CN104404488A - Aluminum alloy chromium-free passivating agent and preparation method thereof - Google Patents

Aluminum alloy chromium-free passivating agent and preparation method thereof Download PDF

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CN104404488A
CN104404488A CN201410648275.6A CN201410648275A CN104404488A CN 104404488 A CN104404488 A CN 104404488A CN 201410648275 A CN201410648275 A CN 201410648275A CN 104404488 A CN104404488 A CN 104404488A
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尤为
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Wuxi Epic Technology Co Ltd
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Abstract

The invention discloses an aluminum alloy chromium-free passivating agent and a preparation method thereof. The aluminum alloy chromium-free passivating agent is prepared from the following raw materials by weight: 12-35 parts of citric acid, 10-22 parts of sodium citrate, 6-16 parts of sodium persulfate, 7-22 parts of sodium silicate, 6-18 parts of phosphoric acid, 2-11 parts of cobalt nitrate, 6-20 parts of sodium sulfite, 12-32 parts of malonic acid, 2-11 parts of ammonium fluoride, 1-9 parts of sodium dodecyl benzene sulfonate, and 25-65 parts of water. The passivating agent provided by the invention can achieve passivation at room temperature, has short passivation time, and is environment-friendly and pollution-free. The formed passivation film enhances the corrosion resistance of aluminum alloy.

Description

A kind of aluminium alloy non-chromium passivator and preparation method thereof
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 passivation always, hexavalent chromate Passivation Treatment significantly improves the erosion resistance of alloy, the passive film generated has self-regeneration effect, and it is cheap, use widely, but containing this hypertoxic carcinogens of sexavalent chrome in chromating liquid, have a strong impact on HUMAN HEALTH and contaminate environment.Current countries in the world all start restriction or prohibit the use chromating processes.Therefore develop the non-hexavalent chromium passivating technique of asepsis environment-protecting, efficient, low consumption, realize high-quality, eco-friendly steel surface passivator demand very urgent.
In addition, many factories employing trivalent chromate carrys out alternative hexavalent chromate and prepares steel surface passivator, as Chinese patent CN101130865A trivalent chromium black passivator and preparation method thereof, provide a kind of trivalent chromium passivator for metal finishing, although the treatment effect of this passivator is better, but trivalent chromium still has certain toxicity, factory is comparatively difficult to the wastewater treatment of trivalent chromic ion, and cost is higher.Therefore, develop chrome-free tanning agent to be more and more subject to people's attention.
For Al alloy parts, form fine and close oxide film because aluminium is easily oxidized in atmosphere, and to aluminium alloy inside, there is certain provide protection, but As time goes on the change of environment, oxide film is easily destroyed.Thus cause workpiece corrosion.Therefore the aluminium alloy non-chromium passivator develop and a kind ofly can protect aluminum workpiece, alleviate its surface corrosion, increasing the service life is particularly urgent.
Summary of the invention
The technical problem solved:
In order to provide one to be applicable to aluminum alloy surface Passivation Treatment, and to the passivator that environment does not pollute, 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, makes by following raw material weight number proportioning: citric acid 12-35 part, Trisodium Citrate 10-22 part, Sodium Persulfate 6-16 part, water glass 7-22 part, phosphoric acid 6-18 part, Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES 2-11 part, S-WAT 6-20 part, propanedioic acid 12-32 part, Neutral ammonium fluoride 2-11 part, Sodium dodecylbenzene 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, Trisodium Citrate 12-20 part, Sodium Persulfate 7-15 part, water glass 9-20 part, phosphoric acid 8-16 part, Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES 3-9 part, S-WAT 8-17 part, propanedioic acid 14-30 part, Neutral ammonium fluoride 4-10 part, Sodium dodecylbenzene 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, Trisodium Citrate 14-20 part, Sodium Persulfate 8-14 part, water glass 10-18 part, phosphatase 79-15 parts, Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES 4-8 part, S-WAT 9-16 part, propanedioic acid 15-28 part, Neutral ammonium fluoride 5-9 part, Sodium dodecylbenzene sulfonate 3-7 part, water 35-60 part.
A preparation method for aluminium alloy non-chromium passivator, comprises the following steps:
(1) citric acid, Trisodium Citrate, Sodium Persulfate, water glass, phosphoric acid and water are poured in reactor, temperature be 13-21 DEG C, pressure stirs 25-40 minute under being 0.05-0.1MPa condition, agitator speed is 400-550 rev/min, is adjusted between 4-6 after having stirred by pH;
(2) Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES, S-WAT, propanedioic acid are added to the water, temperature be 40-58 DEG C, pressure is 0.12-0.24MPa condition lower magnetic force stirring and dissolving, after dissolving completely when solution temperature is down to 22-26 DEG C, add Sodium dodecylbenzene sulfonate wherein, abundant stirring and evenly mixing;
(3) solution that step (2) obtains is added in the solution that step (1) obtains, flow velocity is 0.07-0.32m/s, and reactor temperature is 14-22 DEG C, and pressure is 0.05-0.1MPa, stir while adding, agitator speed is 450-600 rev/min; Add completely after in the solution that step (1) obtains until solution step (2) obtained, agitator continues to stir 35-48 minute;
(4) add Neutral ammonium fluoride in the solution obtained to step (3), reactor temperature is 35-50 DEG C, and pressure is 0.05-0.1MPa, stirs while adding, and agitator speed is 450-600 rev/min.
As a preferred technical solution of the present invention, citric acid, Trisodium Citrate, Sodium Persulfate, water glass, phosphoric acid and water are poured in reactor in (1) by step, temperature be 15-20 DEG C, pressure stirs 28-40 minute under being 0.06-0.1MPa condition, agitator speed is 450-550 rev/min, is adjusted between 4-6 by pH after having stirred.
As a preferred technical solution of the present invention, Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES, S-WAT, propanedioic acid are added to the water in (2) by step, temperature be 45-55 DEG C, pressure is 0.14-0.24MPa condition lower magnetic force stirring and dissolving, after dissolving completely when solution temperature is down to 22-26 DEG C, add Sodium dodecylbenzene sulfonate wherein, abundant stirring and evenly mixing.
As a preferred technical solution of the present invention, in step (3), the solution that step (2) obtains is added in the solution that step (1) obtains, flow velocity is 0.08-0.28m/s, reactor temperature is 14-20 DEG C, pressure is 0.07-0.1MPa, stirs while adding, and agitator speed is 500-600 rev/min; Add completely after in the solution that step (1) obtains until solution step (2) obtained, agitator continues to stir 37-45 minute.
As a preferred technical solution of the present invention, in step (4), in the solution that step (3) obtains, add Neutral ammonium fluoride, reactor temperature is 38-50 DEG C, 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 adopts above technical scheme to have following technique effect: the first, the aluminium alloy non-chromium passivator corrosion resistance nature prepared of the present invention and sexavalent chrome passivator performance close; The second, the passivator that the present invention obtains does not pollute environment; Three, the preparation method of aluminium alloy non-chromium passivator of the present invention avoids volatile acid to damage staff.
Embodiment
Embodiment 1:
A kind of aluminium alloy non-chromium passivator, makes by following raw material weight number proportioning: citric acid 12 parts, Trisodium Citrate 10 parts, Sodium Persulfate 6 parts, water glass 7 parts, phosphoric acid 6 parts, Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES 2 parts, S-WAT 6 parts, propanedioic acid 12 parts, Neutral ammonium fluoride 2 parts, Sodium dodecylbenzene sulfonate 1 part, 25 parts, water.
A preparation method for aluminium alloy non-chromium passivator, comprises the following steps:
(1) citric acid, Trisodium Citrate, Sodium Persulfate, water glass, phosphoric acid and water are poured in reactor, temperature be 13 DEG C, pressure be 0.05MPa condition under stir 25 minutes, agitator speed is 400 revs/min, after having stirred, pH is adjusted to 4;
(2) Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES, S-WAT, propanedioic acid are added to the water, temperature be 40 DEG C, pressure is 0.12MPa condition lower magnetic force stirring and dissolving, after dissolving completely when solution temperature is down to 22 DEG C, add Sodium dodecylbenzene sulfonate wherein, abundant stirring and evenly mixing;
(3) added by the solution that step (2) obtains in the solution that step (1) obtains, flow velocity is 0.07m/s, and reactor temperature is 14 DEG C, and pressure is 0.05MPa, stirs while adding, and agitator speed is 450 revs/min; Add completely after in the solution that step (1) obtains until solution step (2) obtained, agitator continues stirring 35 minutes;
(4) add Neutral ammonium fluoride in the solution obtained to step (3), reactor temperature is 35 DEG C, and pressure is 0.05MPa, stirs while adding, and agitator speed is 450 revs/min.
Embodiment 2:
A kind of aluminium alloy non-chromium passivator, makes by following raw material weight number proportioning: citric acid 15 parts, Trisodium Citrate 12 parts, Sodium Persulfate 8 parts, water glass 9 parts, phosphoric acid 8 parts, Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES 4 parts, S-WAT 8 parts, propanedioic acid 14 parts, Neutral ammonium fluoride 4 parts, Sodium dodecylbenzene sulfonate 2 parts, 35 parts, water.
A preparation method for aluminium alloy non-chromium passivator, comprises the following steps:
(1) citric acid, Trisodium Citrate, Sodium Persulfate, water glass, phosphoric acid and water are poured in reactor, temperature be 15 DEG C, pressure be 0.06MPa condition under stir 30 minutes, agitator speed is 450 revs/min, after having stirred, pH is adjusted to 4;
(2) Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES, S-WAT, propanedioic acid are added to the water, temperature be 45 DEG C, pressure is 0.14MPa condition lower magnetic force stirring and dissolving, after dissolving completely when solution temperature is down to 23 DEG C, add Sodium dodecylbenzene sulfonate wherein, abundant stirring and evenly mixing;
(3) added by the solution that step (2) obtains in the solution that step (1) obtains, flow velocity is 0.12m/s, and reactor temperature is 16 DEG C, and pressure is 0.06MPa, stirs while adding, and agitator speed is 500 revs/min; Add completely after in the solution that step (1) obtains until solution step (2) obtained, agitator continues stirring 38 minutes;
(4) add Neutral ammonium fluoride in the solution obtained to step (3), reactor temperature is 40 DEG C, and pressure is 0.06MPa, stirs while adding, and agitator speed is 500 revs/min.
Embodiment 3:
A kind of aluminium alloy non-chromium passivator, makes by following raw material weight number proportioning: citric acid 20 parts, Trisodium Citrate 15 parts, Sodium Persulfate 10 parts, water glass 12 parts, phosphatase 11 2 parts, Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES 6 parts, S-WAT 10 parts, propanedioic acid 16 parts, Neutral ammonium fluoride 6 parts, Sodium dodecylbenzene sulfonate 4 parts, 45 parts, water.
A preparation method for aluminium alloy non-chromium passivator, comprises the following steps:
(1) citric acid, Trisodium Citrate, Sodium Persulfate, water glass, phosphoric acid and water are poured in reactor, temperature be 17 DEG C, pressure be 0.06MPa condition under stir 33 minutes, agitator speed is 500 revs/min, after having stirred, pH is adjusted to 4;
(2) Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES, S-WAT, propanedioic acid are added to the water, temperature be 48 DEG C, pressure is 0.16MPa condition lower magnetic force stirring and dissolving, after dissolving completely when solution temperature is down to 24 DEG C, add Sodium dodecylbenzene sulfonate wherein, abundant stirring and evenly mixing;
(3) added by the solution that step (2) obtains in the solution that step (1) obtains, flow velocity is 0.15m/s, and reactor temperature is 18 DEG C, and pressure is 0.07MPa, stirs while adding, and agitator speed is 550 revs/min; Add completely after in the solution that step (1) obtains until solution step (2) obtained, agitator continues stirring 42 minutes;
(4) add Neutral ammonium fluoride in the solution obtained to step (3), reactor temperature is 42 DEG C, and pressure is 0.07MPa, stirs while adding, and agitator speed is 550 revs/min.
Embodiment 4:
A kind of aluminium alloy non-chromium passivator, makes by following raw material weight number proportioning: citric acid 25 parts, Trisodium Citrate 18 parts, Sodium Persulfate 13 parts, water glass 16 parts, phosphatase 11 5 parts, Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES 8 parts, S-WAT 15 parts, propanedioic acid 23 parts, Neutral ammonium fluoride 8 parts, Sodium dodecylbenzene sulfonate 6 parts, 50 parts, water.
A preparation method for aluminium alloy non-chromium passivator, comprises the following steps:
(1) citric acid, Trisodium Citrate, Sodium Persulfate, water glass, phosphoric acid and water are poured in reactor, temperature be 19 DEG C, pressure be 0.07MPa condition under stir 36 minutes, agitator speed is 500 revs/min, after having stirred, pH is adjusted to 5;
(2) Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES, S-WAT, propanedioic acid are added to the water, temperature be 52 DEG C, pressure is 0.22MPa condition lower magnetic force stirring and dissolving, after dissolving completely when solution temperature is down to 24 DEG C, add Sodium dodecylbenzene sulfonate wherein, abundant stirring and evenly mixing;
(3) added by the solution that step (2) obtains in the solution that step (1) obtains, flow velocity is 0.22m/s, and reactor temperature is 20 DEG C, and pressure is 0.08MPa, stirs while adding, and agitator speed is 550 revs/min; Add completely after in the solution that step (1) obtains until solution step (2) obtained, agitator continues stirring 45 minutes;
(4) add Neutral ammonium fluoride in the solution obtained to step (3), reactor temperature is 46 DEG C, and pressure is 0.08MPa, stirs while adding, and agitator speed is 550 revs/min.
Embodiment 5:
A kind of aluminium alloy non-chromium passivator, makes by following raw material weight number proportioning: citric acid 35 parts, Trisodium Citrate 22 parts, Sodium Persulfate 16 parts, water glass 22 parts, phosphatase 11 8 parts, Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES 11 parts, S-WAT 20 parts, propanedioic acid 32 parts, Neutral ammonium fluoride 11 parts, Sodium dodecylbenzene sulfonate 9 parts, 65 parts, water.
A preparation method for aluminium alloy non-chromium passivator, comprises the following steps:
(1) citric acid, Trisodium Citrate, Sodium Persulfate, water glass, phosphoric acid and water are poured in reactor, temperature be 21 DEG C, pressure be 0.1MPa condition under stir 40 minutes, agitator speed is 550 revs/min, after having stirred, pH is adjusted to 6;
(2) Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES, S-WAT, propanedioic acid are added to the water, temperature be 58 DEG C, pressure is 0.24MPa condition lower magnetic force stirring and dissolving, after dissolving completely when solution temperature is down to 26 DEG C, add Sodium dodecylbenzene sulfonate wherein, abundant stirring and evenly mixing;
(3) added by the solution that step (2) obtains in the solution that step (1) obtains, flow velocity is 0.32m/s, and reactor temperature is 22 DEG C, and pressure is 0.1MPa, stirs while adding, and agitator speed is 600 revs/min; Add completely after in the solution that step (1) obtains until solution step (2) obtained, agitator continues stirring 48 minutes;
(4) add Neutral ammonium fluoride in the solution obtained to step (3), reactor temperature is 50 DEG C, and pressure is 0.1MPa, stirs while adding, and agitator speed is 600 revs/min.
Carry out performance contrast test with reference to the coating of national standard to aluminium alloy non-chromium passive film of the present invention and traditional chromium hydrochlorate passive film is supporting, result is as following table:
By every testing inspection result in table, can reach a conclusion, aluminium alloy non-chromium passivator of the present invention has the performance close with traditional chromium hydrochlorate passive film at the chromium-free passivating film of Al alloy parts Surface Creation.

Claims (8)

1. an aluminium alloy non-chromium passivator, it is characterized in that, make by following raw material weight number proportioning: citric acid 12-35 part, Trisodium Citrate 10-22 part, Sodium Persulfate 6-16 part, water glass 7-22 part, phosphoric acid 6-18 part, Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES 2-11 part, S-WAT 6-20 part, propanedioic acid 12-32 part, Neutral ammonium fluoride 2-11 part, Sodium dodecylbenzene sulfonate 1-9 part, water 25-65 part.
2. a kind of aluminium alloy non-chromium passivator according to claim 1, it is characterized in that, make by following raw material weight number proportioning: citric acid 15-30 part, Trisodium Citrate 12-20 part, Sodium Persulfate 7-15 part, water glass 9-20 part, phosphoric acid 8-16 part, Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES 3-9 part, S-WAT 8-17 part, propanedioic acid 14-30 part, Neutral ammonium fluoride 4-10 part, Sodium dodecylbenzene sulfonate 2-8 part, water 30-60 part.
3. a kind of aluminium alloy non-chromium passivator according to claim 1, it is characterized in that, make by following raw material weight number proportioning: citric acid 16-28 part, Trisodium Citrate 14-20 part, Sodium Persulfate 8-14 part, water glass 10-18 part, phosphatase 79-15 parts, Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES 4-8 part, S-WAT 9-16 part, propanedioic acid 15-28 part, Neutral ammonium fluoride 5-9 part, Sodium dodecylbenzene sulfonate 3-7 part, water 35-60 part.
4. the preparation method of a kind of aluminium alloy non-chromium passivator described in claim 1, is characterized in that, comprise the following steps:
(1) citric acid, Trisodium Citrate, Sodium Persulfate, water glass, phosphoric acid and water are poured in reactor, temperature be 13-21 DEG C, pressure stirs 25-40 minute under being 0.05-0.1MPa condition, agitator speed is 400-550 rev/min, is adjusted between 4-6 after having stirred by pH;
(2) Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES, S-WAT, propanedioic acid are added to the water, temperature be 40-58 DEG C, pressure is 0.12-0.24MPa condition lower magnetic force stirring and dissolving, after dissolving completely when solution temperature is down to 22-26 DEG C, add Sodium dodecylbenzene sulfonate wherein, abundant stirring and evenly mixing;
(3) added by the solution that step (2) obtains in the solution that step (1) obtains, flow velocity is 0.07-0.32m/s, and reactor temperature is 14-22 DEG C, and pressure is 0.05-0.1MPa, stirs while adding, and agitator speed is 450-600 rev/min; Add completely after in the solution that step (1) obtains until solution step (2) obtained, agitator continues to stir 35-48 minute;
(4) add Neutral ammonium fluoride in the solution obtained to step (3), reactor temperature is 35-50 DEG C, and pressure is 0.05-0.1MPa, stirs while adding, and agitator speed is 450-600 rev/min.
5. the preparation method of a kind of aluminium alloy non-chromium passivator according to claim 4, it is characterized in that, citric acid, Trisodium Citrate, Sodium Persulfate, water glass, phosphoric acid and water are poured in reactor in (1) by step, temperature be 15-20 DEG C, pressure stirs 28-40 minute under being 0.06-0.1MPa condition, agitator speed is 450-550 rev/min, is adjusted between 4-6 by pH after having stirred.
6. the preparation method of a kind of aluminium alloy non-chromium passivator according to claim 4, it is characterized in that, Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES, S-WAT, propanedioic acid are added to the water in (2) by step, temperature be 45-55 DEG C, pressure is 0.14-0.24MPa condition lower magnetic force stirring and dissolving, after dissolving completely when solution temperature is down to 22-26 DEG C, add Sodium dodecylbenzene sulfonate wherein, abundant stirring and evenly mixing.
7. the preparation method of a kind of aluminium alloy non-chromium passivator according to claim 4, it is characterized in that, in step (3), the solution that step (2) obtains is added in the solution that step (1) obtains, flow velocity is 0.08-0.28m/s, and reactor temperature is 14-20 DEG C, and pressure is 0.07-0.1MPa, stir while adding, agitator speed is 500-600 rev/min; Add completely after in the solution that step (1) obtains until solution step (2) obtained, agitator continues to stir 37-45 minute.
8. the preparation method of a kind of aluminium alloy non-chromium passivator according to claim 4, it is characterized in that, in step (4), Neutral ammonium fluoride is added in the solution that step (3) obtains, reactor temperature is 38-50 DEG C, pressure is 0.07-0.1MPa, stirs while adding, and agitator speed is 500-600 rev/min.
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Cited By (4)

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Publication number Priority date Publication date Assignee Title
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
CN113122834A (en) * 2019-12-30 2021-07-16 金盟科技(深圳)有限公司 Magnesium alloy non-phosphorus passivator 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

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CN101899657A (en) * 2010-09-09 2010-12-01 上海丰野表面处理剂有限公司 Chromium-free passivating treatment agent and method for preparing same
CN103215583A (en) * 2013-04-16 2013-07-24 石佳正 Galvanizing chromium-free iridescent passivation agent
CN103255403A (en) * 2013-05-16 2013-08-21 山东建筑大学 Non-chrome black passivator

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US20030150524A1 (en) * 2000-03-04 2003-08-14 Winfried Wichelhaus Method for providing metal surfaces with protection against corrosion
CN1683590A (en) * 2004-04-15 2005-10-19 郭瑞光 Aluminium alloy chromium-free chemical converting liquid and its using method
CN101899657A (en) * 2010-09-09 2010-12-01 上海丰野表面处理剂有限公司 Chromium-free passivating treatment agent and method for preparing same
CN103215583A (en) * 2013-04-16 2013-07-24 石佳正 Galvanizing chromium-free iridescent passivation agent
CN103255403A (en) * 2013-05-16 2013-08-21 山东建筑大学 Non-chrome black passivator

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN113122834A (en) * 2019-12-30 2021-07-16 金盟科技(深圳)有限公司 Magnesium alloy non-phosphorus passivator 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

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