CN104451633A - Rust-removing and rust-preventing solution and preparation method thereof - Google Patents

Rust-removing and rust-preventing solution and preparation method thereof Download PDF

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Publication number
CN104451633A
CN104451633A CN201410826031.2A CN201410826031A CN104451633A CN 104451633 A CN104451633 A CN 104451633A CN 201410826031 A CN201410826031 A CN 201410826031A CN 104451633 A CN104451633 A CN 104451633A
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Prior art keywords
rust
consumption
antirusting agent
agent according
solution
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CN201410826031.2A
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CN104451633B (en
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桂成方
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HUNAN JINYU CHEMICAL Co.,Ltd.
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HUNAN JINYU CHEMICAL Co Ltd
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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
    • C23C22/34—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 fluorides or complex fluorides
    • C23C22/36—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 fluorides or complex fluorides containing also phosphates
    • C23C22/364—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 fluorides or complex fluorides containing also phosphates containing also manganese cations
    • 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
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Treatment Of Metals (AREA)
  • Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)

Abstract

The invention provides rust-removing and rust-preventing solution. The rust-removing and rust-preventing solution is characterized in that 1 L of the solution comprises the following raw material components in the following contents: 360-410 g/L of hexafluorozirconic acid, 80-100 g/L of sodium dihydrogen phosphate, 90-130 g/L of ferric nitrate, 1-5 g/L of ethylene glycol, 1-3 g/L of manganese nitrate, 3-5 g/L of octylphenol polyoxyethylene ether, 5-10 g/L of ethylene diamine tetraacetic acid and the balance of water. According to the rust-removing and rust-preventing solution, a unique decomposition transformation synthesis principle is adopted, so the oil removing, rust removing and rust preventing are performed in one step; the solution is directly used in a normal temperature state without heating and special equipment.

Description

Rust-removing and antirusting agent and preparation method thereof
Technical field
The present invention relates to field of metal surface treatment technology, in particular, relate to a kind of rust-removing and antirusting agent and preparation method thereof.
Background technology
Rust-removing and antirusting agent be a kind ofly not only to have eliminated rust, but also antirust premium quality product.At present, hardware antirusting treating method has single stage method and the method for fractional steps, and single stage method and degreasing derusting rust-proofing once complete, and the method for fractional steps and degreasing derusting rust-proofing substep complete.Single stage method changes the loaded down with trivial details operation process of derusting rust-proofing in the past, only needs simple brushing, spray at normal temperatures or soaks, synchronously can complete degreasing derusting rust-proofing.
Chinese patent CN1418920 discloses a kind of metal rust removing and resisting paint and production method thereof, and the formula of this rust-inhibiting paint is: H 3pO 436-41%; Acetic acid 8-10%; FePO 49-13%; Glycerol 0.1-0.5%; Manganous carbonate 0.1-0.2%; Surplus is water.The production method of this rust-inhibiting paint is: I, by miscible in reactor for the water of the phosphoric acid of 38 ∽ 50 parts, 38 ∽ 42 parts, then, add 8 ∽, 10 parts of acetic acid in it.II, after static 0.5 hour, in solution, add 5 ∽, 7 parts of reduced iron powders several times, stir evenly.III, reaction, after 12 hours, add 0.1 ∽, 0.4 part of glycerol and 0.1 ∽, 0.2 part of manganous carbonate wherein, stir evenly, stand-by after static 24 hours.There is following shortcoming in this patent: the tertiary iron phosphate contained in this formula composition and manganous carbonate, completely not soluble in feed liquid, particularly tertiary iron phosphate, easily forms precipitation.
Summary of the invention
An object of the present invention is to overcome the deficiencies in the prior art; a kind of rust-removing and antirusting agent is provided; it has very strong penetrating power; can effectively disintegrate greasy dirt common on metallic surface rapidly; and convert it into the metal protective film that one deck has anti-corrosion performance while corrosion being decomposed, thus reach excellent rust cleaning and rust-proof effect.
Two of object of the present invention is the preparation method providing above-mentioned rust-removing and antirusting agent.
For achieving the above object, the technical solution used in the present invention is as follows:
A kind of rust-removing and antirusting agent, in 1 liter, in described solution, each feed composition and content thereof are:
Fluorine zirconic acid 360-410 g/L, SODIUM PHOSPHATE, MONOBASIC 80-100 g/L, iron nitrate 90-130 g/L, ethylene glycol 1-5 g/L, manganous nitrate 1-3 g/L, Octylphenol polyoxyethylene ether 3-5 g/L, disodium ethylene diamine tetraacetate 5-10 g/L, surplus is water.
The preferred 370-400 g/L of consumption of wherein said fluorine zirconic acid;
The preferred 90-100 g/L of consumption of wherein said SODIUM PHOSPHATE, MONOBASIC;
The preferred 100-120 g/L of consumption of wherein said iron nitrate;
The preferred 2-4 g/L of consumption of wherein said ethylene glycol;
The preferred 1.5-3 g/L of consumption of wherein said manganous nitrate;
The preferred 4-5 g/L of consumption of wherein said Octylphenol polyoxyethylene ether;
The preferred 7-9 g/L of consumption of wherein said disodium ethylene diamine tetraacetate.
The preparation method of rust-removing and antirusting agent of the present invention in turn includes the following steps:
(1) fluorine zirconic acid and water are stirred evenly to miscible in still;
(2) then to adding SODIUM PHOSPHATE, MONOBASIC in it, stirring evenly, leaving standstill 1-2 hour;
(3) in solution, slowly add reduced iron powder (5-9g/L) several times in stirring to stir evenly, leave standstill 10-12 hour;
(4) contamination precipitation in iron powder to be restored goes down, and adds ethylene glycol, iron nitrate and manganous nitrate wherein, then adds Octylphenol polyoxyethylene ether and disodium ethylene diamine tetraacetate, stirs evenly, and leaves standstill stand-by after 20-24 hour.Wherein Octylphenol polyoxyethylene ether and iron nitrate can be accelerated to eliminate rust and film forming speed, and disodium ethylene diamine tetraacetate plays complexing action, the stability of guarantee system.Ethylene glycol is permeate agent, and adding of it can make rust remover enter into rusty scale inside fast, the resistance to corrosion adding the rustproof layer that can improve formation of manganous nitrate.
Main operational principle of the present invention is as follows:
Excessive fluorine zirconic acid can the effect of playing rust, and phosphoric acid salt plays the effect of film forming corrosion protection, and inorganic manganese salt plays electro-chemical protection.
The main component of reduced iron powder is ferric oxide, and in it and solution, fluorine zirconic acid reacts, and reaction formula is as follows:
Fe 2O 3+H 2ZrF 6→Fe 2（ZrF 6） 3+H 2O
The object adding reduced iron powder is, when metallic surface iron rust quantity not sufficient, still can generate enough fluozirconate classes, plays film forming provide protection.
Iron rust can be transformed into stable compound by this product, and the main component of iron rust is ferrous hydroxide, and its reaction formula is:
Fe(OH) 2+H 2ZrF 6→FeZrF 6+H 2O
FeZrF 6be incorporated into steel surface securely, form fine and close protectiveness protective layer, the formation of fluorine zirconic acid manganese salt, improves the resistance to corrosion of protective layer, thus reaches corrosion protection object.
Rust-removing and antirusting agent of the present invention can be directly used to spray workpiece, brush or soak under normal temperature normality.
Beneficial effect of the present invention is: due to the formulating of recipe of uniqueness; rust-removing and antirusting agent has very strong penetrating power; can effectively disintegrate greasy dirt common on metallic surface rapidly; and convert it into the metal protective film that one deck has anti-corrosion performance while corrosion being decomposed, thus reach excellent rust cleaning and rust-proof effect.
Effect after rust-removing and antirusting agent of the present invention uses is as follows:
1, complete function, effect uniqueness.The multiple performance such as this product integrates " oil removing, decontamination, rust cleaning, phosphatization, passivation, antirust "; adopt unique decomposition and inversion composition principle; degreasing derusting rust-proofing one step is completed; its metal-salt protective membrane sticking power formed is I grade; combine well with various paint, meet the requirements of coating standard.
2, nontoxic, Environmental Safety.The toxic acids of deep-etching such as this product is not hydrochloric, sulfuric acid, hydrofluoric acid, and adopt fluorine zirconic acid, make it keep the acid number of safety and stability.
3, simple to operate, easy to use.This product directly uses under normal temperature normality, without the need to adding gentle specific equipment, can adopt the multiple construction technologies such as immersion, brushing, spray, not needing professional.
4, economical, low cost.Use this product greatly can reduce equipment investment and artificial to drop into, make that the process before application is efficient, low consumption, easily.Under general situation, per kilogram can processing area 12m 2~ 20m 2left and right.As adopted soaking technology, every 100 kilograms can add up treat article about two tons.
5, not chloride and heavy metal, Environmental Safety.By SGS certification, meet RoHS command request.
6, this product raw materials cost is low, and water and fluorine zirconic acid account for most of ratio, are all dirt cheap.This product use cost is low, compares existing antirust rust-resisting paint, and the brushing area of this product unit mass is large; The manufacture craft of this product is also fairly simple, does not have particular requirement, and processing is simple, and tooling cost is low.
In the embodiment of the present invention, after Passivation Treatment, neutral salt spray corrosion test (NSS) method of workpiece is: with reference to ISO3768 standard, salt-mist corrosion tester put into by selected workpiece after Passivation Treatment, salt solution is containing 5%(wt) sodium-chlor, pH value 6.5 ~ 7.2, mist amount 1 ~ 2mL/ (hcm, falls in temperature (35 ± 2) DEG C 2), survey corrosion area after 72 hours time, calculate corrosion area and account for the long-pending per-cent of workpiece surface.
After antirust treatment, the natural Rust Test condition of workpiece is: workpiece is arranged vertically on synthetic glass specimen holder, be placed in temperature (25 ± 2) DEG C, in the fixed temperature and humidity closed room of relative humidity (80 ± 5) %, every day observes once, the test number of days of first workpiece generation corrosion is deducted one day as the number of days that becomes rusty on not.
Anti-rust film sticking power grade: the cross cut test standard according to GB 9286-1998 paint and varnish paint film is tested.
Anti-rust film layer porosity: get the NaCL of 14% and the potassium ferricyanide solution of 3%, the massfraction of tensio-active agent is the distilled water solution of 0.1%, to be kept in brown bottle 24 hours, to use filter paper filtering.Filter paper is cut into the scraps of paper that length and width is 2.5 centimetres during use, with plastic tweezer, the scraps of paper are immersed in above-mentioned solution, propose to drip clean unnecessary test solution, he is covered phosphatize phosphate coat surface to be measured, test paper is taken away after (1 minute) through after a while, observe film surface, have blue color spot point place to indicate aperture sections.
Embodiment
Below in conjunction with specific embodiment, further detailed description is done to the present invention.
Embodiment 1-10 sets forth the composition of rust-removing and antirusting agent of the present invention, concrete listed by table 1, table 2, and wherein, the unit of each batching numerical value is g/L, and liquor capacity is 1L.
Table 1 embodiment 1-5 fills a prescription composition
Embodiment 1 2 3 4 5
Fluorine zirconic acid 360 365 370 375 380
SODIUM PHOSPHATE, MONOBASIC 100 95 90 85 80
Iron nitrate 90 95 100 105 110
Ethylene glycol 2 2.5 3 3.5 4
Manganous nitrate 1 1.5 2 1.5 2
Octylphenol polyoxyethylene ether 5 4.5 4 3.5 4
Disodium ethylene diamine tetraacetate 5 9 8 10 7
Water Surplus Surplus Surplus Surplus Surplus
Table 2 embodiment 5-10 fills a prescription composition
Embodiment 6 7 8 9 10
Fluorine zirconic acid 385 390 395 400 410
SODIUM PHOSPHATE, MONOBASIC 90 95 100 95 90
Iron nitrate 115 120 125 130 120
Ethylene glycol 1 1.5 2 3 4
Manganous nitrate 1.5 2 1.5 2.5 3
Octylphenol polyoxyethylene ether 3.5 5 3 5 5
Disodium ethylene diamine tetraacetate 5 6 9 5 8
Water Surplus Surplus Surplus Surplus Surplus
The preparation method of above embodiment is as follows:
(1) by fluorine zirconic acid and water miscible in reactor;
(2, then to adding SODIUM PHOSPHATE, MONOBASIC in it, leave standstill 1 hour;
(3 add reduced iron powder (7g/L) several times in solution stirs evenly, and leaves standstill 12 hours;
(contamination precipitation in 4 iron powders to be restored goes down, and adds ethylene glycol and manganous nitrate and iron nitrate wherein, then adds Octylphenol polyoxyethylene ether and disodium ethylene diamine tetraacetate, stir evenly, and leaves standstill stand-by after 24 hours.
Table 3 is comparative example formula, and the unit of numerical value of wherein respectively preparing burden is g/L, and liquor capacity is 1L.
Table 3 comparative example formula
Comparative example 1 2 3 4 5 6
Fluorine zirconic acid 360 360 365 365 375 390
SODIUM PHOSPHATE, MONOBASIC 100 100 95 95 85 95
Iron nitrate 90 90 95 95 105 120
Ethylene glycol 2 2 2.5 2.5 3.5 1.5
Manganous nitrate 1 1 1.5 1.5 1.5 2
Octylphenol polyoxyethylene ether 10 0 13.5 0 0 0
Disodium ethylene diamine tetraacetate 0 10 0 13.5 0 0
Water Surplus Surplus Surplus Surplus Surplus Surplus
The using method of above embodiment, comparative example is as follows:
Normal temperature normality directly uses rust-removing and antirusting agent of the present invention to spray ferrous metal workpiece.
The result of use of above embodiment, comparative example is respectively in table 4, table 5, table 6.
The result of use of table 4 embodiment 1-5
Embodiment 1 2 3 4 5
Neutral salt spray corrosion test 1h 1h 1h 0.5h 0.5h
Nature Rust Test 10d 9d 9d 10d 10d
Paint film adhesion grade I grade I grade I grade I grade I grade
Rete hole quantity Nothing Nothing Nothing Nothing Nothing
The result of use of table 5 embodiment 5-10
Embodiment 6 7 8 9 10
Neutral salt spray corrosion test 1h 1h 1h 1h 1h
Nature Rust Test 12d 13d 14d 16d 15d
Paint film adhesion grade 0 grade 0 grade 0 grade 0 grade 0 grade
Rete hole quantity Nothing Nothing Nothing Nothing Nothing
The result of use of table 6 comparative example
Comparative example 1 2 3 4 5 6
Neutral salt spray corrosion test 0.5h 0.5h 0.5h 0.5h 0.5h 0.5h
Nature Rust Test 7d 5d 8d 8d 4d 4d
Paint film adhesion 1 grade 1 grade 2 grades 2 grades 2 grades 2 grades
Rete hole quantity Slightly many Slightly many Slightly many Slightly many Many Many
Table 7 comparative example 7-8 result of use
Comparative example 7 8
Phosphoric acid 36% 41%
Acetic acid 8% 10%
Tertiary iron phosphate 9% 13%
Glycerol 0.1% 0.5%
Manganous carbonate 0.1% 0.2%
Water Surplus Surplus
Table 8 comparative example 7-8 result of use
Comparative example 7 8
Neutral salt spray corrosion test 1h 1h
Nature Rust Test 9d 8d
Paint film adhesion 1 grade 1 grade
Rete hole quantity Many Many
Remarks: every best results of embodiment 9; The result of use of comparative example 7 is preferably in comparative example, but relative to embodiment 9, properties all differs greatly.

Claims (9)

1. a rust-removing and antirusting agent, it is characterized in that in 1 liter, in solution, each feed composition and content thereof are: fluorine zirconic acid 360-410 g/L, SODIUM PHOSPHATE, MONOBASIC 80-100 g/L, iron nitrate 90-130 g/L, ethylene glycol 1-5 g/L, manganous nitrate 1-3 g/L, Octylphenol polyoxyethylene ether 3-5 g/L, disodium ethylene diamine tetraacetate 5-10 g/L, surplus is water.
2. rust-removing and antirusting agent according to claim 1, is characterized in that the consumption of described fluorine zirconic acid is 370-400 g/L.
3. rust-removing and antirusting agent according to claim 1, is characterized in that the consumption of described SODIUM PHOSPHATE, MONOBASIC is 90-100 g/L.
4. rust-removing and antirusting agent according to claim 1, is characterized in that the consumption of described iron nitrate is 100-120 g/L.
5. rust-removing and antirusting agent according to claim 1, is characterized in that the consumption of described ethylene glycol is 2-4 g/L.
6. rust-removing and antirusting agent according to claim 1, is characterized in that the consumption of described manganous nitrate is 1.5-3 g/L.
7. rust-removing and antirusting agent according to claim 1, is characterized in that the consumption of described Octylphenol polyoxyethylene ether is 4-5 g/L.
8. rust-removing and antirusting agent according to claim 1, is characterized in that the consumption of described disodium ethylene diamine tetraacetate is 7-9 g/L.
9. the preparation method of rust-removing and antirusting agent according to claim 1, is characterized in that in turn including the following steps:
(1) fluorine zirconic acid and water are stirred evenly to miscible in still;
(2) then to adding SODIUM PHOSPHATE, MONOBASIC in it, stirring evenly, leaving standstill 1-2 hour;
(3) in solution, slowly add reduced iron powder (5-9g/L) several times in stirring to stir evenly, leave standstill 10-12 hour;
(4) contamination precipitation in iron powder to be restored goes down, and adds ethylene glycol, iron nitrate and manganous nitrate wherein, then adds Octylphenol polyoxyethylene ether and disodium ethylene diamine tetraacetate, stirs evenly, and leaves standstill 20-24 hour.
CN201410826031.2A 2014-12-26 2014-12-26 Rust-removing and rust-preventing solution and preparation method thereof Active CN104451633B (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105755478A (en) * 2016-03-08 2016-07-13 湖南金裕环保科技有限公司 Preparation method of rust remover capable of fast removing oxide layer on surface of metal under normal temperature
CN106702365A (en) * 2016-04-24 2017-05-24 佛山瑞箭体育器材有限公司 Rust prevention solution and preparation method thereof
WO2018104796A1 (en) * 2016-12-01 2018-06-14 Win Chemicals, Ltd. Fluorinated acid compounds, compositions and methods of use
CN109112554A (en) * 2018-10-31 2019-01-01 三达奥克化学股份有限公司 Aluminum alloy pattern plate cement slurry efficient cleaner for building and preparation method thereof
CN112759991A (en) * 2020-12-29 2021-05-07 上海承一化学科技有限公司 Water-based non-phosphatized primer and preparation method thereof

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CN103374715A (en) * 2012-04-27 2013-10-30 中国钢铁股份有限公司 Aqueous metal surface treatment agent and metal surface treatment method using same

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105755478A (en) * 2016-03-08 2016-07-13 湖南金裕环保科技有限公司 Preparation method of rust remover capable of fast removing oxide layer on surface of metal under normal temperature
CN106702365A (en) * 2016-04-24 2017-05-24 佛山瑞箭体育器材有限公司 Rust prevention solution and preparation method thereof
WO2018104796A1 (en) * 2016-12-01 2018-06-14 Win Chemicals, Ltd. Fluorinated acid compounds, compositions and methods of use
US10280521B2 (en) 2016-12-01 2019-05-07 Win Chemicals, Ltd. Fluorinated acid compounds, compositions and methods of use
CN109112554A (en) * 2018-10-31 2019-01-01 三达奥克化学股份有限公司 Aluminum alloy pattern plate cement slurry efficient cleaner for building and preparation method thereof
CN112759991A (en) * 2020-12-29 2021-05-07 上海承一化学科技有限公司 Water-based non-phosphatized primer and preparation method thereof

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