CN107326353A - For the galvanized steel plain sheet rapid phosphorization agent of color coating and its application - Google Patents

For the galvanized steel plain sheet rapid phosphorization agent of color coating and its application Download PDF

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Publication number
CN107326353A
CN107326353A CN201710592345.4A CN201710592345A CN107326353A CN 107326353 A CN107326353 A CN 107326353A CN 201710592345 A CN201710592345 A CN 201710592345A CN 107326353 A CN107326353 A CN 107326353A
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CN
China
Prior art keywords
galvanized steel
acid
color coating
plain sheet
steel plain
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Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201710592345.4A
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Chinese (zh)
Inventor
钟金环
彭强
徐孙令
张凯
李翀
王建
王一建
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Hangzhou Pentatomic Science & Technology Co Ltd
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Hangzhou Pentatomic Science & Technology Co Ltd
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Priority to CN201710592345.4A priority Critical patent/CN107326353A/en
Publication of CN107326353A publication Critical patent/CN107326353A/en
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    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C22/00Chemical 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
    • C23C22/05Chemical 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
    • C23C22/06Chemical 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
    • C23C22/34Chemical 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 fluorides or complex fluorides
    • C23C22/36Chemical 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 fluorides or complex fluorides containing also phosphates
    • C23C22/362Chemical 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 fluorides or complex fluorides containing also phosphates containing also zinc cations

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  • Chemical & Material Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Treatment Of Metals (AREA)

Abstract

The invention discloses a kind of for the galvanized steel plain sheet rapid phosphorization agent of color coating and its application, the rapid phosphorization agent is mainly made up of zinc oxide, phosphoric acid, nitrate, organic acid (salt), organic phosphorus compound, inorganic fluoro complex, compound accelerant, additive and water etc., can be applied to the processing of the galvanized steel fast bonderizing before color steel application.The rapid phosphorization agent has processing time short, efficient film forming, 5 15 seconds can be in zinc-plated substrate surface formation phosphating coat, and normal temperature processing saves the energy without heating, and phosphorization membrane uniform and smooth is smooth without show-through, and the resistance to neutral salt spray test time was up to more than 48 hours.

Description

For the galvanized steel plain sheet rapid phosphorization agent of color coating and its application
Technical field
The present invention relates to a kind for the treatment of technology of protecting metallic surface, more particularly to a kind of galvanized steel plain sheet for color coating Rapid phosphorization agent and its application.
Technical background
Color coated steel sheet is, for substrate, to pass through on tandem mill with cold-strip steel or galvanized steel plain sheet (electrogalvanizing and galvanizing) External coating pre-treatment (degreasing, cleaning, chemical conversion treatment), applies in continuous method and coats (rolling method), through overbaking Solidification and the product for cooling down and being made.Because color coated steel sheet with the good coloring of organic coating, mouldability, corrosion resistance, Dicoration, the high intensity and workability for having steel plate again can easily carry out panel beating manufacture, and be widely used in and build Build, electrical equipment, the production field such as transport.
Galvanized steel plain sheet has certain corrosion resistance, but does not carry out Seal treatment or rust preventing, also easily in hygrothermal environment Produce different degrees of corrosion and discoloration.And carry out chemical conversion treatment film process (such as before galvanized steel plain sheet substrate carries out color coating Phosphatization) it is extremely necessary treatment process together.Usually, the production technology speed of processing unit is generally 25~120 ms/min (general effective phosphorization treatment time is 5-15 seconds), the fast filming that high-speed and continuous operation is converted to its surface chemistry is proposed will Ask.Quick phosphorization process or phosphating solution disclosed in the patents such as CN201410124896.4, only it is qualitative for " processing time is short " (not Its is quick for quantitative description);CN201310702824.9、CN201310148650.6、CN201410672073.5、 Quick phosphorization process or phosphating solution disclosed in the patents such as CN201410744600.9 then illustrate that phosphorization treatment time is 1.5-6 points Clock, in addition it is longer;The patents such as CN201210187500.1 disclose a kind of quick electrolysis phosphating solution suitable for wire drawing and Its phosphating process, 5~120 seconds its processing times, but because its application need to be limited with stand-by power source and electrode system.It is above-described Many quick phosphorization process or phosphating solution can not still meet the color coated steel sheet pre-treatment production requirement run at high speed.
The content of the invention
For above technical problem, it is an object of the invention to provide a kind of galvanized steel plain sheet rapid phosphorization agent for color coating And its application, galvanized steel plain sheet coiled material is handled using the rapid phosphorization agent, with following advantage:(1) processing time is short, film forming Efficiency high, 5-15 seconds can be in substrate surface formation phosphating coat;(2) save, normal-temperature operation, without heating, save the energy;(3) Superior performance, the phosphating coat uniform and smooth of acquisition is smooth without show-through, and the resistance to neutral salt spray test time was up to more than 48 hours.
Technical solution of the present invention is specific as follows:
Preparation and application for the galvanized steel plain sheet rapid phosphorization agent of color coating, it is characterised in that:Constitutive material each component Mass percent is:
The preparation method of described fast bonderizing liquor comprises the following steps:
(1) toward addition phosphoric acid in reactor, open reactor and be stirred;
(2) toward the 40-50% of water inventory needed for addition in reactor;
(3) the pulpous state zinc oxide being tuned into advance with a small amount of water toward addition in reactor, stirring makes it thoroughly dissolve;
(4) toward addition in reactor to the 80-90% of required water inventory;
(5) respectively toward adding nitrate in reactor, it is organic acid (salt), organic phosphorus compound, inorganic fluoro complex, compound Accelerator, stirring is thoroughly mixed it;
(6) toward addition additive in reactor, stirring is thoroughly mixed it;
(7) excess water is finally supplied, stirring makes it produce rapid phosphorization agent after being thoroughly mixed.
It is preferred that, described nitrate is selected from zinc nitrate, copper nitrate, calcium nitrate, magnesium nitrate, cerous nitrate, cerous nitrate One or more.
It is preferred that, described organic acid (salt) is selected from citric acid, acrylic acid, tartaric acid, oxalic acid and gluconic acid and its salt In one or more.
It is preferred that, the one or more of described organic phosphorus compound in phytic acid and its salt.
It is preferred that, the one kind or many of described inorganic fluoro complex in fluosilicic acid, fluoboric acid, fluorophosphoric acid and its salt Kind.
It is preferred that, described compound accelerant is selected from sodium chlorate, sodium molybdate, sodium nitrate, natrium nitrosum, HAS, nitre Two or more in base guanidine and nitrobenzene sodium sulfonate, quality hundred of any one selected component relative to compound accelerant Divide and be not less than 5% than content.
It is preferred that, described additive is 0.2-0.8mol/L ferrous sulfate (ammonium) solution and 0.2-0.8mol/L EDTA Isometric mixture of solution (both molar concentrations are identical).
The invention also discloses the application that described fast bonderizing liquor is handled in the galvanized steel plain sheet fast bonderizing for color coating. The application optimum condition is:Treatment temperature is 20-35 DEG C, and pH is 2.5-3.5, and the time is 6-9 seconds, is handled using roller coat.
Above-mentioned rapid phosphorization agent is applied to work continuously, its production technology is:Unreel → pre- oil removing → washing 1 → removes Oil → 2 → activation of washing → washing 3 → zinc-plated → 4 → table of washing tune → fast bonderizing → 5 → drying of washing → winding.Processing is received After testing, phosphating coat uniform and smooth is without show-through, lightness more than 85% (electrolytic zinc-coated steel sheet), resistance to neutral salt spray examination for zinc-plated base material after volume Test 48 hours and occur without red rust, meet product technology requirement.
To the zinc-plated coil being disposed, it can be painted or the production of water paint roller coat.
Galvanized steel plain sheet fast bonderizing processing for color coating has following advantage:(1) processing time is short, film forming efficiency Height, 5-15 seconds can be in substrate surface formation phosphating coat;(2) save, normal-temperature operation, without heating, save the energy;(3) performance Superior, the phosphating coat uniform and smooth of acquisition is smooth without show-through, and the resistance to neutral salt spray test time was up to more than 48 hours.
Embodiment
Embodiment 1:
Preparation and application for the plated steel sheet rapid phosphorization agent of color coating, it is characterised in that:Constitutive material each component Mass percent be:
The preparation method of described fast bonderizing liquor comprises the following steps:
(1) toward addition phosphoric acid in reactor, open reactor and be stirred;
(2) toward the 40-50% of water inventory needed for addition in reactor;
(3) the pulpous state zinc oxide being tuned into advance with a small amount of water toward addition in reactor, stirring makes it thoroughly dissolve;
(4) toward addition in reactor to the 80-90% of required water inventory;
(5) respectively toward addition zinc nitrate, tartaric acid, phytic acid, fluosilicic acid, sodium nitrate/HAS (5 in reactor:1 mixes Compound), stirring is thoroughly mixed it;
(6) toward addition copperas solution and EDTA solution (concentration is 0.2mol/L) mixture in reactor, stirring Uniformly it is thoroughly mixed it;
(7) excess water is finally supplied, stirring makes it produce rapid phosphorization agent after being thoroughly mixed.
Fast bonderizing liquor is 25 DEG C in the temperature of the plated steel sheet fast bonderizing processing for color coating, pH3.5, and the time is 9 seconds, handled using roller coat.Technique for applying is:Unreel → pre- oil removing → 1 → oil removing of washing → 2 → activation of washing → washing 3 → plating Zinc → 4 → table of washing tune → fast bonderizing → 5 → drying of washing → winding.Electrogalvanizing base material after processing after testing, phosphating coat Weigh about 3.6g/m2, phosphating coat uniform and smooth is smooth, and without show-through, lightness 88%, resistance to neutral salt spray test occurs without red rust in 48 hours, Meet product technology requirement.
Comparative example 1:
Plated steel sheet for color coating does not carry out fast bonderizing processing, its base material after testing, zinc coat about 10.2g/m2, Lightness 86%, resistance to neutral salt spray test<There is red rust within 5 hours.
Embodiment 2:
Preparation and application for the plated steel sheet rapid phosphorization agent of color coating, it is characterised in that:Constitutive material each component Mass percent be:
The preparation method step be the same as Example 1 of described fast bonderizing liquor.
Fast bonderizing liquor is 35 DEG C in the temperature of the plated steel sheet fast bonderizing processing for color coating, pH2.5, and the time is 6 seconds, handled using roller coat.After testing, phosphating coat uniform and smooth is smooth without show-through, lightness 87% for electrogalvanizing base material after processing, Resistance to neutral salt spray test occurs without red rust in 48 hours, meets product technology requirement.
Embodiment 3:
Preparation and application for the hot-dip galvanizing sheet steel rapid phosphorization agent of color coating, it is characterised in that:Constitutive material each component Mass percent be:
The preparation method step be the same as Example 1 of described fast bonderizing liquor.
Fast bonderizing liquor is 20 DEG C in the temperature of the hot-dip galvanizing sheet steel fast bonderizing processing for color coating, pH2.8, and the time is 8 seconds, handled using roller coat.After testing, phosphating coat uniform and smooth is smooth without show-through, resistance to neutral salt spray for galvanizing base material after processing Experiment occurs without red rust in 72 hours, meets product technology requirement.
Comparative example 2:
Hot-dip galvanizing sheet steel for color coating does not carry out fast bonderizing processing, its base material after testing, zinc coat about 41.3g/m2, Resistance to neutral salt spray test can be by 24 hours, but do not tested by 40 hours.

Claims (10)

1. a kind of galvanized steel plain sheet rapid phosphorization agent for color coating, it is characterised in that:The mass percent of constitutive material each component For:
The preparation method step of described fast bonderizing liquor is as follows:
(1) toward addition phosphoric acid in reactor, open reactor and be stirred;
(2) toward the 40-50% of water inventory needed for addition in reactor;
(3) the pulpous state zinc oxide being tuned into advance with a small amount of water toward addition in reactor, stirring makes it thoroughly dissolve;
(4) toward addition in reactor to the 80-90% of required water inventory;
(5) respectively toward addition nitrate, organic acid (salt), organic phosphorus compound, inorganic fluoro complex, compound promotion in reactor Agent, stirring is thoroughly mixed it;
(6) toward addition additive in reactor, stirring is thoroughly mixed it;
(7) excess water is finally supplied, stirring makes it produce rapid phosphorization agent after being thoroughly mixed.
2. it is used for the galvanized steel plain sheet rapid phosphorization agent of color coating as claimed in claim 1, it is characterised in that described nitrate choosing One or more from zinc nitrate, copper nitrate, calcium nitrate, magnesium nitrate, cerous nitrate, cerous nitrate.
3. it is used for the galvanized steel plain sheet rapid phosphorization agent of color coating as claimed in claim 1, it is characterised in that described organic acid The one or more of (salt) in citric acid, acrylic acid, tartaric acid, oxalic acid and gluconic acid and its salt.
4. it is used for the galvanized steel plain sheet rapid phosphorization agent of color coating as claimed in claim 1, it is characterised in that described organic phosphatization One or more of the compound in phytic acid and its salt.
5. it is used for the galvanized steel plain sheet rapid phosphorization agent of color coating as claimed in claim 1, it is characterised in that described inorganic fluorine network One or more of the compound in fluosilicic acid, fluoboric acid, fluorophosphoric acid and its salt.
6. the described galvanized steel plain sheet rapid phosphorization agent for color coating as claimed in claim 1, it is characterised in that described answers Close two of accelerator in sodium chlorate, sodium molybdate, sodium nitrate, natrium nitrosum, HAS, nitroguanidine and nitrobenzene sodium sulfonate Plant or a variety of.
7. the described galvanized steel plain sheet rapid phosphorization agent for color coating as claimed in claim 6, it is characterised in that compound to promote The selected component of any one in agent is not less than 5% relative to the mass percentage content of compound accelerant.
8. it is used for the galvanized steel plain sheet rapid phosphorization agent of color coating as claimed in claim 1, it is characterised in that described additive is Isometric mixture of 0.2-0.8mol/LEDTA solution and 0.2-0.8mol/L ferrous sulfate or sulfuric acid imonium solution, and mixing The molar concentration of EDTA and ferrous sulfate or sulfuric acid imonium is equal in thing.
9. application of the rapid phosphorization agent in the protection of zinc-plated substrate surface described in claim 1, it is characterised in that for color coating Galvanized steel plain sheet fast bonderizing processing.
10. application as claimed in claim 9, it is characterised in that be to the application conditions of zinc-plated base material:Treatment temperature is 1-40 DEG C, pH1.5-4, the time is 5-15 seconds, is handled using roller coat.
CN201710592345.4A 2017-07-19 2017-07-19 For the galvanized steel plain sheet rapid phosphorization agent of color coating and its application Pending CN107326353A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107881495A (en) * 2017-11-18 2018-04-06 蚌埠市宏大制药机械有限公司 A kind of processing method of medicine die surface
CN109778161A (en) * 2019-02-23 2019-05-21 浙江华锦建筑装饰设计有限公司 A kind of antidetonation prefabricated buildings
CN110252630A (en) * 2019-07-16 2019-09-20 山东圣士达环保科技有限公司 A kind of thin plate hot galvanizing toner paint line and its production technology
CN110699681A (en) * 2019-10-24 2020-01-17 河南北方红阳机电有限公司 Spraying phosphating process for high-strength steel and hard aluminum alloy combination
CN111304574A (en) * 2020-03-27 2020-06-19 句容市茅山交通工程镀锌材料有限公司 Steel surface galvanizing rust-proof treatment process
WO2024027666A1 (en) * 2022-08-01 2024-02-08 宝山钢铁股份有限公司 Environment-friendly water-based treatment agent for improving phosphatability of high-strength steel

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5141575A (en) * 1989-04-07 1992-08-25 Henkel Corporation Surface treatment for zinciferous surfaces
CN101935831A (en) * 2010-08-16 2011-01-05 景阳富 Phosphatizing liquid and preparation method thereof
CN102719819A (en) * 2011-03-30 2012-10-10 重庆市荣时金属表面处理剂有限公司 General phosphating agent
CN103114282A (en) * 2013-02-27 2013-05-22 湖南中骏科技有限公司 Washing-free normal-temperature phosphating solution after steel workpiece phosphating and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5141575A (en) * 1989-04-07 1992-08-25 Henkel Corporation Surface treatment for zinciferous surfaces
CN101935831A (en) * 2010-08-16 2011-01-05 景阳富 Phosphatizing liquid and preparation method thereof
CN102719819A (en) * 2011-03-30 2012-10-10 重庆市荣时金属表面处理剂有限公司 General phosphating agent
CN103114282A (en) * 2013-02-27 2013-05-22 湖南中骏科技有限公司 Washing-free normal-temperature phosphating solution after steel workpiece phosphating and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
黄玉媛等: "《精细化学品实用配方手册》", 31 January 2009 *

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107881495A (en) * 2017-11-18 2018-04-06 蚌埠市宏大制药机械有限公司 A kind of processing method of medicine die surface
CN109778161A (en) * 2019-02-23 2019-05-21 浙江华锦建筑装饰设计有限公司 A kind of antidetonation prefabricated buildings
CN110252630A (en) * 2019-07-16 2019-09-20 山东圣士达环保科技有限公司 A kind of thin plate hot galvanizing toner paint line and its production technology
CN110699681A (en) * 2019-10-24 2020-01-17 河南北方红阳机电有限公司 Spraying phosphating process for high-strength steel and hard aluminum alloy combination
CN110699681B (en) * 2019-10-24 2021-12-14 河南北方红阳机电有限公司 Spraying phosphating process for high-strength steel and hard aluminum alloy combination
CN111304574A (en) * 2020-03-27 2020-06-19 句容市茅山交通工程镀锌材料有限公司 Steel surface galvanizing rust-proof treatment process
WO2024027666A1 (en) * 2022-08-01 2024-02-08 宝山钢铁股份有限公司 Environment-friendly water-based treatment agent for improving phosphatability of high-strength steel

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Application publication date: 20171107