CN103590086A - Nickel-free hole sealing agent for aluminum alloy and hole sealing treatment process of agent - Google Patents
Nickel-free hole sealing agent for aluminum alloy and hole sealing treatment process of agent Download PDFInfo
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- CN103590086A CN103590086A CN201310567738.1A CN201310567738A CN103590086A CN 103590086 A CN103590086 A CN 103590086A CN 201310567738 A CN201310567738 A CN 201310567738A CN 103590086 A CN103590086 A CN 103590086A
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Abstract
The invention discloses a nickel-free hole sealing agent for an aluminum alloy. The nickel-free hole sealing agent comprises water solutions of fluorotitanic acid, a corrosion inhibitor and a chelating agent, wherein on the basis of the volume of the hole sealing agent, the concentration of the fluorotitanic acid is 6.0-9.0 g/L, the concentration of the corrosion inhibitor is 1.0-3.0 g/L and the concentration of the chelating agent is 1.0-3.0 g/L. The hole sealing agent takes the fluorotitanic acid as the main ingredient, and pollution of nickel salt to the aluminum alloy and the water quality is eliminated from the source. The invention further provides a hole sealing treatment process using the nickel-free hole sealing agent for the aluminum alloy. The operation is simple, energy conservation and environment protection are realized, waste water is easy to treat, the hole sealing agent is suitable for large-scale production, nickel pollution in the building aluminum alloy finished surface treatment process, the aluminum alloy using process and the waste treatment process is completely ended, and the bottleneck problem about restricting the industry development over the years is solved.
Description
Technical field
The invention belongs to the chemically treated technical field of metal material surface, particularly a kind of to oxidized aluminum alloy rete carry out sealing of hole processing without nickel hole sealing agent and hole-sealing treatment process thereof.
Background technology
At present, China's building aluminium alloy anode oxide sealing of hole mainly adopts cold hole-sealing technology and middle temperature hole-sealing technology, and nickel salt is the main component of hole sealing agent.
The aluminium alloy sealing technical process of prior art, first carries out pre-treatment by aluminium alloy as shown in Figure 1, then carries out anodic oxidation and electrolytic coloring, then carries out sealing of hole processing again.After sealing of hole, need to wash processing through washing 1 and washing baths more than washing 2 twice, the residual nickeliferous sealing of hole liquid of aluminum alloy surface in anode purge oxidation sealing of hole process, can descend wire wrapping.This sealing of hole processing mode, the metallic nickel that can produce following two aspects is compound polluted: the one, the nickel contamination in rinse water, the 2nd, the nickel contamination of the aluminum alloy surface that sealing of hole was processed.At present, various Al-alloy products, comprise that various electronic products go deep into the daily life of ordinary populace day by day, and international cancer research general administration (IARC), as far back as nineteen ninety, nickel compound has been classified as at people and the animal equal sufficient first group of carcinogens of cancer evidence with it, therefore the potential injury that, nickeliferous hole sealing technology causes environment and human body must cause the great attention of aluminium processing industry.
Summary of the invention
To the object of the invention is the problem that has serious nickel contamination in existing aluminium alloy sealing treating processes in order solving, to provide a kind of aluminium alloy without nickel hole sealing agent and hole-sealing treatment process thereof, promote aluminum alloy surface treatment technology to environmental protection, efficient, energy saving direction development.
Technical scheme of the present invention is achieved in that
The invention provides a kind of aluminium alloy without nickel hole sealing agent, comprise hydrofluotitanic acid, the aqueous solution of inhibiter and sequestrant, the volume of hole sealing agent of take is benchmark, the concentration of described hydrofluotitanic acid is 6.0-9.0g/L, and the concentration of described inhibiter is 1.0-3.0g/L, and the concentration of described sequestrant is 1.0-3.0g/L.
Preferably, described inhibiter be ethylene glycol, glycerol and sorbyl alcohol one or more.
Preferably, described sequestrant is one or more in trolamine, ethylenediamine tetraacetic acid (EDTA), tripoly phosphate sodium STPP, trisodium phosphate, sodium-metaphosphate, Amino Trimethylene Phosphonic Acid and phosphinylidyne butane tricarboxylic acid.
Preferably, described hole sealing agent working temperature is 20-30 ℃, and the pH value of described hole sealing agent is 3.0-4.0.
The present invention also provides a kind of aluminium alloy without nickel hole-sealing treatment process, and aluminum alloy base material, by processing without nickel process unit, is comprised the steps:
(1) will be heated to 15-35 ℃ without nickel hole sealing agent, the aluminum alloy base material after anodic oxidation is immersed in hole sealing agent without nickel, sealing of hole speed is 1-3 μ m/min;
(2) hole sealing agent of the aluminum alloy base material remained on surface through soaking without nickel hole sealing agent of step (1) gained is washed, after flushing, dried up, pack.
Preferably, describedly without nickel process unit, comprise production system, heating system, gas agitating system, filtering system and Waste Water Treatment;
Described production system comprises 1# sealing of hole groove, 2# washing bath and 3# washing bath, and described 1# sealing of hole groove is main work nest, and for completing the sealing of hole of Process on Aluminum Alloy Oxidation Film, described 2# washing bath and 3# washing bath are for cleaning the residual hole sealing agent of aluminum alloy surface after sealing of hole;
Described heating system comprises steam heating tube and be arranged at the 8# valve on described steam heating tube, and described steam heating tube is arranged at respectively the both sides of described 1# sealing of hole groove, for the heating of described 1# sealing of hole groove;
Described Waste Water Treatment is comprised of 2# washing bath, 3# washing bath, 4# settling bath, acid proof pump, strainer, 3# valve, 4# valve, 5# valve and pipeline, described Waste Water Treatment, for purifying the scavenging solution of described 2# washing bath and 3# washing bath, is realized cycling utilization of wastewater;
Described gas agitating system comprises air compressor machine, feed channel and is arranged at 6# valve and the 7# valve in described feed channel, and described gas agitating system is for the uniform stirring of described 1# sealing of hole groove and 4# settling bath solution;
Described filtering system is connected to form by 1# sealing of hole groove, 2# washing bath, 3# washing bath, 4# settling bath, acid proof pump, strainer, 1# valve, 2# valve, 3# valve, 4# valve, 5# valve and pipeline, and described filtering system is for the filtration of described 1# sealing of hole groove, described 2# washing bath and 3# washing bath water lotion.
Preferably, open 8# valve, heat described 1# sealing of hole groove, open 3# valve, 4# valve, 5# valve, start acid proof pump, the water lotion in 4# settling bath, to 2# washing bath and 3# washing bath, then returns to 4# settling bath;
After oxidized aluminum alloy, in 1# sealing of hole groove, sealing of hole speed is 1-3 μ m/min, after sealing of hole completes, and through 2# washing bath and 3# washing bath, cleaning aluminum alloy remained on surface hole sealing agent, then air-dry, packing.
Preferably, during described 1# sealing of hole groove heating, described 8# valve is controlled hole sealing agent temperature automatically between 20-30 ℃.
Preferably, after adding without nickel hole sealing agent, open 7# valve in described 1# sealing of hole groove, the hole sealing agent in by described gas agitating system, 1# sealing of hole groove being stirred is mixed evenly, continues to produce; Close 3# valve, 4# valve, 5# valve, open gas agitating 6# valve, unslaked lime is added to 4# settling bath, limit edged stirs, to pH value be 8.0 o'clock, stop adding unslaked lime and stirring.
Preferably, the water lotion filter regeneration that also comprises hole sealing agent filter regeneration, 2# washing bath and 3# washing bath in 1# sealing of hole groove;
Hole sealing agent filter regeneration in described 1# sealing of hole groove, closes 3# valve and 4# valve, cleans acid proof pump, strainer and pipeline; Open 1# valve, 2# valve; Start acid proof pump, circulating filtration hole sealing agent groove, till so clear that you can see the bottom, completes hole sealing agent regeneration;
The water lotion filter regeneration of described 2# washing bath and 3# washing bath, closes 1# valve and 2# valve, opens 3# valve, 4# valve and 5# valve; Start acid proof pump, after the water lotion of 4# settling bath is filtered, be evacuated to 3# washing bath, then through 2# washing bath, certainly flow back into 4# settling bath, complete the circulating filtration of washing bath; When the pH value of water lotion is lower than 5.0 time, stop acid proof pump, close 3# valve, 4# valve and 5# valve, open gas agitating 6# valve, unslaked lime is added to 4# settling bath, limit edged stirs, and pH value is surveyed on limit, approaches at 8.0 o'clock to pH value, stop adding unslaked lime and stirring, standing 1 hour, restart Waste Water Treatment, complete the recycling of Cleaning Wastewater.
Than prior art, beneficial effect of the present invention is:
1, the present invention has thoroughly eliminated the pollution of nickel salt to aluminium alloy and water quality from source, has solved pore-sealing liquid and has decomposed sedimentation problem, reduces molten aluminium amount, reduce powder on substrate surface, the sealing of hole film water white transparency forming at substrate surface, has reduced aluminium true qualities and the life-span of prolongation tank liquor; Adopt hydrofluotitanic acid as the main component of hole sealing agent, sealing of hole speed is more than the twice of nickel salt, has improved production efficiency; Adopt hydrofluotitanic acid as the main component of hole sealing agent, sealing of hole temperature can be low to moderate 15 ℃, save energy.
2, aluminium alloy of the present invention is simple to operate without nickel hole-sealing treatment process, energy-conserving and environment-protective, wastewater treatment is easy, be easy to scale operation, by thoroughly finishing to build the nickel contamination of aluminium alloy finished surface treating processes, aluminium alloy use and waste treatment process, solved the bottleneck problem that restricts for many years industry development.
Accompanying drawing explanation
In order to be illustrated more clearly in the embodiment of the present invention or technical scheme of the prior art, to the accompanying drawing of required use in embodiment or description of the Prior Art be briefly described below, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skills, do not paying under the prerequisite of creative work, can also obtain according to these accompanying drawings other accompanying drawing.
Fig. 1 is the aluminium alloy sealing processing technological flow figure of prior art;
Fig. 2 is that aluminium alloy of the present invention is without the system architecture schematic diagram of the hole-sealing treatment process of nickel hole sealing agent.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described, obviously, described embodiment is only the present invention's part embodiment, rather than whole embodiment.Embodiment based in the present invention, those of ordinary skills, not making the every other embodiment obtaining under creative work prerequisite, belong to the scope of protection of the invention.
Aluminium alloy provided by the invention, without nickel hole sealing agent, comprises hydrofluotitanic acid, the aqueous solution of inhibiter and sequestrant, the volume of hole sealing agent of take is benchmark, the concentration of hydrofluotitanic acid is 6.0-9.0g/L, and the concentration of inhibiter is 1.0-3.0g/L, and the concentration of sequestrant is 1.0-3.0g/L.Inhibiter be ethylene glycol, glycerol and sorbyl alcohol one or more; Sequestrant is one or more in trolamine, ethylenediamine tetraacetic acid (EDTA), tripoly phosphate sodium STPP, trisodium phosphate, sodium-metaphosphate, Amino Trimethylene Phosphonic Acid and phosphinylidyne butane tricarboxylic acid; Hole sealing agent working temperature is 20-30 ℃, and hole sealing agent pH value is 3.0-4.0.
The present invention selects hydrofluotitanic acid as main sealing of hole composition, and its ionization, hydrolysis are reacted with sealing of hole and be:
H
2tiF
6=2H
++ TiF
6 2-(hydrofluotitanic acid ionization) (1)
3TiF
6 2-+6H
2O=Ti(OH)
3F
3 2-+Ti(OH)
2F
4 2-+Ti(OH)F
5 2-+6H
++6F
- (2)
(hydrofluotitanic acid hydrolysis)
By (2) formula, the aqueous solution of hydrofluotitanic acid is unstable, and facile hydrolysis becomes monohydroxy, dihydroxyl and trihydroxy-hydrofluotitanic acid root, discharges H simultaneously
+and F
-, tank liquor pH value is declined, F
-concentration increases; If improve pH value, by (2) formula, reaction is moved to the right, and when pH value is greater than 4.5, trihydroxy-hydrofluotitanic acid is further hydrolyzed, and occurs turbidity and precipitation:
Ti (OH)
3f
3 2-+ H
2o=Ti (OH)
4↓+H
++ 3F
-(hydrofluotitanic acid decomposes, separates out titanium hydroxide) (3)
While putting into the aluminium alloy containing oxide film in tank liquor, F
-react with oxide film:
Al
2o
3+ 12F
-+ 3H
2o=2AlF
6 3-+ 6OH
-(oxide film is dissolved, and pH value raises) (4)
2AlF
6 3-+ Al
2o
3+ 3H
2o=2Al
2(OH)
3f
3↓+6F
-(powder on aluminium) (5)
Formula (1)-(5) show the dynamic (dynamical) whole process of sealing of hole.Formula (1) shows that hydrofluotitanic acid is ionized into 2H in tank liquor
++ TiF
6 2-; Formula (2) shows that hydrofluotitanic acid root is hydrolyzed into Ti (OH) in tank liquor
3f
3 2-+ Ti (OH)
2f
4 2-+ Ti (OH) F
5 2-, and discharge 6H
++ 6F
-; Formula (4) shows F
-in the reaction of oxide film micropore, discharge OH
-, improve the pH value in micropore; Formula (3) is surperficial in oxide film micropore, the rising of pH value, Ti (OH)
3f
3 2-further hydrolysis, generates sealing of hole goods and materials Ti (OH)
4, complete sealing of hole.
(1), the impact of sealing of hole time on sealing quality
The sealing of hole time directly determines sealing quality.Time is too short, and sealing of hole is incomplete, and the time is oversize, easily causes that sealing of hole, aluminum alloy surface played ash serious, affects the visual appearance of aluminium; Anodic oxidation film thickness is larger, and sealing of hole is more difficult, and oxide film weightlessness is larger, and sealing quality is poorer, will note rationally controlling the thickness of oxide film during production.The sealing of hole time is the embodiment of hole sealing agent sealing of hole ability, is subject to the impact of temperature, pH value, hole sealing agent composition and concentration, additive component and concentration larger.Under equal conditions, compare with nickelous fluoride, the sealing of hole ability of hydrofluotitanic acid is three times of left and right.The sealing of hole time that is hydrofluotitanic acid is 1/3 of nickelous fluoride.If the thickness of oxide film is 15 μ m, nickelous fluoride needs sealing of hole 15 minutes, and hydrofluotitanic acid needs about 5 minutes.
(2), the impact of sealing of hole temperature on sealing quality
Temperature affects chemical reaction velocity, is generally that 10 ℃ of chemical reaction velocities of every rising improve l doubly, and the sealing of hole time can shorten 1 half.According to the sealing of hole test under differing temps, can obtain the Changing Pattern of hydrofluotitanic acid sealing quality and temperature.When temperature is during in 15-20 ℃, sealing quality is better; When temperature raises, ion velocity of diffusion is accelerated, and hydrolysis rate is accelerated, Ti in oxide film micropore (OH)
3f
3 2-+ Ti (OH)
2f
4 2-+ Ti (OH) F
5 2-concentration increase, F
-concentration improves, and reacts quickening, the Ti of generation (OH) with oxide film
4many, sealing of hole speed improves; When temperature is too low, F
-concentration is low, a little less than reacting with oxide film, and the Ti of generation (OH)
4few, sealing of hole effect is poor.Experiment shows, when other control indexs in working range, the sealing of hole temperature of hydrofluotitanic acid and the pass of sealing of hole speed are: temperature in the time of 15-20 ℃, sealing of hole speed approximately 1 μ m/min; Temperature in the time of 20-25 ℃, sealing of hole speed approximately 2 μ m/min; Temperature in the time of 25-30 ℃, sealing of hole speed approximately 3 μ m/min.Now, can be according to definite sealing of hole times such as oxide film character, thickness, sealing of hole temperature.
(3), the impact of pH value on sealing quality
Impact test according to pH value on sealing quality, can obtain the affect rule of pH value on sealing quality.With the rising of tank liquor pH value, by (2) formula, hydrofluotitanic acid hydrolysis increases, and sealing quality improves; But pH value is too high, Surface of profile easily produces lime, and this is mainly because hydrofluotitanic acid loss of stability, in a large number hydrolysis; PH value is too low, is not enough to cause hydrofluotitanic acid hydrolysis, does not reach sealing of hole effect.PH value is by the chemical reaction of (2) (3) (4) formula to the action principle of sealing of hole, the hydrolysis of hydrofluotitanic acid, and fluorine reacts with oxide film, the rising of pH value in micropore, the Ti generating in fenestra (OH)
4deposition reaches the object of sealing of hole, and how many direct effects that affect sealing of hole of hydrolyzate deposition.PH value deposition of hydrofluotitanic acid hydrolysis between 2.5-4.5 is more, can reach the object of sealing of hole, and pH value sealing of hole effect when 3.0-4.0 left and right is best, and the very good control of acidity is at this moment controlled, and just in time in the hydrolysising balance interval of hydrofluotitanic acid, pH value is very stable.
(4) impact of hydrofluotitanic acid concentration on sealing quality
The present invention selects hydrofluotitanic acid as primary seal hole material, and hydrofluotitanic acid root is one of topmost ion in liquor of hole-sealing tank.Sealing of hole enters oxidation fenestra carrying out hydrolyzing and precipitating by hydrofluotitanic acid root and is achieved, and hydrofluotitanic acid system is the reaction of hydrolysis-dissolution-deposition without the mechanism of nickel rapid hole sealing, and its sealing of hole material is mainly by Ti (OH)
4and Al
2(OH)
3f
3forming, is by the synthesis result of (1)-(5) formula reaction.Ti (OH)
4filling speed directly affects sealing of hole speed, and hydrofluotitanic acid content is very large on sealing quality impact.Experimental result shows that hydrofluotitanic acid (50wt.%) concentration is controlled between 6.0-9.0g/L.
(5), the impact of density of corrosion inhibitor on sealing quality
Inhibiter of the present invention is selected low molecular polylol class, and as ethylene glycol, glycerol and sorbyl alcohol etc., be adsorbed on positively charged aluminum alloy surface by electronegative hydroxyl, isolation tank liquor, slowing down corrosion.Under hydrofluotitanic acid sealing of hole system, pH value operation interval 2.5-4.5, slant acidity, by (4) (5) formula, low pH value is conducive to Al
2o
3with F
-reaction, generates AlF
6 3-, Al (OH) F
5 3-, Al (OH)
2f
4 3-, when its content reaches certain value, interionic associates, is hydrolyzed and be concentrated, is finally converted into stable phase complexing aluminum fluoride Al
2(OH)
3f
3,, in oxide film micropore, Al
2(OH)
3f
3sealing of hole goods and materials, in aluminum alloy surface, Al
2(OH)
3f
3pollen, in tank liquor, Al
2(OH)
3f
3it is muddy thing.So the molten aluminium amount of tank liquor is too large, aluminium alloy is easily gone up powder, and tank liquor is muddy dead groove easily.The interpolation of inhibiter, just in order to protect oxide film not go up powder, reduces molten aluminium amount, extends tank liquor work-ing life.By experimental result, the concentration interval of Organic Alcohol inhibiter is 1-3g/L.
(6), the impact of sequestrant concentration on sealing quality
Sequestrant of the present invention selects acetic acid system (as trolamine; ethylenediamine tetraacetic acid (EDTA) etc.); phosphoric acid system (as tripoly phosphate sodium STPP, trisodium phosphate, sodium-metaphosphate, Amino Trimethylene Phosphonic Acid (ATMP) etc.); with phosphate carboxylic acid system (as phosphinylidyne butane tricarboxylic acid (PBTCA) etc.); with its powerful chelating bond energy, stablize Ti
4+and Al
3+, guarantee that tank liquor is not muddy, aluminium alloy is not gone up powder.By (2) (5) formula, when pH raises, easily generate Ti (OH)
4and Al
2(OH)
3f
3.These goods and materials, if be created on oxide film micropore, are sealing of hole goods and materials; If be created on aluminum alloy surface, be powder; If be created in tank liquor, be muddy thing.Adding of sequestrant, improved Ti (OH)
4and Al
2(OH)
3f
3generation threshold.By (4) formula, in micropore, F
-with Al
2o
3the OH that reaction produces
-be difficult for being diffused into the tank liquor outside aluminum alloy surface, in hole, pH rises highlyer, and chelate bond is opened, Ti
4+and Al
3+be released, generate Ti (OH)
4and Al
2(OH)
3f
3, realize sealing of hole; And in aluminum alloy surface, OH
-be diffused into rapidly in tank liquor, surface p H rises limited, can not open chelate bond, can not generate Ti (OH)
4and Al
2(OH)
3f
3, aluminium alloy is difficult for upper powder, and tank liquor is difficult for muddy.In addition, the acidic group in sequestrant is electronegative, can be adsorbed on positively charged oxide film, plays inhibiter effect, reduces the meltage of aluminium alloy.The consumption of sequestrant will be paid special attention to, and concentration is too high, and chelate bond is bad to be opened, and sealing of hole ability sharply declines; Sequestrant concentration is too low, though sealing of hole is good, and powder on aluminium alloy, tank liquor is muddy.Experiment shows, appropriate sequestrant concentration is 1-3g/L.
(7), the impact of foreign ion on sealing quality
Constantly bring in process of production foreign ion into, cause the accumulation of impurity, as NH
4 +, Na
+, K
+, Ca
2+, Mg
2+deng positively charged ion, increase, sequestrant consumption is accelerated.Therefore, holding cleaning closes most important.In addition, when tank liquor pH is too low, available ammoniacal liquor regulates pH value to 3.5 left and right, with sodium hydroxide, does not regulate, and can effectively stop Na like this
+add, consume sequestrant.Select hydrofluotitanic acid rather than potassium fluotitanate as main sealing of hole composition, key reason is K
+consumption to sequestrant.
Affect aluminium alloy a lot of without the factor of nickel sealing quality, mainly contain hydrofluotitanic acid concentration, density of corrosion inhibitor and sequestrant concentration, these 3 factors are the keys that determine aluminium alloy sealing quality; The pH value of tank liquor, temperature and sealing of hole time are the important factors that affects aluminium alloy sealing quality; And improve the cleanliness factor of tank liquor, the content that reduces impurity is the important guarantee of aluminium alloy sealing quality.Test shows, aluminium alloy should be without the manufacturing condition of nickel hole sealing agent:
Hydrofluotitanic acid (50wt.%) concentration interval is 6.0-9.0g/L
The concentration interval of inhibiter is 1-3g/L
Sequestrant concentration interval is 1-3g/L
Sealing of hole speed 1-3um/min
Temperature 15-35 ℃
Time 5-15min
PH value 2.5-4.5
Fluting: adopt tap water preparation tank liquor, bring other tank liquor into but should note in the course of processing reducing, reduce the extra consumption to sequestrant.
Embodiment 1
Select hydrofluotitanic acid (50wt.%) 7.5g/L as sealing of hole composition; Ethylene glycol 2.0g/L is as inhibiter, and tripoly phosphate sodium STPP 2.0g/L is as chelating composition, and adopting working temperature is 25 ℃, and pH value is 3.5, sealing of hole speed 1 μ m/ minute.
Embodiment 2
Select hydrofluotitanic acid (50wt.%) 7.5g/L as sealing of hole composition; Glycerol 2.0g/L is as inhibiter, and tripoly phosphate sodium STPP 2.0g/L is as chelating composition, and working temperature is 25 ℃, and pH value is 3.5, sealing of hole speed 1 μ m/ minute.
Embodiment 3
Select hydrofluotitanic acid (50wt.%) 7.5g/L as sealing of hole composition; Sorbyl alcohol 2.0g/L is as inhibiter, and tripoly phosphate sodium STPP 2.0g/L is as chelating composition, and working temperature is 25 ℃, and pH value is 3.5, sealing of hole speed 1 μ m/ minute;
Embodiment 4
Select hydrofluotitanic acid (50wt.%) 7.5g/L as sealing of hole composition; Glycerol 2.0g/L is as inhibiter, and trolamine 2.0g/L is as chelating composition, and working temperature is 25 ℃, and pH value is 3.5, sealing of hole speed 1 μ m/ minute.
Embodiment 5
Select hydrofluotitanic acid (50wt.%) 7.5g/L as sealing of hole composition; Glycerol 2.0g/L is as inhibiter, and ethylenediamine tetraacetic acid (EDTA) 2.0g/L is as chelating composition, and working temperature is 25 ℃, and pH value is 3.5, sealing of hole speed 1 μ m/ minute.
Embodiment 6
Select hydrofluotitanic acid (50wt.%) 7.5g/L as sealing of hole composition; Glycerol 2.0g/L is as inhibiter, and trisodium phosphate 2.0g/L is as chelating composition, and working temperature is 25 ℃, and pH value is 3.5, sealing of hole speed 1 μ m/ minute.
Embodiment 7
Select hydrofluotitanic acid (50wt.%) 7.5g/L as sealing of hole composition; Glycerol 2.0g/L is as inhibiter, and sodium-metaphosphate 2.0g/L is as chelating composition, and working temperature is 25 ℃, and pH value is 3.5, sealing of hole speed 1 μ m/ minute.
Embodiment 8
Select hydrofluotitanic acid (50wt.%) 7.5g/L as sealing of hole composition; Glycerol 2.0g/L is as inhibiter, and Amino Trimethylene Phosphonic Acid 2.0g/L is as chelating composition, and working temperature is 25 ℃, and pH value is 3.5, sealing of hole speed 1 μ m/ minute.
Embodiment 9
Select hydrofluotitanic acid (50wt.%) 7.5g/L as sealing of hole composition; Glycerol 2.0g/L is as inhibiter, and phosphinylidyne butane tricarboxylic acid 2.0g/L is as chelating composition, and working temperature is 25 ℃, and pH value is 3.5, sealing of hole speed 1 μ m/ minute.
Embodiment 10
Select hydrofluotitanic acid (50wt.%) 6.0g/L as sealing of hole composition; Glycerol 2.0g/L is as inhibiter, and phosphinylidyne butane tricarboxylic acid 2.0g/L is as chelating composition, and working temperature is 25 ℃, and pH value is 3.5, sealing of hole speed 1 μ m/ minute.
Embodiment 11
Select hydrofluotitanic acid (50wt.%) 9.0g/L as sealing of hole composition; Glycerol 2.0g/L is as inhibiter, and phosphinylidyne butane tricarboxylic acid 2.0g/L is as chelating composition, and working temperature is 25 ℃, and pH value is 3.5, sealing of hole speed 1 μ m/ minute.
Embodiment 12
Select hydrofluotitanic acid (50wt.%) 7.5g/L as sealing of hole composition; Glycerol 1.0g/L is as inhibiter, and phosphinylidyne butane tricarboxylic acid 2.0g/L is as chelating composition, and working temperature is 25 ℃, and pH value is 3.5, sealing of hole speed 1 μ m/ minute.
Embodiment 13
Select hydrofluotitanic acid (50wt.%) 7.5g/L as sealing of hole composition; Glycerol 3.0g/L is as inhibiter, and phosphinylidyne butane tricarboxylic acid 2.0g/L is as chelating composition, and working temperature is 25 ℃, and pH value is 3.5, sealing of hole speed 1 μ m/ minute.
Embodiment 14
Select hydrofluotitanic acid (50wt.%) 7.5g/L as sealing of hole composition; Glycerol 2.0g/L is as inhibiter, and phosphinylidyne butane tricarboxylic acid 1.0g/L is as chelating composition, and working temperature is 25 ℃, and pH value is 3.5, sealing of hole speed 1 μ m/ minute.
Embodiment 15
Select hydrofluotitanic acid (50wt.%) 7.5g/L as sealing of hole composition; Glycerol 2.0g/L is as inhibiter, and phosphinylidyne butane tricarboxylic acid 3.0g/L is as chelating composition, and working temperature is 25 ℃, and pH value is 3.5, sealing of hole speed 1 μ m/ minute.
Embodiment 16
Select hydrofluotitanic acid (50wt.%) 7.5g/L as sealing of hole composition; Glycerol 2.0g/L is as inhibiter, and phosphinylidyne butane tricarboxylic acid 2.0g/L is as chelating composition, and working temperature is 15 ℃, and pH value is 3.5, sealing of hole speed 1 μ m/ minute.
Embodiment 17
Select hydrofluotitanic acid (50wt.%) 7.5g/L as sealing of hole composition; Glycerol 2.0g/L is as inhibiter, and phosphinylidyne butane tricarboxylic acid 2.0g/L is as chelating composition, and working temperature is 25 ℃, and pH value is 3.5, sealing of hole speed 2 μ m/ minute.
Embodiment 18
Select hydrofluotitanic acid (50wt.%) 7.5g/L as sealing of hole composition; Glycerol 2.0g/L is as inhibiter, and phosphinylidyne butane tricarboxylic acid 2.0g/L is as chelating composition, and working temperature is 35 ℃, and pH value is 3.5, sealing of hole speed 3 μ m/ minute.
Embodiment 19
Select hydrofluotitanic acid (50wt.%) 7.5g/L as sealing of hole composition; Glycerol 2.0g/L is as inhibiter, and phosphinylidyne butane tricarboxylic acid 2.0g/L is as chelating composition, and working temperature is 25 ℃, and pH value is 2.5, sealing of hole speed 1 μ m/ minute.
Embodiment 20
Select hydrofluotitanic acid (50wt.%) 7.5g/L as sealing of hole composition; Glycerol 2.0g/L is as inhibiter, and phosphinylidyne butane tricarboxylic acid 2.0g/L is as chelating composition, and working temperature is 25 ℃, and pH value is 3.5, sealing of hole speed 1 μ m/ minute.
Embodiment 21
Select hydrofluotitanic acid (50wt.%) 7.5g/L as sealing of hole composition; Glycerol 2.0g/L is as inhibiter, and phosphinylidyne butane tricarboxylic acid 2.0g/L is as chelating composition, and working temperature is 25 ℃, and pH value is 4.5, sealing of hole speed 1 μ m/ minute.
As seen from the above embodiment, along with the increase of hydrofluotitanic acid concentration, aluminium alloy strengthens without the sealing of hole ability of nickel hole sealing agent in the present invention; The concentration interval of hydrofluotitanic acid is 6-9g/L; Along with the increase of glycerol concentration, aluminium alloy slightly reduces without the sealing of hole ability of nickel hole sealing agent; But aluminum alloy surface pollen reduces; Its concentration interval is 1.0-3.0g/L; Along with the increase of phosphinylidyne butane tricarboxylic acid concentration, aluminium alloy reduces without the sealing of hole ability of nickel hole sealing agent; Liquor of hole-sealing tank contamination resistance strengthens, and aluminum alloy surface pollen reduces; Its concentration interval is 1.0-3.0g/L; Along with working temperature raises, aluminium alloy rises without the sealing of hole ability of nickel hole sealing agent, and sealing of hole temperature range is 15-35 ℃; Temperature is too low, and sealing of hole ability is inadequate, and temperature is too high, and oxide film corrosion is too fast, powder on surface; Between optimal zone, be 20-30 ℃; Along with work pH value raises, aluminium alloy first rises without the sealing of hole ability of nickel hole sealing agent, rear decline, and sealing of hole pH value interval is 2.5-4.5; PH value is too low, and sealing of hole ability is inadequate, powder on surface; PH value is too high, and sealing of hole ability declines; Between optimal zone, be 3.0-4.0.
In order to guarantee life-time service after alumilite process, must carry out sealing of hole processing, the object of sealing of hole is color and fast light, the weathering resistance of solidity to corrosion, its surface anti-pollution ability and coloring film thereof in order to improve aluminium, so sealing of hole is very important sport technique segment.The present invention also provides a kind of aluminium alloy without nickel hole-sealing treatment process, and aluminum alloy base material, by processing without nickel process unit, is comprised the steps:
(1) will be heated to 15-35 ℃ without nickel hole sealing agent, the aluminum alloy base material after anodic oxidation is immersed in hole sealing agent without nickel, sealing of hole speed is 1-3 μ m/min;
(2) hole sealing agent of the aluminum alloy base material remained on surface through soaking without nickel hole sealing agent of step (1) gained is washed, after flushing, dried up, pack.
Without nickel process unit, comprise production system, heating system, gas agitating system, filtering system and Waste Water Treatment in the present invention.This production system comprises 1# sealing of hole groove, 2# washing bath and 3# washing bath, and 1# sealing of hole groove is main work nest, and for completing the sealing of hole of Process on Aluminum Alloy Oxidation Film, 2# washing bath and 3# washing bath are for cleaning the residual hole sealing agent of aluminum alloy surface after sealing of hole; Heating system comprises steam heating tube and be arranged at the 8# valve on described steam heating tube, and described steam heating tube is arranged at respectively the both sides of described 1# sealing of hole groove, for the heating of described 1# sealing of hole groove; Waste Water Treatment is comprised of 2# washing bath, 3# washing bath, 4# settling bath, acid proof pump, strainer, 3# valve, 4# valve, 5# valve and pipeline, described Waste Water Treatment, for purifying the scavenging solution of described 2# washing bath and 3# washing bath, is realized cycling utilization of wastewater; Gas agitating system comprises air compressor machine, feed channel and is arranged at 6# valve and the 7# valve in described feed channel, and described gas agitating system is for the uniform stirring of described 1# sealing of hole groove and 4# settling bath solution; Filtering system is connected to form by 1# sealing of hole groove, 2# washing bath, 3# washing bath, 4# settling bath, acid proof pump, strainer, 1# valve, 2# valve, 3# valve, 4# valve, 5# valve and pipeline, and described filtering system is for the filtration of described 1# sealing of hole groove, described 2# washing bath and 3# washing bath water lotion.
Aluminium alloy sealing operation, open 8# valve, heating 1# sealing of hole groove, checks and confirms that indices is within following scope: between the concentration 1-3g/L of hydrofluotitanic acid (50wt.%) concentration 6.0-9.0g/L, inhibiter, sequestrant concentration 1-3g/L, temperature 15-35 ℃, pH value 2.5-4.5; Along with the increase of hydrofluotitanic acid concentration, aluminium alloy strengthens without the sealing of hole ability of nickel hole sealing agent.
Open 3# valve, 4# valve, 5# valve, start acid proof pump, confirm that the pH value of 4# settling bath is between 5-8, the water lotion in circulation 4# settling bath, to 2# washing bath and 3# washing bath, then returns to 4# settling bath.After sealing of hole completes, through 2# washing bath and 3# washing bath, cleaning aluminum alloy remained on surface hole sealing agent, then air-dry, packing, completes production whole process.
In the present invention, during the heating of 1# sealing of hole groove, 8# valve is opened, and 8# valve is controlled sealing of hole temperature automatically between 20-30 ℃.In 1# sealing of hole groove, add after hole sealing agent, open 7# valve, by gas agitating system, stirred, continue to produce; Close 3# valve, 4# valve, 5# valve, open gas agitating 6# valve, unslaked lime is added to 4# settling bath, limit edged stirs, to pH value be 8.0 o'clock, stop adding unslaked lime and stirring.
Aluminium alloy of the present invention, without nickel hole-sealing technology, also comprises: the hole sealing agent filter regeneration in 1# sealing of hole groove: close 3# valve and 4# valve, clean acid proof pump, strainer and pipeline; Open 1# valve, 2# valve; Start acid proof pump, circulating filtration 1# sealing of hole groove, till so clear that you can see the bottom, completes hole sealing agent regeneration; Water lotion filter regeneration in 2# washing bath and 3# washing bath: in water washing process, hole sealing agent is constantly brought into washing bath, has reduced the pH value of washing bath, starts Waste Water Treatment, to water lotion filter regeneration, recycle; Close 1# valve and 2# valve, open 3# valve, 4# valve and 5# valve; Start acid proof pump, after the water lotion of 4# settling bath is filtered, be evacuated to 3# washing bath, then through 2# washing bath, certainly flow back to 4# settling bath, complete the circulating filtration of washing bath.When the pH value of water lotion is lower than 5.0 time, stop acid proof pump, close 3#, 4#, 5# valve, open gas agitating 6# valve, unslaked lime is added to 4# settling bath, limit edged stirs, and pH value is surveyed on limit, approaches at 8.0 o'clock to pH value, stop adding unslaked lime and stirring, standing 1 hour, restart Waste Water Treatment, complete the recycling of Cleaning Wastewater.
The foregoing is only preferred embodiment of the present invention, in order to limit the present invention, within the spirit and principles in the present invention not all, any modification of doing, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (10)
1. aluminium alloy, without nickel hole sealing agent, is characterized in that, comprises hydrofluotitanic acid, the aqueous solution of inhibiter and sequestrant, the volume of hole sealing agent of take is benchmark, the concentration of described hydrofluotitanic acid is 6.0-9.0g/L, the concentration of described inhibiter is 1.0-3.0g/L, and the concentration of described sequestrant is 1.0-3.0g/L.
2. aluminium alloy according to claim 1, without nickel hole sealing agent, is characterized in that, described inhibiter be ethylene glycol, glycerol and sorbyl alcohol one or more.
According to aluminium alloy claimed in claim 1 without nickel hole sealing agent; it is characterized in that, described sequestrant is one or more in trolamine, ethylenediamine tetraacetic acid (EDTA), tripoly phosphate sodium STPP, trisodium phosphate, sodium-metaphosphate, Amino Trimethylene Phosphonic Acid and phosphinylidyne butane tricarboxylic acid.
4. aluminium alloy according to claim 1, without nickel hole sealing agent, is characterized in that, described hole sealing agent working temperature is 20-30 ℃, and the pH value of described hole sealing agent is 3.0-4.0.
5. aluminium alloy, without a nickel hole-sealing treatment process, is characterized in that, aluminum alloy base material, by processing without nickel process unit, is comprised the steps:
(1) will be heated to 15-35 ℃ without nickel hole sealing agent, the aluminum alloy base material after anodic oxidation is immersed in hole sealing agent without nickel, sealing of hole speed is 1-3 μ m/min;
(2) hole sealing agent of the aluminum alloy base material remained on surface through soaking without nickel hole sealing agent of step (1) gained is washed, after flushing, dried up, pack.
6. aluminium alloy according to claim 5, without nickel hole-sealing treatment process, is characterized in that, describedly without nickel process unit, comprises production system, heating system, gas agitating system, filtering system and Waste Water Treatment;
Described production system comprises 1# sealing of hole groove, 2# washing bath and 3# washing bath, and described 1# sealing of hole groove is main work nest, and for completing the sealing of hole of Process on Aluminum Alloy Oxidation Film, described 2# washing bath and 3# washing bath are for cleaning the residual hole sealing agent of aluminum alloy surface after sealing of hole;
Described heating system comprises steam heating tube and be arranged at the 8# valve on described steam heating tube, and described steam heating tube is arranged at respectively the both sides of described 1# sealing of hole groove, for the heating of described 1# sealing of hole groove;
Described Waste Water Treatment is comprised of 2# washing bath, 3# washing bath, 4# settling bath, acid proof pump, strainer, 3# valve, 4# valve, 5# valve and pipeline, described Waste Water Treatment, for purifying the scavenging solution of described 2# washing bath and 3# washing bath, is realized cycling utilization of wastewater;
Described gas agitating system comprises air compressor machine, feed channel and is arranged at 6# valve and the 7# valve in described feed channel, and described gas agitating system is for the uniform stirring of described 1# sealing of hole groove and 4# settling bath solution;
Described filtering system is connected to form by 1# sealing of hole groove, 2# washing bath, 3# washing bath, 4# settling bath, acid proof pump, strainer, 1# valve, 2# valve, 3# valve, 4# valve, 5# valve and pipeline, and described filtering system is for the filtration of described 1# sealing of hole groove, described 2# washing bath and 3# washing bath water lotion.
7. aluminium alloy according to claim 6, without nickel hole-sealing treatment process, is characterized in that, opens 8# valve, heat described 1# sealing of hole groove, open 3# valve, 4# valve, 5# valve, start acid proof pump, water lotion in 4# settling bath, to 2# washing bath and 3# washing bath, then returns to 4# settling bath;
After oxidized aluminum alloy, in 1# sealing of hole groove, sealing of hole speed is 1-3 μ m/min, after sealing of hole completes, and through 2# washing bath and 3# washing bath, cleaning aluminum alloy remained on surface hole sealing agent, then air-dry, packing.
8. aluminium alloy according to claim 7, without nickel hole-sealing treatment process, is characterized in that, during described 1# sealing of hole groove heating, described 8# valve is controlled hole sealing agent temperature automatically between 20-30 ℃.
9. aluminium alloy according to claim 6, without nickel hole-sealing treatment process, is characterized in that, after adding without nickel hole sealing agent, opens 7# valve in described 1# sealing of hole groove, and the hole sealing agent in by described gas agitating system, 1# sealing of hole groove being stirred is mixed evenly, continues to produce; Close 3# valve, 4# valve, 5# valve, open gas agitating 6# valve, unslaked lime is added to 4# settling bath, limit edged stirs, to pH value be 8.0 o'clock, stop adding unslaked lime and stirring.
10. aluminium alloy according to claim 6, without nickel hole-sealing treatment process, is characterized in that, also comprises the water lotion filter regeneration of hole sealing agent filter regeneration, 2# washing bath and 3# washing bath in 1# sealing of hole groove;
Hole sealing agent filter regeneration in described 1# sealing of hole groove, closes 3# valve and 4# valve, cleans acid proof pump, strainer and pipeline; Open 1# valve, 2# valve; Start acid proof pump, circulating filtration hole sealing agent groove, till so clear that you can see the bottom, completes hole sealing agent regeneration;
The water lotion filter regeneration of described 2# washing bath and 3# washing bath, closes 1# valve and 2# valve, opens 3# valve, 4# valve and 5# valve; Start acid proof pump, after the water lotion of 4# settling bath is filtered, be evacuated to 3# washing bath, then through 2# washing bath, certainly flow back into 4# settling bath, complete the circulating filtration of washing bath; When the pH value of water lotion is lower than 5.0 time, stop acid proof pump, close 3# valve, 4# valve and 5# valve, open gas agitating 6# valve, unslaked lime is added to 4# settling bath, limit edged stirs, and pH value is surveyed on limit, approaches at 8.0 o'clock to pH value, stop adding unslaked lime and stirring, standing 1 hour, restart Waste Water Treatment, complete the recycling of Cleaning Wastewater.
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