CN110042405A - The preparation method of aqueous low surface clean antirust one-step method treatment fluid - Google Patents
The preparation method of aqueous low surface clean antirust one-step method treatment fluid Download PDFInfo
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- CN110042405A CN110042405A CN201910465894.4A CN201910465894A CN110042405A CN 110042405 A CN110042405 A CN 110042405A CN 201910465894 A CN201910465894 A CN 201910465894A CN 110042405 A CN110042405 A CN 110042405A
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- treatment fluid
- degreaser
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- low surface
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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
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F11/00—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent
-
- 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
- C23G1/08—Iron or steel
- C23G1/088—Iron or steel solutions containing organic acids
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Treatment Of Metals (AREA)
- Preventing Corrosion Or Incrustation Of Metals (AREA)
Abstract
The invention discloses a kind of preparation methods of aqueous low surface clean antirust one-step method treatment fluid, comprising the following steps: and appropriate degreaser is soluble in water, it is stand-by to be configured to the degreaser working solution that concentration is 50g/L;By concentration be 0.8-2.8g/l Butyl Phthalate and concentration be 2.0-10.0g/l citric acid mix and stir and be allowed to dissolve, then the tannic acid that concentration is 0.2-1.2g/l is added and the propylene oxide derivatives stirring that concentration is 1.2-2.8g/l is allowed to dissolve, the fluosilicic acid that concentration is 1.0-6.0ml/l is finally added dropwise, it adds water and stirs uniformly, adjusting pH value is 3-7, and treatment fluid can be obtained.Treatment fluid performance prepared by the present invention is stablized, and operating procedure is simple and environmentally friendly, and the anti-corrosion ability of carbon steel and the adhesive force of coating can be improved to a certain extent, can be used cooperatively with anticorrosive paint.
Description
Technical field
The present invention relates to aqueous low surface metal treatment process technical fields, more particularly, to a kind of aqueous low surface clean
The preparation method of antirust one-step method treatment fluid.
Background technique
The antiseptic projects such as band large-scale metal framework, basin, pipeline, when spary anticorrosive paint, early period, derusting rust-proofing was taken
Conventional method is all inconvenient, and it is dangerous that sanding is also easy to produce spark, and it is again secondary quickly get rusty, take pickling unlikely.So
A kind of safe and environment-friendly, easy constructing operation is researched and developed, the good technique of derusting rust-proofing performance is significant.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of aqueous low surface clean antirust one-step method treatment fluid, preparation
Treatment fluid performance is stablized, and operating procedure is simple and environmental protection, can be improved to a certain extent carbon steel anti-corrosion ability and coating it is attached
Put forth effort, can be used cooperatively with anticorrosive paint.
To achieve the above object, the present invention provides a kind of preparation sides of aqueous low surface clean antirust one-step method treatment fluid
Method, comprising the following steps:
(1) degreaser working solution is configured
Appropriate degreaser is soluble in water, it is stand-by to be configured to the degreaser working solution that concentration is 50g/L;
(2) preparation for the treatment of fluid
By concentration be 0.8-2.8g/l Butyl Phthalate and concentration be 2.0-10.0g/l citric acid mix and stir
It mixes and is allowed to dissolve, the tannic acid that concentration is 0.2-1.2g/l and the propylene oxide derivatives that concentration is 1.2-2.8g/l is then added
Stirring is allowed to dissolve, and the fluosilicic acid that concentration is 1.0-6.0ml/l is finally added dropwise, and adds water and stirs uniformly, and adjusting pH value is 3-7, i.e.,
Treatment fluid can be obtained.
Preferably, the degreaser working solution is LS-206 degreaser.
Preferably, pH value is adjusted by tartaric acid or sodium hydroxide in the step (2).
Preferably, test piece is prepared using above-mentioned treatment fluid, the carbon steel test piece of same size is immersed in 5% LS-
10-15min in 206 degreaser working solutions, is rinsed well after taking-up with tap water, and then test piece is put into above-mentioned treatment fluid
Film forming experiment is carried out, takes out test piece later, is rinsed well with clear water, dries to obtain conversion film.
Therefore, the present invention uses the preparation method of above-mentioned aqueous low surface clean antirust one-step method treatment fluid, the place of preparation
Reason fluidity can be stablized, and operating procedure is simple and environmentally friendly, and the attachment of the anti-corrosion ability and coating of carbon steel can be improved to a certain extent
Power can be used cooperatively with anticorrosive paint.
Below by embodiment, technical scheme of the present invention will be described in further detail.
Detailed description of the invention
Fig. 1 is the open circuit potential curve of film forming procedure;
Fig. 2 is the SEM pattern of chemical composition coating made from optimization process liquid.
Specific embodiment
The present invention provides a kind of preparation methods of aqueous low surface clean antirust one-step method treatment fluid, including following step
It is rapid:
(1) degreaser working solution is configured
Appropriate degreaser is soluble in water, be configured to concentration be 50g/L degreaser working solution it is stand-by, degreaser working solution
For LS-206 degreaser;
(2) preparation for the treatment of fluid
By concentration be 0.8-2.8g/l Butyl Phthalate and concentration be 2.0-10.0g/l citric acid mix and stir
It mixes and is allowed to dissolve, the tannic acid that concentration is 0.2-1.2g/l and the propylene oxide derivatives that concentration is 1.2-2.8g/l is then added
Stirring is allowed to dissolve, and the fluosilicic acid that concentration is 1.0-6.0ml/l is finally added dropwise, adds water and stirs uniformly, passes through tartaric acid or hydrogen-oxygen
Changing sodium to adjust pH value is 3-7, and treatment fluid can be obtained.Test piece is prepared using above-mentioned treatment fluid, the carbon steel iron of same size is tried
Piece is immersed in 10-15min in 5% LS-206 degreaser working solution, is rinsed well after taking-up with tap water, then puts test piece
Enter and carry out film forming experiment into above-mentioned treatment fluid, take out test piece later, rinsed well with clear water, dries to obtain conversion film.To turn
Change film and carry out droplet test, drips detection liquid on the surface of conversion film and carry out drop, while starting stopwatch, observe and record liquid
The time for dripping discoloration, the average value of three points is taken to ensure the reliability of experimental result.Evaluation criterion is: the time of drop discoloration
Longer, the corrosion resistance of conversion film is better.Detect the composition of liquid are as follows: concentration is the CuSO of 41g/L4·5H2O, the NaCl of 35g/L,
HCl (ρ=1.19g/mL) 3ml/L of 0.1mol/L.
Embodiment 1
The measurement of Φ-t curve: take the film forming working solution 250mL prepared by the formula of optimization of orthogonal test in electrolytic cell
In, film forming working solution is by salt bridge and saturated potassium chloride solution connection filled with saturated potassium chloride solution, with saturated calomel electrode
For reference electrode (insertion saturated potassium chloride solution in), through degreaser, treated that test piece (being tailored into 12cm × 1.5cm) is work
Make electrode, connection salt bridge while working electrode is inserted into working solution measures film forming procedure with CH660C electrochemical workstation
Open circuit potential change over time φ-t curve.As shown in Figure 1, electrode potential by initial 0.6346V in 180s rapidly on
0.686V is risen to, film forming incipient stage current potential rises rapidly, this process is the important growth course of film.Steel surface passes through
Chemical action forms the conversion film of one layer of even compact.It is raised slowly to 0.6879V in 300s after 180s, is in later
Relatively steady state, so far conversion film has been formed.With the extension of time, current potential gradually becomes just, illustrate the anti-of conversion film
Erosion ability gradually increases.Current potential increases slowly after 360s, illustrates that the formation of film and the process of falling off reach approximately dynamic equilibrium.
Current potential is basically unchanged after 600s, is tended towards stability, it is believed that conversion film has been formed, so film formation time optimum range is
6min-10min.From the point of view of measuring the φ-t curve that open circuit potential changes over time, the film forming procedure of the research is mainly logical
Cross suction-operated completion.
Embodiment 2
It is the Butyl Phthalate of 1.6g/L, the citric acid of 4g/L, the tannic acid of 0.4g/L and the fluosilicic acid of 4mL/L by concentration
Be added in tap water and mixed, take different amounts of propylene oxide derivatives, respectively 0.2g, 0.3g, 0.4g, 0.5g,
0.6g, 0.7g in above-mentioned mixed liquor, add tap water be diluted to graduation mark propylene oxide derivatives concentration be respectively 0.8g/L,
1.2g/L, 1.6g/L, 2.0g/L, 2.4g/L, 2.8g/L adjust pH to 4 with tartaric acid or sodium hydroxide, and film formation time is
8min carries out cupric sulphate dropping test to processed test piece.As can be seen from the test results, with propylene oxide derivatives plus
Enter the increase of amount, corrosion stability increases therewith, when reaching 1.6g/L, continues growing the amount of propylene oxide derivatives, the corrosion stability of film
It can decline, the optimum range of propylene oxide derivatives concentration is 1.2g/L-2.0g/L.
Embodiment 3
It is the Butyl Phthalate of 1.6g/L, the citric acid of 4g/L, the propylene oxide derivatives of 1.6g/L, 4mL/L by concentration
Fluosilicic acid is added in tap water and is mixed, be then respectively adding concentration be 0.2g/L, 0.4g/L, 0.6g/L, 0.8g/L,
The tannic acid of 1.0g/L, 1.2g/L are mixed, and adjust pH to 4, film formation time 8min, to place with tartaric acid or sodium hydroxide
The test piece managed carries out the experiment of copper sulphate drop.As can be seen from the test results, a large amount of hydroxyl is contained in tannic acid, is being originated
Stage, interface hydrogen ion are reduced, and solution acidity reduces, and increase part [OH-] moment, and [OH-] and tannic acid polyhydroxy H are tied
Closing dehydration makes oxygen in tannic acid form chemisorbed film in conjunction with the surface active matrix [Fe], so the corrosion stability of metal surface increases
By force, when continuing growing with additional amount, the corrosion stability of conversion film reduces instead.This is because tannic acid reaches single layer in metal surface
After saturation absorption, then increase its adsorbance to will lead to the chemisorbed film to be formed loose, corrosion stability reduces, so tannic acid is dense
The optimum range of degree is 0.2g/L-0.6g/L.
Embodiment 4
It is the Butyl Phthalate of 1.6g/L, the citric acid of 4g/L, the tannic acid of 0.4g/L, 1.6g/L propylene oxide by concentration
Derivative is added in tap water and is mixed, and takes different amounts of fluosilicic acid, respectively 0.25mL, 0.50mL, 0.75mL,
1.0mL, 1.25mL, 1.5mL add tap water to be diluted to graduation mark in above-mentioned mixed liquor, and the concentration of fluosilicic acid is respectively
1.0mL/L, 2.0mL/L, 3.0mL/L, 4.0mL/L, 5.0mL/L, 6.0mL/L adjust pH to 4 with tartaric acid or sodium hydroxide,
Film formation time is 8min, carries out the experiment of copper sulphate drop to processed test piece.The mechanism of action of the fluosilicic acid in steel surface are as follows:
H2SiF6+Fe→Fe2++HSiF6-+H2↑ (1)
2HSiF6-+Me2+→MeSiF6↓+H2SiF6 (2)
The effect of reaction (1) is the hydrogen ion for reducing metal surface;The effect of reaction (2) is to generate indissoluble in matrix surface
Object is deposited on metal surface.When a small amount of fluosilicic acid is added, reaction (1) cannot be carried out sufficiently, therefore reaction (2) cannot be sent out
It is raw, cause corrosion stability very poor, with the addition of fluosilicic acid, reacts the degree that (2) carry out and increase, corrosion stability is consequently increased.When
When being added to a certain amount of, inhibit the generation of reaction (2), corrosion stability reduces instead.Therefore the optimum range of fluosilicic acid concentration is
2.0mL/L-4.0mL/L。
Embodiment 5
It is the fluorine of the citric acid of 4g/L, the tannic acid of 0.4g/L, the propylene oxide derivatives of 1.6g/L, 3mL/L by concentration
Silicic acid is added in tap water and is mixed, and takes different amounts of Butyl Phthalate, respectively 0.2g, 0.3g, 0.4g, 0.5g,
0.6g, 0.7g add tap water to be diluted to graduation mark in above-mentioned mixed liquor, and the concentration of Butyl Phthalate is respectively 0.8g/L, 1.2g/
L, 1.6g/L, 2.0g/L, 2.4g/L, 2.8g/L adjust pH to 4 with tartaric acid or sodium hydroxide, film formation time 8min, right
Processed test piece carries out the experiment of copper sulphate drop.With the increase of Butyl Phthalate additional amount, rising is presented in the corrosion stability of film
Trend, but after additional amount increases to 2.0g/L, the corrosion stability of conversion film reduces instead, the short texture of film, so phthalandione fourth
The optimum range of ester concentration is 1.6g/L-2.4g/L.
Embodiment 6
It is propylene oxide derivatives, the 3mL/L of the Butyl Phthalate of 2.0g/L, the tannic acid of 0.4g/L, 1.6g/L by concentration
Fluosilicic acid be added in tap water and mixed, take different amounts of citric acid, respectively 0.5g, 1.0g, 1.5g, 2.0g,
2.5g adds tap water to be diluted to graduation mark in above-mentioned mixed liquor, and the concentration of citric acid is respectively 2g/L, 4g/L, 6g/L, 8g/
L, 10g/L, adjusts pH to 4, film formation time 8min with tartaric acid or sodium hydroxide, carries out copper sulphate point to processed test piece
Drop experiment.When the concentration of citric acid is lower, the corrosion stability of film is lower, and with the increase of its additional amount, the corrosion stability of film is gradually increased,
But additional amount is excessive, corrosion stability decreases, so the optimum range of citric acid concentration is 2g/L-6g/L.
Embodiment 7
It is the epoxy third of the Butyl Phthalate of 2.0g/L, the citric acid of 4g/L, the tannic acid of 0.4g/L, 1.6g/L by concentration
Alkane derivatives, 3mL/L fluosilicic acid be added in tap water and mixed, add tap water to be diluted to graduation mark, with tartaric acid or
Sodium hydroxide adjusts pH, and making pH value of solution is respectively 3,4,5,6,7, film formation time 8min, carries out sulfuric acid to processed test piece
The experiment of copper drop.By preliminary experiment exploration discovery, the stabilization of film forming liquid and the shape of film just can guarantee only under acidic environment
At, when pH is less than 3, reacted with metal erosion based on, in not film-forming state, with the increase of pH, corrosion stability also increases therewith
Add, when pH is greater than 5, inhibit reaction, corrosion stability reduces instead, therefore the optimum range of pH that preliminary experiment obtains is 4-
6。
Embodiment 8
According to a large amount of preliminary experiments, it is changed to each factor design in film liquid and does orthogonal test (L73), each factor level is shown in Table
1, use the copper sulphate drop time as the Quantitative Factors of performance evaluation, orthogonal experiments are shown in Table 2.It is filtered out most according to index K
Good technique are as follows: Butyl Phthalate 1.6g/L, citric acid 6g/L, tannic acid 0.6g/L, glycidic acid derivative 1.6g/L, fluosilicic acid
3mL/L, pH=4, film formation time 8min.Influence sequence of each factor to experimental result is judged according to R value are as follows: fluosilicic acid > lemon
Acid > Butyl Phthalate > pH value > film formation time > glycidic acid derivative > tannic acid.
1 factor level table of table
2 orthogonal experiments of table
Embodiment 9
The specification that the carbon steel test piece made from optimization process liquid is cut into 5 × 5mm is subjected to SEM scanning, as a result such as Fig. 2 institute
Show, iron surface can be observed and generate one layer of uniform amorphous film.
Therefore, the present invention uses the preparation method of above-mentioned aqueous low surface clean antirust one-step method treatment fluid, the place of preparation
Reason fluidity can be stablized, and operating procedure is simple and environmentally friendly, and the attachment of the anti-corrosion ability and coating of carbon steel can be improved to a certain extent
Power can be used cooperatively with anticorrosive paint.
Finally, it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention rather than is limited,
Although the present invention is described in detail with reference to preferred embodiments, those skilled in the art should understand that: its according to
So can be with modification or equivalent replacement of the technical solution of the present invention are made, and these modifications or equivalent replacement cannot also make to repair
Technical solution after changing is detached from the spirit and scope of technical solution of the present invention.
Claims (4)
1. a kind of preparation method of aqueous low surface clean antirust one-step method treatment fluid, which comprises the following steps:
(1) degreaser working solution is configured
Appropriate degreaser is soluble in water, it is stand-by to be configured to the degreaser working solution that concentration is 50g/L;
(2) preparation for the treatment of fluid
By concentration be 0.8-2.8g/l Butyl Phthalate and concentration be 2.0-10.0g/l citric acid mix and stir and make
Dissolution, then be added concentration be 0.2-1.2g/l tannic acid and concentration be 1.2-2.8g/l propylene oxide derivatives stirring
It is allowed to dissolve, the fluosilicic acid that concentration is 1.0-6.0ml/l is finally added dropwise, add water and stir uniformly, adjusting pH value is 3-7, can be obtained
To treatment fluid.
2. the preparation method of aqueous low surface clean antirust one-step method treatment fluid according to claim 1, it is characterised in that:
The degreaser working solution is LS-206 degreaser.
3. the preparation method of aqueous low surface clean antirust one-step method treatment fluid according to claim 2, it is characterised in that:
PH value is adjusted by tartaric acid or sodium hydroxide in the step (2).
4. the preparation method of aqueous low surface clean antirust one-step method treatment fluid according to claim 3, it is characterised in that:
Test piece is prepared using above-mentioned treatment fluid, the carbon steel test piece of same size is immersed in 5% LS-206 degreaser working solution
10-15min is rinsed well after taking-up with tap water, and then test piece is put into above-mentioned treatment fluid and carries out film forming experiment, later
Test piece is taken out, is rinsed well with clear water, dries to obtain conversion film.
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Citations (4)
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CN108060414A (en) * | 2017-12-14 | 2018-05-22 | 马鞍山新徽铝业有限公司 | A kind of aluminium sheet passivating solution |
CN109518174A (en) * | 2019-01-10 | 2019-03-26 | 廊坊师范学院 | The preparation process of coatings for aluminum materials front surface treatment fluid |
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2019
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CN101003769A (en) * | 2006-12-27 | 2007-07-25 | 江苏科技大学 | Water based detergent for oil dirty |
CN103757623A (en) * | 2011-12-31 | 2014-04-30 | 天津三环乐喜新材料有限公司 | Titanate treatment fluid, surface treatment method for permanent magnet material and permanent magnet material |
CN108060414A (en) * | 2017-12-14 | 2018-05-22 | 马鞍山新徽铝业有限公司 | A kind of aluminium sheet passivating solution |
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