CN110042384A - A kind of steel iron phosphatising film confining liquid and preparation method thereof and application method - Google Patents

A kind of steel iron phosphatising film confining liquid and preparation method thereof and application method Download PDF

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Publication number
CN110042384A
CN110042384A CN201910313403.4A CN201910313403A CN110042384A CN 110042384 A CN110042384 A CN 110042384A CN 201910313403 A CN201910313403 A CN 201910313403A CN 110042384 A CN110042384 A CN 110042384A
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CN
China
Prior art keywords
confining liquid
film
steel iron
iron phosphatising
phosphatising
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Pending
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CN201910313403.4A
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Chinese (zh)
Inventor
胡秀英
胡贵芳
江鑫慧
姚鹏飞
傅建
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Jiangsu University of Technology
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Jiangsu University of Technology
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Priority to CN201910313403.4A priority Critical patent/CN110042384A/en
Publication of CN110042384A publication Critical patent/CN110042384A/en
Pending legal-status Critical Current

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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
    • C23C22/82After-treatment
    • C23C22/83Chemical after-treatment

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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 belongs to steel surface processing technology fields, more particularly to a kind of steel iron phosphatising film confining liquid and preparation method thereof and application method, the formula of the confining liquid is to contain sodium metasilicate 9-21g, thiocarbamide 2-5g, phytic acid 2-5ml, sodium molybdate 2-4g in every liter of confining liquid, and surplus is water.The present invention carries out Seal treatment using Chrome-free confining liquid, avoids murder by poisoning of the chromium to environment and human body, and the phosphating coat confining bed of formation has good corrosion resistance.

Description

A kind of steel iron phosphatising film confining liquid and preparation method thereof and application method
Technical field
The invention belongs to steel surface processing technology fields, and in particular to a kind of steel iron phosphatising film confining liquid and its preparation side Method and application method.
Background technique
Steel is the widest structural material of modern Application.In order to which the corrosion of oxygen and water in atmosphere can be born, lead to Phosphorating treatment often is carried out to steel material surface and forms phosphating coat, but phosphating coat there are many gaps, corrosion resistance is poor.To improve The corrosion resistance of phosphating coat, is usually further continued for being passivated after phosphatization or Seal treatment.The passivation that traditional Passivation Treatment uses Containing hypertoxic carcinogenic substance Cr VI in liquid, the waste liquid that Passivation Treatment generates in the process is very big to environmental hazard.Therefore a kind of steel is found Iron phosphating coat Chrome-free confining liquid has important practical significance.
Corrosion proof passivation or seal treatment technique are improved there are still certain defect currently used for steel iron phosphatising film, are needed It is further improved.A kind of high-efficiency environment friendly compound closure agent is disclosed in Chinese invention patent application CN106085218A, the compound envelope Agent is closed by methyl silicon resin, alkyd resin, alumina sol, redox graphene, catalyst, film forming agent, lubricant, promotion Agent, metal inhibitor, surfactant, silane coupling agent, low-carbon alcohol and water composition, the formula components are complicated, increase production Cost is unsuitable for industrialization promotion.A kind of metal rust-removing anti-rust envelope is disclosed in Chinese invention patent application CN107142484A Agent and preparation method are closed, includes phosphoric acid, aluminium powder, complexing agent, tartaric acid, zinc dihydrogen phosphate, dodecyl in the sealant components Benzene sulfonic acid sodium salt, potassium bichromate part, nickel nitrate contain Cr VI in the component of the patent of invention, seriously endanger environment.
Summary of the invention
Invention broadly provides a kind of steel iron phosphatising film confining liquid and preparation method thereof and application methods, are sealed using Chrome-free It closes liquid and carries out Seal treatment, avoid murder by poisoning of the chromium to environment and human body, the phosphating coat confining bed of formation has good corrosion-resistant Property.Its technical solution is as follows:
A kind of steel iron phosphatising film confining liquid, in every liter of confining liquid containing sodium metasilicate 9-21g, thiocarbamide 2-5g, phytic acid 2-5ml, Sodium molybdate 2-4g, surplus are water.
Preferably, remaining containing sodium metasilicate 14-18g, thiocarbamide 3-4g, phytic acid 3-4ml, sodium molybdate 3-4g in every liter of confining liquid Amount is water.
Preferably, the pH of the confining liquid is 8-11.
Preferably, the water is deionized water.
The preparation method of above-mentioned steel iron phosphatising film confining liquid be specifically the sodium metasilicate for taking formula ratio, thiocarbamide, phytic acid, Sodium molybdate is soluble in water, is configured to mixed solution, adjusts the pH to 8-11 of mixed solution, obtains confining liquid.
The application method of above-mentioned steel iron phosphatising film confining liquid is specifically, to steel iron phosphatising film when the confining liquid uses Seal treatment temperature is 70-80 DEG C, close process time 10-15min.
Preferably, after the completion of confining liquid use, steel iron phosphatising film surface is cleaned using deionized water, and with 70-75 DEG C Heated-air drying.
Using the above scheme, the invention has the following advantages that
Confining liquid prepared by the present invention does not contain chromium, avoids chromium to the murder by poisoning problem of environment and human body, the feature of environmental protection is good.Envelope It is simple to close liquid component, " locked in " operation method is convenient, and sealing effect is good, closes film layer even compact, the corrosion resistance after closing Higher than traditional cbromate seal, there is good application value.
Detailed description of the invention
Fig. 1 is the SEM figure of steel iron phosphatising film before closing;
Fig. 2 is the SEM figure of the steel iron phosphatising film after the confining liquid Seal treatment in embodiment 1.
Specific embodiment
Experimental method in following embodiment is conventional method unless otherwise required, related experiment reagent and material Material is conventional biochemical reagent and material unless otherwise required.
Embodiment 1
The steel iron phosphatising film of the present embodiment closes liquid making method are as follows:
Sodium metasilicate 12g, thiocarbamide 2g, phytic acid 3ml, sodium molybdate 4g are taken, is dissolved in deionized water, the mixing for being configured to 1L is molten Liquid adjusts the pH value of mixed solution to 8.5, obtains confining liquid.
The temperature of steel iron phosphatising film Seal treatment in above-mentioned confining liquid is 70 DEG C, off-period 15min, and closing is completed Afterwards, steel iron phosphatising film surface is cleaned using deionized water, and with 70 DEG C of heated-air dryings.
The closing film layer copper sulphate drop time reaches 647s, and NaCl solution soaking time reaches 18h.
Embodiment 2
The steel iron phosphatising film of the present embodiment closes liquid making method are as follows:
Sodium metasilicate 16g, thiocarbamide 3g, phytic acid 3ml, sodium molybdate 4g are taken, is dissolved in deionized water, the mixing for being configured to 1L is molten Liquid adjusts the pH value of mixed solution to 9.0, obtains confining liquid.
The temperature of steel iron phosphatising film Seal treatment in above-mentioned confining liquid is 75 DEG C, off-period 10min, and closing is completed Afterwards, steel iron phosphatising film surface is cleaned using deionized water, and with 75 DEG C of heated-air dryings.
The closing film layer copper sulphate drop time reaches 720s, and NaCl solution soaking time reaches for 24 hours.
Embodiment 3
The steel iron phosphatising film of the present embodiment closes liquid making method are as follows:
Sodium metasilicate 20g, thiocarbamide 5g, phytic acid 2ml, sodium molybdate 3g are taken, is dissolved in deionized water, the mixing for being configured to 1L is molten Liquid adjusts the pH value of mixed solution to 10.0, obtains confining liquid.
The temperature of steel iron phosphatising film Seal treatment in above-mentioned confining liquid is 80 DEG C, off-period 12min, and closing is completed Afterwards, steel iron phosphatising film surface is cleaned using deionized water, and with 75 DEG C of heated-air dryings.
The closing film layer copper sulphate drop time reaches 673s, and NaCl solution soaking time reaches 20h.
Comparative experiments 1
The closing membranous layer corrosion resistance of existing confining liquid and the preparation of 2 confining liquid of the embodiment of the present invention is compared, as a result such as 1 institute of table Show.
The comparison of 1 confining liquid corrosion resistance of table
Closing membranous layer corrosion resistance is measured using copper sulphate drop experimental method.From the data result in table it is found that using this hair Bright confining liquid can obtain the high phosphatization close membrane of corrosion resistance, when phosphatization made from confining liquid of the invention closes film layer drop Between much larger than the closing film layer of phosphatization obtained by existing confining liquid the drop time.
Comparative experiments 2
Two pieces of identical steel test pieces are taken, after being handled using identical pretreatment mode, are put into phosphating solution, in phosphorus Change phosphatization under temperature 60 C and phosphating time 15min, dried up after washing, obtains the steel test piece that surface has phosphating coat.Phosphating solution Formula are as follows: Mazhev salt 60g/L, nickel nitrate 35g/L, sodium chlorate 6g/L, citric acid 1g/L, zinc nitrate 35g/L, manganese nitrate 15g/L, neopelex 0.4g/L.
One of steel test piece with phosphating coat is taken to be not processed, the SEM figure such as Fig. 1 of surface steel iron phosphatising film layer It is shown.Another piece is put into the confining liquid of the preparation of embodiment 1, and the SEM figure of surface steel iron phosphatising film layer is as shown in Figure 2.
By Fig. 1 and Fig. 2 comparison it is found that unclosed phosphating coat is in thin dendroid, surface covering is more complete, but phosphorization membrane There are still small pores for intercrystalline.Phosphating coat after closing, surface are deposited with layer silicate precipitating, enclose phosphatization film surface Micropore further increase the corrosion resistance of phosphating coat to reduce the hole of phosphating coat.
It will be apparent to those skilled in the art that can make various other according to the above description of the technical scheme and ideas Corresponding change and deformation, and all these changes and deformation all should belong to the protection scope of the claims in the present invention Within.

Claims (7)

1. a kind of steel iron phosphatising film confining liquid, it is characterised in that: contain sodium metasilicate 9-21g, thiocarbamide 2-5g, plant in every liter of confining liquid Sour 2-5ml, sodium molybdate 2-4g, surplus are water.
2. steel iron phosphatising film confining liquid according to claim 1, it is characterised in that: contain sodium metasilicate in every liter of confining liquid 14-18g, thiocarbamide 3-4g, phytic acid 3-4ml, sodium molybdate 3-4g, surplus are water.
3. steel iron phosphatising film confining liquid according to claim 1, it is characterised in that: the pH of the confining liquid is 8-11.
4. steel iron phosphatising film confining liquid according to claim 1, it is characterised in that: the water is deionized water.
5. a kind of preparation method of steel iron phosphatising film confining liquid described in claim 1, it is characterised in that: be specifically to take and match Sodium metasilicate, thiocarbamide, phytic acid, the sodium molybdate just measured are soluble in water, are configured to mixed solution, adjust the pH to 8-11 of mixed solution, Obtain confining liquid.
6. a kind of application method of steel iron phosphatising film confining liquid described in claim 1, it is characterised in that: the confining liquid uses When be 70-80 DEG C to the Seal treatment temperature of steel iron phosphatising film, close process time 10-15min.
7. the application method of steel iron phosphatising film confining liquid according to claim 6, it is characterised in that: confining liquid uses completion Afterwards, steel iron phosphatising film surface is cleaned using deionized water, and with 70-75 DEG C of heated-air drying.
CN201910313403.4A 2019-04-18 2019-04-18 A kind of steel iron phosphatising film confining liquid and preparation method thereof and application method Pending CN110042384A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103255462A (en) * 2013-04-17 2013-08-21 佛山科学技术学院 Environment-friendly hole sealing liquid for anodic aluminum oxide profiles and hole sealing method thereof
CN103469196A (en) * 2013-08-26 2013-12-25 重庆建设工业(集团)有限责任公司 Phosphatization film sealing fluid and sealing technology
CN105779982A (en) * 2016-05-17 2016-07-20 广东海洋大学 Chrome-free metal surface conversion liquid and conversion coating preparation method
CN108179409A (en) * 2017-12-26 2018-06-19 廊坊京磁精密材料有限公司 The phosphatization antirust method of neodymium iron boron magnetic body

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103255462A (en) * 2013-04-17 2013-08-21 佛山科学技术学院 Environment-friendly hole sealing liquid for anodic aluminum oxide profiles and hole sealing method thereof
CN103469196A (en) * 2013-08-26 2013-12-25 重庆建设工业(集团)有限责任公司 Phosphatization film sealing fluid and sealing technology
CN105779982A (en) * 2016-05-17 2016-07-20 广东海洋大学 Chrome-free metal surface conversion liquid and conversion coating preparation method
CN108179409A (en) * 2017-12-26 2018-06-19 廊坊京磁精密材料有限公司 The phosphatization antirust method of neodymium iron boron magnetic body

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
于锦等: "《电镀实际操作手册》", 31 October 2007, 辽宁科学技术出版社 *
安成强等: "锌锰系磷化膜硅酸钠封闭工艺研究", 《表面技术》 *
文斯雄: "中温锰系抗蚀黑色磷化工艺", 《电镀与环保》 *

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Application publication date: 20190723

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