG C, and the pH value of acidic electrolysis bath 3~7 and is being free of 7, and the conductivity of acidic electrolysis bath is 1ms/
Cm~9ms/cm；
Preferably, the time of the aluminium powder anodic oxidation is 10~50min.
9. according to the described in any item methods of claim 4-8, which is characterized in that the method also includes by aluminium powder with separation bag
It takes out, directly carries out the step of centrifugal filtration, washing and drying；
Preferably, it is washed using pure water, the number of washing is preferably 3~5 times；
Preferably, the temperature of the drying is 45~80 DEG C.
10. according to the described in any item methods of claim 4-9, which is characterized in that the described method comprises the following steps:
(1) aluminium powder is wrapped up with filter bag or diaphragm bag, contacts aluminium powder with cathode groove body, and by the metal agitating paddle component of anode
It is inserted into filter bag or diaphragm bag, is then placed in the cathode groove body containing acidic electrolysis bath；
(2) the metal agitating paddle of starting cathode is stirred, stirring rate in 1000rpm hereinafter, and connect DC power supply, control
For voltage in 10~240V, anodic current density is 0.5~6A/100cm2, temperature is 30~55 DEG C, and the pH value of acidic electrolysis bath exists
3~7 and be free of 7, the conductivity of acidic electrolysis bath is 100 μ s/cm~10ms/cm, carries out 10~50min of aluminium powder anodic oxidation；
(3) metal agitating paddle component is taken out from filter bag or diaphragm bag, separates anode with filter bag or diaphragm bag, then by institute
It obtains aluminium powder to take out with filter bag or diaphragm bag, directly progress centrifugal filtration, washing and drying obtains the aluminium powder of anodic oxidation.
The acidic electrolysis bath is non-volatile acidic electrolysis bath, and pH value is 3~7 and is free of 7；
The solvent of the non-volatile acidic electrolysis bath is water, and the content of each component are as follows: 5~100g/L of boric acid, di(2-ethylhexyl)phosphate
Hydrogen ammonium 0.1-10g/L, monoammonium phosphate 0.1-10g/L g/L, adipic acid 0.1-20g/Lg/L, glutaric acid 0.1-20g/L, rich horse
Sour 0.1-20g/L, azelaic acid 0.1-20g/L or hexadecylic acid 0.1-20g/L.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101198726A (en) * | 2005-06-17 | 2008-06-11 | 国立大学法人东北大学 | Metal oxide film, laminated body, metal member and manufacturing method thereof |
| CN101651048A (en) * | 2009-06-23 | 2010-02-17 | 吴江飞乐天和电子材料有限公司 | Formation method of electrode foil of aluminum electrolytic capacitor |
| CN102554212A (en) * | 2010-12-23 | 2012-07-11 | 中国科学院金属研究所 | Method for inhibiting hydrogen separation through anodic oxidation of aluminum powder under acidic condition |
| CN104988553A (en) * | 2015-06-16 | 2015-10-21 | 马淑云 | High purity alumina powder preparing device and method |
| CN105297078A (en) * | 2014-06-17 | 2016-02-03 | 中山大学 | Ultrasonic-assisted pulp electrolysis method for tailing sand |
-
2017
- 2017-09-18 CN CN201710840182.7A patent/CN109518247A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101198726A (en) * | 2005-06-17 | 2008-06-11 | 国立大学法人东北大学 | Metal oxide film, laminated body, metal member and manufacturing method thereof |
| CN101651048A (en) * | 2009-06-23 | 2010-02-17 | 吴江飞乐天和电子材料有限公司 | Formation method of electrode foil of aluminum electrolytic capacitor |
| CN102554212A (en) * | 2010-12-23 | 2012-07-11 | 中国科学院金属研究所 | Method for inhibiting hydrogen separation through anodic oxidation of aluminum powder under acidic condition |
| CN105297078A (en) * | 2014-06-17 | 2016-02-03 | 中山大学 | Ultrasonic-assisted pulp electrolysis method for tailing sand |
| CN104988553A (en) * | 2015-06-16 | 2015-10-21 | 马淑云 | High purity alumina powder preparing device and method |
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