CN104404488B - A kind of aluminium alloy non-chromium passivator and preparation method thereof - Google Patents
A kind of aluminium alloy non-chromium passivator and preparation method thereof Download PDFInfo
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- CN104404488B CN104404488B CN201410648275.6A CN201410648275A CN104404488B CN 104404488 B CN104404488 B CN 104404488B CN 201410648275 A CN201410648275 A CN 201410648275A CN 104404488 B CN104404488 B CN 104404488B
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Abstract
The invention discloses a kind of aluminium alloy non-chromium passivator and preparation method thereof, make by following raw material weight number proportioning: citric acid 12 35 parts, sodium citrate 10 22 parts, sodium peroxydisulfate 6 16 parts, sodium silicate 7 22 parts, phosphoric acid 6 18 parts, cobalt nitrate 2 11 parts, sodium sulfite 6 20 parts, malonic acid 12 32 parts, ammonium fluoride 2 11 parts, dodecylbenzene sodium sulfonate 19 parts, 25 65 parts of water.Passivator of the present invention can be passivated at normal temperatures, and passivation time is short, environment friendly and pollution-free；The passivating film formed enhances the corrosion resistance of aluminium alloy.
Description
Technical field
The present invention relates to a kind of passivator, particularly relate to a kind of aluminium alloy non-chromium passivator and preparation method thereof.
Background technology
In recent decades, China uses hexavalent chromate to be passivated always, and hexavalent chromate Passivation Treatment significantly improves the resistance to of alloy
Corrosivity, the passivating film of generation has self-regeneration effect, and cheap, uses widely, but chromating liquid
In containing Cr VI this severe toxicity carcinogen, have a strong impact on health and pollute environment.At present countries in the world all start to limit or
Prohibit the use of chromating processes.Therefore asepsis environment-protecting, efficient, the non-hexavalent chromium passivating technique of low consumption are developed, it is achieved Gao Pin
Matter, eco-friendly steel surface passivator demand the most urgent.
Additionally, many factories use trivalent chromate to substitute hexavalent chromate prepares steel surface passivator, such as Chinese patent
CN101130865A trivalent chromium black passivator and preparation method thereof, it is provided that a kind of trivalent chromium for Treatment of Metal Surface is blunt
Agent, although the treatment effect of this passivator is preferable, but trivalent chromium still has certain toxicity, and factory is to trivalent chromic ion
Waste water process more difficulty, and relatively costly.Therefore, exploitation chrome-free tanning agent is increasingly subject to people's attention.
For Al alloy parts, form the oxide-film of densification because aluminum is the most oxidized, and aluminium alloy inside is had one
Fixed protective effect, but As time goes on the change of environment, oxide-film is easily destroyed.Thus cause workpiece rotten
Erosion.Therefore develop and a kind of can protect aluminum workpiece, the aluminium alloy non-chromium passivator alleviating its surface corrosion, increasing the service life
The most urgent.
Summary of the invention
Solve the technical problem that:
In order to provide one to be applicable to aluminum alloy surface Passivation Treatment, and the passivator that environment is not polluted, the invention provides
A kind of aluminium alloy non-chromium passivator and preparation method thereof.
Technical scheme:
A kind of aluminium alloy non-chromium passivator, is made by following raw material weight number proportioning: citric acid 12-35 part, sodium citrate 10-22
Part, sodium peroxydisulfate 6-16 part, sodium silicate 7-22 part, phosphoric acid 6-18 part, cobalt nitrate 2-11 part, sodium sulfite 6-20 part, third
Diacid 12-32 part, ammonium fluoride 2-11 part, dodecylbenzene sodium sulfonate 1-9 part, water 25-65 part.
As a preferred embodiment of the present invention, make aluminium alloy non-chromium passivator by following raw material weight number proportioning: citric acid
15-30 part, sodium citrate 12-20 part, sodium peroxydisulfate 7-15 part, sodium silicate 9-20 part, phosphoric acid 8-16 part, cobalt nitrate 3-9
Part, sodium sulfite 8-17 part, malonic acid 14-30 part, ammonium fluoride 4-10 part, dodecylbenzene sodium sulfonate 2-8 part, water 30-60
Part.
As a preferred embodiment of the present invention, make aluminium alloy non-chromium passivator by following raw material weight number proportioning: citric acid
16-28 part, sodium citrate 14-20 part, sodium peroxydisulfate 8-14 part, sodium silicate 10-18 part, phosphatase 79-15 parts, cobalt nitrate 4-8
Part, sodium sulfite 9-16 part, malonic acid 15-28 part, ammonium fluoride 5-9 part, dodecylbenzene sodium sulfonate 3-7 part, water 35-60
Part.
The preparation method of a kind of aluminium alloy non-chromium passivator, comprises the following steps:
(1) citric acid, sodium citrate, sodium peroxydisulfate, sodium silicate, phosphoric acid and water are poured in reactor, be 13-21 in temperature
DEG C, pressure be to stir 25-40 minute under the conditions of 0.05-0.1MPa, agitator speed is 400-550 rev/min, and stirring completes
After pH is adjusted between 4-6；
(2) cobalt nitrate, sodium sulfite, malonic acid are added to the water, temperature be 40-58 DEG C, pressure be 0.12-0.24MPa
Under the conditions of magnetic agitation dissolve, after being completely dissolved when solution temperature is down to 22-26 DEG C, be added thereto to dodecylbenzene sodium sulfonate,
It is sufficiently stirred for mixing；
(3) solution step (2) obtained adds in the solution that step (1) obtains, and flow velocity is 0.07-0.32m/s, reaction
Temperature in the kettle is 14-22 DEG C, and pressure is 0.05-0.1MPa, stirs while adding, and agitator speed is 450-600 rev/min；
After being added completely in the solution that step (1) obtains by the solution that step (2) is obtained, agitator continues stirring 35-48 and divides
Clock；
(4) adding ammonium fluoride in the solution that step (3) obtains, reactor temperature is 35-50 DEG C, and pressure is 0.05-0.1MPa,
Stirring while adding, agitator speed is 450-600 rev/min.
As a preferred technical solution of the present invention, in step (1) by citric acid, sodium citrate, sodium peroxydisulfate, sodium silicate,
Phosphoric acid and water are poured in reactor, temperature be 15-20 DEG C, pressure be 0.06-0.1MPa under the conditions of stir 28-40 minute, stir
Mix device rotating speed and be 450-550 rev/min, after having stirred, pH is adjusted between 4-6.
As a preferred technical solution of the present invention, cobalt nitrate, sodium sulfite, malonic acid are added to the water in (2) by step,
Temperature be 45-55 DEG C, magnetic agitation is dissolved under the conditions of pressure is 0.14-0.24MPa, treats that solution temperature is down to after being completely dissolved
When 22-26 DEG C, it is added thereto to dodecylbenzene sodium sulfonate, is sufficiently stirred for mixing.
As a preferred technical solution of the present invention, in step (3), solution step (2) obtained adds step (1)
In the solution obtained, flow velocity is 0.08-0.28m/s, and reactor temperature is 14-20 DEG C, and pressure is 0.07-0.1MPa, and limit adds
Limit is stirred, and agitator speed is 500-600 rev/min；Treat that the solution that step (2) is obtained is added completely into step (1) obtains
After in the solution obtained, agitator continues stirring 37-45 minute.
As a preferred technical solution of the present invention, in step (4), in the solution that step (3) obtains, add fluorination
Ammonium, reactor temperature is 38-50 DEG C, and pressure is 0.07-0.1MPa, stirs while adding, and agitator speed is 500-600
Rev/min.
Beneficial effect
A kind of aluminium alloy non-chromium passivator of the present invention and preparation method thereof uses above technical scheme to have following technical effect that
The first, the aluminium alloy non-chromium passivator decay resistance that prepared by the present invention is close with Cr VI passivator performance；The second, the present invention
Environment is not polluted by the passivator obtained；3rd, the preparation method of aluminium alloy non-chromium passivator of the present invention avoids volatilization
Property acid staff is damaged.
Detailed description of the invention
Embodiment 1:
A kind of aluminium alloy non-chromium passivator, is made by following raw material weight number proportioning: citric acid 12 parts, sodium citrate 10 parts,
Sodium peroxydisulfate 6 parts, sodium silicate 7 parts, phosphoric acid 6 parts, cobalt nitrate 2 parts, sodium sulfite 6 parts, malonic acid 12 parts, ammonium fluoride
2 parts, dodecylbenzene sodium sulfonate 1 part, 25 parts of water.
The preparation method of a kind of aluminium alloy non-chromium passivator, comprises the following steps:
(1) citric acid, sodium citrate, sodium peroxydisulfate, sodium silicate, phosphoric acid and water are poured in reactor, be 13 in temperature
DEG C, pressure be to stir 25 minutes under the conditions of 0.05MPa, agitator speed is 400 revs/min, is adjusted to by pH after having stirred
4；
(2) cobalt nitrate, sodium sulfite, malonic acid are added to the water, temperature be 40 DEG C, under the conditions of pressure is 0.12MPa
Magnetic agitation is dissolved, and after being completely dissolved when solution temperature is down to 22 DEG C, is added thereto to dodecylbenzene sodium sulfonate, fully stirs
Mix mixing；
(3) solution step (2) obtained adds in the solution that step (1) obtains, and flow velocity is 0.07m/s, in reactor
Temperature is 14 DEG C, and pressure is 0.05MPa, stirs while adding, and agitator speed is 450 revs/min；Treat step (2)
After the solution obtained is added completely in the solution that step (1) obtains, agitator continues stirring 35 minutes；
(4) adding ammonium fluoride in the solution that step (3) obtains, reactor temperature is 35 DEG C, and pressure is 0.05MPa,
Stirring while adding, agitator speed is 450 revs/min.
Embodiment 2:
A kind of aluminium alloy non-chromium passivator, is made by following raw material weight number proportioning: citric acid 15 parts, sodium citrate 12 parts,
Sodium peroxydisulfate 8 parts, sodium silicate 9 parts, phosphoric acid 8 parts, cobalt nitrate 4 parts, sodium sulfite 8 parts, malonic acid 14 parts, ammonium fluoride
4 parts, dodecylbenzene sodium sulfonate 2 parts, 35 parts of water.
The preparation method of a kind of aluminium alloy non-chromium passivator, comprises the following steps:
(1) citric acid, sodium citrate, sodium peroxydisulfate, sodium silicate, phosphoric acid and water are poured in reactor, be 15 in temperature
DEG C, pressure be to stir 30 minutes under the conditions of 0.06MPa, agitator speed is 450 revs/min, is adjusted to by pH after having stirred
4；
(2) cobalt nitrate, sodium sulfite, malonic acid are added to the water, temperature be 45 DEG C, under the conditions of pressure is 0.14MPa
Magnetic agitation is dissolved, and after being completely dissolved when solution temperature is down to 23 DEG C, is added thereto to dodecylbenzene sodium sulfonate, fully stirs
Mix mixing；
(3) solution step (2) obtained adds in the solution that step (1) obtains, and flow velocity is 0.12m/s, in reactor
Temperature is 16 DEG C, and pressure is 0.06MPa, stirs while adding, and agitator speed is 500 revs/min；Treat step (2)
After the solution obtained is added completely in the solution that step (1) obtains, agitator continues stirring 38 minutes；
(4) adding ammonium fluoride in the solution that step (3) obtains, reactor temperature is 40 DEG C, and pressure is 0.06MPa,
Stirring while adding, agitator speed is 500 revs/min.
Embodiment 3:
A kind of aluminium alloy non-chromium passivator, is made by following raw material weight number proportioning: citric acid 20 parts, sodium citrate 15 parts,
Sodium peroxydisulfate 10 parts, sodium silicate 12 parts, phosphatase 11 2 parts, cobalt nitrate 6 parts, sodium sulfite 10 parts, malonic acid 16 parts, fluorine
Change ammonium 6 parts, dodecylbenzene sodium sulfonate 4 parts, 45 parts of water.
The preparation method of a kind of aluminium alloy non-chromium passivator, comprises the following steps:
(1) citric acid, sodium citrate, sodium peroxydisulfate, sodium silicate, phosphoric acid and water are poured in reactor, be 17 in temperature
DEG C, pressure be to stir 33 minutes under the conditions of 0.06MPa, agitator speed is 500 revs/min, is adjusted to by pH after having stirred
4；
(2) cobalt nitrate, sodium sulfite, malonic acid are added to the water, temperature be 48 DEG C, under the conditions of pressure is 0.16MPa
Magnetic agitation is dissolved, and after being completely dissolved when solution temperature is down to 24 DEG C, is added thereto to dodecylbenzene sodium sulfonate, fully stirs
Mix mixing；
(3) solution step (2) obtained adds in the solution that step (1) obtains, and flow velocity is 0.15m/s, in reactor
Temperature is 18 DEG C, and pressure is 0.07MPa, stirs while adding, and agitator speed is 550 revs/min；Treat step (2)
After the solution obtained is added completely in the solution that step (1) obtains, agitator continues stirring 42 minutes；
(4) adding ammonium fluoride in the solution that step (3) obtains, reactor temperature is 42 DEG C, and pressure is 0.07MPa,
Stirring while adding, agitator speed is 550 revs/min.
Embodiment 4:
A kind of aluminium alloy non-chromium passivator, is made by following raw material weight number proportioning: citric acid 25 parts, sodium citrate 18 parts,
Sodium peroxydisulfate 13 parts, sodium silicate 16 parts, phosphatase 11 5 parts, cobalt nitrate 8 parts, sodium sulfite 15 parts, malonic acid 23 parts, fluorine
Change ammonium 8 parts, dodecylbenzene sodium sulfonate 6 parts, 50 parts of water.
The preparation method of a kind of aluminium alloy non-chromium passivator, comprises the following steps:
(1) citric acid, sodium citrate, sodium peroxydisulfate, sodium silicate, phosphoric acid and water are poured in reactor, be 19 in temperature
DEG C, pressure be to stir 36 minutes under the conditions of 0.07MPa, agitator speed is 500 revs/min, is adjusted to by pH after having stirred
5；
(2) cobalt nitrate, sodium sulfite, malonic acid are added to the water, temperature be 52 DEG C, under the conditions of pressure is 0.22MPa
Magnetic agitation is dissolved, and after being completely dissolved when solution temperature is down to 24 DEG C, is added thereto to dodecylbenzene sodium sulfonate, fully stirs
Mix mixing；
(3) solution step (2) obtained adds in the solution that step (1) obtains, and flow velocity is 0.22m/s, in reactor
Temperature is 20 DEG C, and pressure is 0.08MPa, stirs while adding, and agitator speed is 550 revs/min；Treat step (2)
After the solution obtained is added completely in the solution that step (1) obtains, agitator continues stirring 45 minutes；
(4) adding ammonium fluoride in the solution that step (3) obtains, reactor temperature is 46 DEG C, and pressure is 0.08MPa,
Stirring while adding, agitator speed is 550 revs/min.
Embodiment 5:
A kind of aluminium alloy non-chromium passivator, is made by following raw material weight number proportioning: citric acid 35 parts, sodium citrate 22 parts,
Sodium peroxydisulfate 16 parts, sodium silicate 22 parts, phosphatase 11 8 parts, cobalt nitrate 11 parts, sodium sulfite 20 parts, malonic acid 32 parts,
Ammonium fluoride 11 parts, dodecylbenzene sodium sulfonate 9 parts, 65 parts of water.
The preparation method of a kind of aluminium alloy non-chromium passivator, comprises the following steps:
(1) citric acid, sodium citrate, sodium peroxydisulfate, sodium silicate, phosphoric acid and water are poured in reactor, be 21 in temperature
DEG C, pressure be to stir 40 minutes under the conditions of 0.1MPa, agitator speed is 550 revs/min, is adjusted to by pH after having stirred
6；
(2) cobalt nitrate, sodium sulfite, malonic acid are added to the water, temperature be 58 DEG C, under the conditions of pressure is 0.24MPa
Magnetic agitation is dissolved, and after being completely dissolved when solution temperature is down to 26 DEG C, is added thereto to dodecylbenzene sodium sulfonate, fully stirs
Mix mixing；
(3) solution step (2) obtained adds in the solution that step (1) obtains, and flow velocity is 0.32m/s, in reactor
Temperature is 22 DEG C, and pressure is 0.1MPa, stirs while adding, and agitator speed is 600 revs/min；Treat step (2) institute
After the solution obtained is added completely in the solution that step (1) obtains, agitator continues stirring 48 minutes；
(4) adding ammonium fluoride in the solution that step (3) obtains, reactor temperature is 50 DEG C, and pressure is 0.1MPa, limit
Adding limit stirring, agitator speed is 600 revs/min.
With reference to national standard, to the aluminium alloy non-chromium passivating film of the present invention and the coating of traditional chromium hydrochlorate passivating film is supporting carries out performance pair
Than testing, result such as following table:
By testing inspection every in table as a result, it is possible to reach a conclusion, the aluminium alloy non-chromium passivator of the present invention is at Al alloy parts
The chromium-free passivating film of Surface Creation has the performance close with traditional chromium hydrochlorate passivating film.
Claims (1)
1. an aluminium alloy non-chromium passivator, is made by following raw material weight number proportioning: citric acid 35 parts, sodium citrate 22 parts,
Sodium peroxydisulfate 16 parts, sodium silicate 22 parts, phosphatase 11 8 parts, cobalt nitrate 11 parts, sodium sulfite 20 parts, malonic acid 32 parts,
Ammonium fluoride 11 parts, dodecylbenzene sodium sulfonate 9 parts, 65 parts of water；Described aluminium alloy non-chromium passivator is prepared by following methods:
(1) citric acid, sodium citrate, sodium peroxydisulfate, sodium silicate, phosphoric acid and water are poured in reactor, temperature be 21 DEG C,
Pressure is to stir 40 minutes under the conditions of 0.1MPa, and agitator speed is 550 revs/min, after having stirred, pH is adjusted to 6；(2)
Cobalt nitrate, sodium sulfite, malonic acid are added to the water, temperature be 58 DEG C, magnetic agitation is molten under the conditions of pressure is 0.24MPa
Solve, after being completely dissolved when solution temperature is down to 26 DEG C, be added thereto to dodecylbenzene sodium sulfonate, be sufficiently stirred for mixing；(3)
Solution step (2) obtained adds in the solution that step (1) obtains, and flow velocity is 0.32m/s, and reactor temperature is 22 DEG C,
Pressure is 0.1MPa, stirs while adding, and agitator speed is 600 revs/min；Treat that solution step (2) obtained is complete
After entirely adding in the solution that step (1) obtains, agitator continues stirring 48 minutes；(4) in the solution that step (3) obtains
Adding ammonium fluoride, reactor temperature is 50 DEG C, and pressure is 0.1MPa, stirs while adding, agitator speed is 600 turns/
Minute.
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| CN106521472A (en) * | 2016-12-09 | 2017-03-22 | 江美丽 | Aluminium alloy passivating reagent and passivating process |
| CN108179410A (en) * | 2017-11-22 | 2018-06-19 | 无锡伊佩克科技有限公司 | A kind of electronickelling chrome-free tanning agent and preparation method thereof |
| CN113122832A (en) * | 2019-12-30 | 2021-07-16 | 金盟科技（深圳）有限公司 | Chromium-free passivator and preparation method thereof |
| CN113122834B (en) * | 2019-12-30 | 2022-11-18 | 金盟科技（深圳）有限公司 | Magnesium alloy phosphorus-free passivator and preparation method thereof |
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| DE10010758A1 (en) * | 2000-03-04 | 2001-09-06 | Henkel Kgaa | Corrosion protection of zinc, aluminum and/or magnesium surfaces such as motor vehicle bodies, comprises passivation using complex fluorides of Ti, Zr, Hf, Si and/or B and organic polymers |
| CN100335680C (en) * | 2004-04-15 | 2007-09-05 | 郭瑞光 | Aluminium alloy chromium-free chemical converting liquid and its using method |
| CN101899657B (en) * | 2010-09-09 | 2011-12-14 | 上海丰野表面处理剂有限公司 | Chromium-free passivating treatment agent and method for preparing same |
| CN103215583B (en) * | 2013-04-16 | 2015-03-25 | 石佳正 | Galvanizing chromium-free iridescent passivation agent |
| CN103255403B (en) * | 2013-05-16 | 2015-07-01 | 山东建筑大学 | Non-chrome black passivator |
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