CN108085667A - Suitable for the corrosion-resistant black phosphating inorganic agent of medium temperature and preparation method of cast iron, carbon steel work-piece - Google Patents
Suitable for the corrosion-resistant black phosphating inorganic agent of medium temperature and preparation method of cast iron, carbon steel work-piece Download PDFInfo
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- CN108085667A CN108085667A CN201711419948.0A CN201711419948A CN108085667A CN 108085667 A CN108085667 A CN 108085667A CN 201711419948 A CN201711419948 A CN 201711419948A CN 108085667 A CN108085667 A CN 108085667A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
- C23C22/40—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing molybdates, tungstates or vanadates
- C23C22/44—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing molybdates, tungstates or vanadates containing also fluorides or complex fluorides
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- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Treatment Of Metals (AREA)
Abstract
The present invention disclose it is a kind of reduce phosphatization temperature, improve phosphatization speed, improve phosphatization quality suitable for cast iron, the corrosion-resistant black phosphating inorganic agent of the medium temperature of carbon steel work-piece, raw materials used and mass percent is as follows:Phosphatase 11 0 ~ 20%, zinc oxide 6 ~ 8%, the nitric acid 15 ~ 20% of mass percent concentration 69%, manganese nitrate 1 ~ 12%, manganese carbonate 1 ~ 10%, nickel nitrate 0.1 ~ 2%, 4 sodium 0.1 ~ 2% of EDTA, sodium fluoride 0.1 ~ 2%, fluosilicic acid 0.1 ~ 2%, ammonium citrate 0.1 ~ 2%, cupric sulfate pentahydrate 0.1 ~ 1%, sodium molybdate 0.1 ~ 1%, ammonium molybdate 0.1 ~ 1%, sodium peroxydisulfate 0.1 ~ 1%, selenous acid 0.1 ~ 1% and water surplus.
Description
Technical field
Phosphatization temperature, raising phosphatization speed can be reduced the present invention relates to a kind of black phosphating inorganic agent, especially one kind, carried
High phosphatization quality is suitable for cast iron, the corrosion-resistant black phosphating inorganic agent of the medium temperature of carbon steel work-piece and preparation method.
Background technology
Traditional cast iron, wear-resisting, the anticorrosion phosphatization of carbon steel work-piece use high temperature manganese-series phosphorized substantially.High temperature is manganese-series phosphorized
Film layer is mainly by Mn3(PO4)2、(Mn·Fe)2 PO4(OH)、Mn3(PO4)2·1.5H2The mixing stereotyped crystal of O compositions.It is tied
Structure is spread microcellular structure, and appearance is in ash or grey black.The manganese-series phosphorized film layer of high temperature has preferable antirust heat-resisting and against corrosion
Performance, and can effectively reduce coefficient of friction, increase lubricity, prevent from stinging scratch.But phosphating process operation temperature is high(90~98
℃), phosphorization treatment time is longer, therefore energy consumption is higher.At present, in order to obtain the phosphating coat of black beauty on cast iron, carbon steel surface
Layer, generally require cycle using phosphatization-pickling-phosphatization phosphating process either it is first pre- it is black after phosphating process or by phosphatization
The black treatment process of after stain, there is technique is cumbersome, low production efficiency, unstable tank liquor and phosphorization membrane performance the shortcomings of.It removes
Outside this, phosphatization poststaining can also cause phosphorization membrane centainly to damage, and influence wear-resistant and corrosion resistance.
The content of the invention
The present invention be in order to solve the above-mentioned technical problem present in the prior art, provide one kind can reduce phosphatization temperature,
Improve phosphatization speed, improve phosphatization quality be suitable for cast iron, the corrosion-resistant black phosphating inorganic agent of the medium temperature of carbon steel work-piece and system
Preparation Method.
The present invention technical solution be:It is a kind of to be suitable for cast iron, at the corrosion-resistant black phosphating of the medium temperature of carbon steel work-piece
Manage agent, it is characterised in that raw materials used and mass percent is as follows:Phosphatase 11 0 ~ 20%, zinc oxide 6 ~ 8%, mass percent concentration
69% nitric acid 15 ~ 20%, manganese nitrate 1 ~ 12%, manganese carbonate 1 ~ 10%, nickel nitrate 0.1 ~ 2%, EDTA-4 sodium 0.1 ~ 2%, sodium fluoride 0.1
~ 2%, fluosilicic acid 0.1 ~ 2%, ammonium citrate 0.1 ~ 2%, cupric sulfate pentahydrate 0.1 ~ 1%, sodium molybdate 0.1 ~ 1%, ammonium molybdate 0.1 ~ 1%, mistake
Sodium sulphate 0.1 ~ 1%, selenous acid 0.1 ~ 1% and water surplus.
It is a kind of above-mentioned suitable for cast iron, the preparation method of the corrosion-resistant black phosphating inorganic agent of the medium temperature of carbon steel work-piece, it is special
Sign is to carry out in accordance with the following steps:Quantitative water of weighing first is added in stainless steel cauldron, starts blender, setting speed
For 60 ~ 80 revs/min, the phosphoric acid of weighing is sequentially added, nitric acid stirs 30 minutes, the oxidation that addition weighs slowly successively afterwards
Zinc, manganese carbonate, stirring to being transparent, then add in slowly successively the nickel nitrate weighed, sodium fluoride, fluosilicic acid, ammonium citrate,
EDTA-4 sodium, stirring add cupric sulfate pentahydrate, sodium molybdate, sodium peroxydisulfate, selenous acid, fully in greenish transparent liquid
Stirring is to being light blue green transparent liquid.
The present invention is on the basis of conventional medium temperature Zn-Al hydrotalcite bonderite, introduces chelating agent, nigrescence substance and phosphatization and promotes
The substances such as agent, each component interaction can form one layer of fine and close, fine and smooth ater phosphatization on cast iron, carbon steel work-piece surface
Film layer improves the degree of blackness of phosphorization membrane, the uniformity, adhesive force, corrosion resistance and the performances such as wear-resisting, improves phosphorization membrane
Quality;Black phosphating temperature can be reduced(65~75℃), phosphatization speed is improved, and then reduces phosphatization energy consumption, improve production efficiency.
Specific embodiment
Embodiment 1:
The present invention's is suitable for cast iron, the corrosion-resistant black phosphating inorganic agent of the medium temperature of carbon steel work-piece, raw materials used and quality percentage
Than as follows:Phosphoric acid 20%, zinc oxide 6%, the nitric acid 20% of mass percent concentration 69%, manganese nitrate 1%, manganese carbonate 10%, nickel nitrate
0.1%th, EDTA-4 sodium 2%, sodium fluoride 0.1%, fluosilicic acid 2%, ammonium citrate 0.1%, cupric sulfate pentahydrate 1%, sodium molybdate 0.1%, molybdic acid
Ammonium 1%, sodium peroxydisulfate 0.1%, selenous acid 1% and water surplus.
Preparation method carries out in accordance with the following steps:Quantitative water of weighing first is added in stainless steel cauldron, starts stirring
Device, setting speed are 60 revs/min, sequentially add the phosphoric acid of weighing, nitric acid stirs 30 minutes, addition weighing slowly successively afterwards
Zinc oxide, manganese carbonate, stirring is to being transparent, then adds in the nickel nitrate weighed, sodium fluoride, fluosilicic acid, lemon slowly successively
Sour ammonium, EDTA-4 sodium, stirring add cupric sulfate pentahydrate, sodium molybdate, sodium peroxydisulfate, selenous acid to being in greenish transparent liquid,
It is stirred well to and is light blue green transparent liquid.
Embodiment 2:
The present invention's is suitable for cast iron, the corrosion-resistant black phosphating inorganic agent of the medium temperature of carbon steel work-piece, raw materials used and quality percentage
Than as follows:Phosphatase 11 0%, zinc oxide 8%, the nitric acid 15% of mass percent concentration 69%, manganese nitrate 12%, manganese carbonate 1%, nickel nitrate
2%th, EDTA-4 sodium 0.1%, sodium fluoride 2%, fluosilicic acid 0.1%, ammonium citrate 2%, cupric sulfate pentahydrate 0.1%, sodium molybdate 1%, ammonium molybdate
0.1%th, sodium peroxydisulfate 1%, selenous acid 0.1% and water surplus.
Preparation method carries out in accordance with the following steps:Quantitative water of weighing first is added in stainless steel cauldron, starts stirring
Device, setting speed are 70 revs/min, sequentially add the phosphoric acid of weighing, nitric acid stirs 30 minutes, addition weighing slowly successively afterwards
Zinc oxide, manganese carbonate, stirring is to being transparent, then adds in the nickel nitrate weighed, sodium fluoride, fluosilicic acid, lemon slowly successively
Sour ammonium, EDTA-4 sodium, stirring add cupric sulfate pentahydrate, sodium molybdate, sodium peroxydisulfate, selenous acid to being in greenish transparent liquid,
It is stirred well to and is light blue green transparent liquid.
Embodiment 3:
The present invention's is suitable for cast iron, the corrosion-resistant black phosphating inorganic agent of the medium temperature of carbon steel work-piece, raw materials used and quality percentage
Than as follows:Phosphatase 11 5%, zinc oxide 7%, the nitric acid 18% of mass percent concentration 69%, manganese nitrate 6%, manganese carbonate 5%, nickel nitrate
1%th, EDTA-4 sodium 1%, sodium fluoride 1%, fluosilicic acid 1%, ammonium citrate 1%, cupric sulfate pentahydrate 0.5%, sodium molybdate 0.5%, ammonium molybdate
0.5%th, sodium peroxydisulfate 0.5%, selenous acid 0.5% and water surplus.
Preparation method carries out in accordance with the following steps:Quantitative water of weighing first is added in stainless steel cauldron, starts stirring
Device, setting speed are 60 ~ 80 revs/min, sequentially add the phosphoric acid of weighing, nitric acid stirs 30 minutes, addition slowly successively afterwards
Zinc oxide, the manganese carbonate of weighing, stirring to being transparent, then add in slowly successively the nickel nitrate weighed, sodium fluoride, fluosilicic acid,
Ammonium citrate, EDTA-4 sodium, stirring add cupric sulfate pentahydrate, sodium molybdate, sodium peroxydisulfate, Asia in greenish transparent liquid
Selenic acid is stirred well to and is light blue green transparent liquid.
The corrosion-resistant black phosphating process parameter of medium temperature of the embodiment of the present invention is as follows:
20% add in the preparation working solution of the embodiment of the present invention 1,2 or 3 by mass percentage;
Total acidity:75~95 pt;
Sour ratio:8~12;
Temperature:65~75℃;
Time:6~12 min.
Technological process is:
Cast iron, carbon steel work-piece enter:Degreasing → washing → washing → pickling(There are rust, oxide skin workpiece)→ washing → neutralization(Through
Pickling workpiece)→ washing → table tune → black phosphating → washing → washing → drying.
By treated cast iron, the carbon steel work-piece of the embodiment of the present invention 1,2 or 3, can be formed in its face one layer it is fine and close,
Fine and smooth, corrosion-resistant, wear-resisting ater phosphorization membrane.
Claims (2)
1. it is a kind of be suitable for cast iron, the corrosion-resistant black phosphating inorganic agent of the medium temperature of carbon steel work-piece, it is characterised in that it is raw materials used and
Mass percent is as follows:Phosphatase 11 0 ~ 20%, zinc oxide 6 ~ 8%, the nitric acid 15 ~ 20% of mass percent concentration 69%, manganese nitrate 1 ~
12%th, manganese carbonate 1 ~ 10%, nickel nitrate 0.1 ~ 2%, EDTA-4 sodium 0.1 ~ 2%, sodium fluoride 0.1 ~ 2%, fluosilicic acid 0.1 ~ 2%, citric acid
Ammonium 0.1 ~ 2%, cupric sulfate pentahydrate 0.1 ~ 1%, sodium molybdate 0.1 ~ 1%, ammonium molybdate 0.1 ~ 1%, sodium peroxydisulfate 0.1 ~ 1%, selenous acid 0.1 ~
1% and water surplus.
2. a kind of preparation for being suitable for cast iron, the corrosion-resistant black phosphating inorganic agent of the medium temperature of carbon steel work-piece as described in claim 1
Method, it is characterised in that carry out in accordance with the following steps:Quantitative water of weighing first is added in stainless steel cauldron, starts stirring
Device, setting speed are 60 ~ 80 revs/min, sequentially add the phosphoric acid of weighing, nitric acid stirs 30 minutes, addition slowly successively afterwards
Zinc oxide, the manganese carbonate of weighing, stirring to being transparent, then add in slowly successively the nickel nitrate weighed, sodium fluoride, fluosilicic acid,
Ammonium citrate, EDTA-4 sodium, stirring add cupric sulfate pentahydrate, sodium molybdate, sodium peroxydisulfate, Asia in greenish transparent liquid
Selenic acid is stirred well to and is light blue green transparent liquid.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110565102A (en) * | 2019-09-24 | 2019-12-13 | 广州市方立新材料科技有限公司 | iron material oil removal laminating liquid and preparation method thereof |
JP2021055122A (en) * | 2019-09-27 | 2021-04-08 | 株式会社Adeka | Surface treatment method of stainless steel |
CN113774367A (en) * | 2021-09-09 | 2021-12-10 | 浙江伟星实业发展股份有限公司 | Coloring liquid and application thereof |
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CN1127800A (en) * | 1995-08-01 | 1996-07-31 | 刘光炳 | Cold black coslettising liquid |
CN101665936A (en) * | 2009-09-27 | 2010-03-10 | 大连三达奥克化学股份有限公司 | Normal-temperature phosphating agent for pre-processing before spray-coating of steel plate workpiece and preparation method thereof |
CN101671823A (en) * | 2009-09-27 | 2010-03-17 | 大连三达奥克化学股份有限公司 | Barrel plating phosphating agent before coating electrophoresis of cartridge case and preparation method thereof |
CN104711560A (en) * | 2013-12-14 | 2015-06-17 | 三达奥克化学股份有限公司 | Novel medium-temperature zinc-manganese system phosphating agent and production method thereof |
CN106048577A (en) * | 2016-07-06 | 2016-10-26 | 安徽红桥金属制造有限公司 | Hardware stamping part surface treatment process |
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2017
- 2017-12-25 CN CN201711419948.0A patent/CN108085667A/en active Pending
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
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CN1127800A (en) * | 1995-08-01 | 1996-07-31 | 刘光炳 | Cold black coslettising liquid |
CN101665936A (en) * | 2009-09-27 | 2010-03-10 | 大连三达奥克化学股份有限公司 | Normal-temperature phosphating agent for pre-processing before spray-coating of steel plate workpiece and preparation method thereof |
CN101671823A (en) * | 2009-09-27 | 2010-03-17 | 大连三达奥克化学股份有限公司 | Barrel plating phosphating agent before coating electrophoresis of cartridge case and preparation method thereof |
CN104711560A (en) * | 2013-12-14 | 2015-06-17 | 三达奥克化学股份有限公司 | Novel medium-temperature zinc-manganese system phosphating agent and production method thereof |
CN106048577A (en) * | 2016-07-06 | 2016-10-26 | 安徽红桥金属制造有限公司 | Hardware stamping part surface treatment process |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110565102A (en) * | 2019-09-24 | 2019-12-13 | 广州市方立新材料科技有限公司 | iron material oil removal laminating liquid and preparation method thereof |
JP2021055122A (en) * | 2019-09-27 | 2021-04-08 | 株式会社Adeka | Surface treatment method of stainless steel |
JP7377658B2 (en) | 2019-09-27 | 2023-11-10 | 株式会社Adeka | Methods for surface treatment of stainless steel, methods for producing surface-treated stainless steel, and solutions used in these methods |
CN113774367A (en) * | 2021-09-09 | 2021-12-10 | 浙江伟星实业发展股份有限公司 | Coloring liquid and application thereof |
CN113774367B (en) * | 2021-09-09 | 2024-03-26 | 浙江伟星实业发展股份有限公司 | Coloring liquid and application thereof |
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Application publication date: 20180529 |