CN109055946A - Carbon steel and low-alloy steel cut surface oxide layer pickling solution and acid washing method - Google Patents
Carbon steel and low-alloy steel cut surface oxide layer pickling solution and acid washing method Download PDFInfo
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- CN109055946A CN109055946A CN201811132904.4A CN201811132904A CN109055946A CN 109055946 A CN109055946 A CN 109055946A CN 201811132904 A CN201811132904 A CN 201811132904A CN 109055946 A CN109055946 A CN 109055946A
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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
- 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
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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
- 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
- C23G1/04—Cleaning or pickling metallic material with solutions or molten salts with acid solutions using inhibitors
- C23G1/06—Cleaning or pickling metallic material with solutions or molten salts with acid solutions using inhibitors organic inhibitors
- C23G1/061—Cleaning or pickling metallic material with solutions or molten salts with acid solutions using inhibitors organic inhibitors nitrogen-containing compounds
Abstract
The present invention relates to field of metal surface treatment technology more particularly to a kind of carbon steel and low-alloy steel cut surface oxide layer pickling solution and acid washing method.Specifically, the pickling solution is made of dilute hydrochloric acid and hexamethylenetetramine.Specifically, the acid washing method is the following steps are included: sample is put into the pickling solution of heat by (1), constant temperature impregnates；(2) it is washed and is dried after taking out sample；(3) after dry, using ethyl alcohol cleaning sample and drying.Using pickling solution and acid washing method of the invention, sample preparation process can simplify, realize that disposable sample preparation can measure oxygen, nitrogen content simultaneously.
Description
Technical field
The present invention relates to field of metal surface treatment technology more particularly to a kind of carbon steel and low-alloy steel cut surface to aoxidize
Layer pickling solution and acid washing method.
Background technique
The continuous advancement that manufacturing industry pushes clean steel to produce the continuous improvement of metallurgical material performance requirement, clean steel are raw
The important feature produced is exactly strict control oxygen content in production.The smelting process of certain low-alloy steel requires nitrogen content to answer
Strict control in a certain range, to guarantee suitable Al/N ratio.This requires being capable of quick, Accurate Determining steel in smelting process
The oxygen and nitrogen content of middle trace.
Common and reliable oxygen, Miniature coulomb titrimeter for measuring nitrogen content are PULSE HEATING inert gas fusion-infrared absorption (thermal conductivities
Method), sample is disposably weighed using oxygen-nitrogen analyzer can detect two kinds of oxygen, nitrogen elements simultaneously.Wherein, when measuring nitrogen content, grain
Shape sample and clastic sample；And when measuring oxygen content, it is desirable that sample to be tested is necessary for that specific surface area is small, surface is without dirt
It contaminates, metallic matrix is exposed and the granulated samples of smooth pieces.At present in production inspection, technical staff is by bulk sample
A part preparation granulated samples (for measuring oxygen content), another part using drilling machine drilling cuttings preparation clastic sample (be used for
Nitrogen analysis).During preparing particulate samples, since high-speed cutting, grinding make sample surfaces form thicker oxidation
Layer and deeper mechanical scratch, are unable to satisfy requirement of the analysis method to granulated samples surface roughness and cleanliness.Therefore it needs
The oxide layer of sample surfaces is removed using pickling solution.
Currently, iron rust or oxide skin of the existing pickling solution mainly for cleaning steel surface, and to steel sample after cleaning
Product Surface Oxygen, nitrogen remaining situation and surface roughness are without particular/special requirement.And iron rust and oxide skin are often thicker, need acid
Property and dissolubility stronger solution removal, for herein when easily cause excessive erosion, be unable to satisfy oxygen-nitrogen analyzer to sample light
The requirement of cleanliness.It when selecting acid relatively weak pickling solution to handle cut surface oxide layer or will increase pickling time,
The processing of cut surface oxide layer is not clean, to can not meet the requirement of steel-making both analysis nitrogen, oxygen content.In addition,
Existing pickling solution complicated component, in addition to containing there are many other than inorganic acid, other chemical substances also containing there are many, such as acid mist inhibit
Agent, emulsifier, the rust remover that deoils, buffer etc. are unfavorable for the cleaning removal of sample surfaces trace oxygen, nitrogen after pickling, together
When, the production cost of pickling solution is not only increased, environmental protection and the requirement of Green Chemistry are had not been met.
Thus, it would be highly desirable to research and develop a kind of suitable pickling solution, and design corresponding acid cleaning process, not only may be implemented sample
Surface oxide layer removes clean target, moreover it is possible to guarantee that once purged sample surfaces are remained without any oxygen-containing, nitrogen substance, it is full
Sufficient oxygen, nitrogen content while testing requirements.
Summary of the invention
The purpose of the present invention is in view of the drawbacks of the prior art, provide a kind of carbon steel and the oxidation of low-alloy steel cut surface
Layer pickling solution and acid washing method.
Specifically, on the one hand, described the present invention provides a kind of carbon steel and low-alloy steel cut surface oxide layer pickling solution
Pickling solution is made of dilute hydrochloric acid and hexamethylenetetramine.
Above-mentioned pickling solution, the concentration of the dilute hydrochloric acid are 1.2-2.4mol/L.
Above-mentioned pickling solution, the concentration of the dilute hydrochloric acid are 1.2-1.8mol/L.
Above-mentioned pickling solution, mass concentration of the hexamethylenetetramine in pickling solution are 0.5%-3%.
Above-mentioned pickling solution, mass concentration of the hexamethylenetetramine in pickling solution are 0.8%-1.2%.
On the other hand, the present invention provides a kind of carbon steel and low-alloy steel cut surface oxide layer acid washing method, including with
Lower step:
(1) sample is put into the pickling solution of heat, constant temperature impregnates；
(2) it is washed and is dried after taking out sample；
(3) after dry, using ethyl alcohol cleaning sample and drying.
Above-mentioned acid washing method, the sample are the carbon steel and/or low-alloy steel that carbon content is less than or equal to 0.70%.
Above-mentioned acid washing method, the step (1) are to be put into sample in 70 ± 5 DEG C of pickling solution, impregnate 3-6min.
Above-mentioned acid washing method, the step (2) are to adopt 5 times wash with distilled water after taking out sample, and blown with hair dryer
It is dry.
Above-mentioned acid washing method using washes of absolute alcohol sample 2 times, and uses hair dryer after the step (3) is dry
Drying.
Technical solution of the present invention have it is following the utility model has the advantages that
1. using pickling solution and acid washing method of the invention, it can simplify sample preparation process, realize disposable sample preparation just
Oxygen, nitrogen content can be measured simultaneously.The sample survey period is effectively shortened, smelting iron and steel production process oxygen, nitrogen content are realized
Control advances the improvement of clean steel smelting process, improves steel product quality and economic benefit.
2. pickling solution and acid washing method of the invention realize the oxide layer that quickly removal is generated due to cutting, make sample
Any surface finish, and without oxygen-containing, nitrogen substance is remaining, meet GB/T11261-2006, GB/T20124-2006 analysis method to sample
The requirement (Ra >=1.6 μm) of product.
3. pickling solution and acid washing method of the invention, pickling is high-efficient, in a short period of time can produce machining
Raw oxide layer cleans up, and whole programs only need 6-8 minutes, and sample surfaces are residual without oxygen carrier and nitrogen substance after pickling
It stays, can satisfy the requirement of steel-making both analysis nitrogen and trace oxygen content.
4. pickling solution and acid washing method of the invention, the equipment used in acid cleaning process is simple, and operating process is easy, and
And pickling solution can repeatedly use, and have the advantages that inexpensive, environmentally friendly.
Specific embodiment
In order to fully understand the purpose of the present invention, feature and effect, by following specific embodiments, the present invention is made detailed
It describes in detail bright.For process of the invention in addition to following the description, remaining is all made of the conventional method or device of this field.Following nouns
Term is unless otherwise stated, all have the normally understood meaning of those skilled in the art.
Specifically, according to an aspect of the present invention, the present invention provides a kind of carbon steel and low-alloy steel cut surface to aoxidize
Layer pickling solution, wherein the pickling solution is made of dilute hydrochloric acid and hexamethylenetetramine.
Wherein, pickling solution of the invention passes through certain volume, certain density diluted hydrochloric acid dissolution and dilution certain mass
After hexamethylenetetramine solid, it is uniformly mixed and forms.
Wherein, dilute hydrochloric acid is used to dissolve the oxide layer of granulated samples cutting surfaces.Hexamethylenetetramine can as corrosion inhibiter
Metal surface forms film to prevent excessive erosion after pickling, improves sample surfaces finish after pickling；Due to six methines four
Aqueous amine dissolubility is extremely strong, and after sample leaves pickling solution, washing with water can be easy to get rid of, and eliminates the shadow detected to subsequent nitrogen content
It rings.
In cutting sample, the oxidated layer thickness that cutting surfaces are formed is uneven, therefore, corrosion inhibiter need to be added in hydrochloric acid.
Specific to having multiple amidos for hexamethylenetetramine corrosion inhibiter, it is attached to the newborn matrix surface of sample, prevents base
Body continues to corrode, and promotes pickling solution to remove the continued dissolution of remaining oxide layer, obtains the bright and clean sample of cutting surfaces, meets
To the requirement of sample surfaces finish when test sample oxygen, nitrogen content.Without adding other chemicals in pickling solution of the invention
Matter, it is only necessary to after hydrochloric acid and hexamethylenetetramine are prepared mixing according to the set concentration of the present invention, existing pickling solution can be reached
Inaccessiable pickling effect.
Wherein, in some preferred embodiments, the concentration of the dilute hydrochloric acid is 1.2-2.4mol/L, preferably 1.2-
1.8mol/L。
It, need to be to pickling in order to shorten the round of visits of sample when using pickling solution cleaning sample cutting surfaces oxide layer
Liquid is heated (70 ± 5 DEG C).When the concentration of hydrochloric acid in pickling solution is less than 1.2mol/L, in order to reach ideal pickling effect
Fruit need to further increase the temperature of pickling solution.However, the volatilization of pickling solution will be promoted when the temperature of pickling solution is higher than 75 DEG C,
To be unfavorable for the stabilization of each component content in pickling solution, and a large amount of volatilizations of pickling solution also will lead to environmental pollution.Work as acid
When the concentration of dilute hydrochloric acid is greater than 2.4mol/L in washing lotion, pickling solution is strong to the dissolubility of matrix, and the slow release effect of corrosion inhibiter reduces
It is be easy to cause the excessive corrosion to sample cutting surfaces new life matrix, forms a large amount of grooves to influence the light of sample cutting surfaces
Cleanliness.The concentration of dilute hydrochloric acid in pickling solution of the present invention is set as 1.2-2.4mol/L, can not only guarantee the effect of pickling, also
Pickling time can be shortened, guarantee the quality stability of pickling solution, when the concentration of dilute hydrochloric acid is 1.2-1.8mol/L, pickling solution
Pickling effect and the stability of pickling solution reach best.
Wherein, in some preferred embodiments, the mass concentration of the hexamethylenetetramine is 0.5%-3%, excellent
It is selected as 0.8%-1.0%.
Wherein, the mass concentration of the hexamethylenetetramine is the concentration that hexamethylenetetramine accounts for pickling solution gross mass.
Specifically, hexamethylenetetramine can form film to prevent excessive erosion in metal surface after pickling, surface light is improved
Cleanliness.Through experimental results demonstrate cannot reach when the mass concentration of hexamethylenetetramine is less than 0.5% or is greater than 3%
Ideal corrosion mitigating effect.When the mass concentration of hexamethylenetetramine is 0.8%-1.0%, corrosion mitigating effect reaches best.
According to another aspect of the present invention, the present invention also provides a kind of carbon steel and low-alloy steel cut surface oxide layer acid
Washing method, specifically includes the following steps:
(1) sample is put into the pickling solution of heat, constant temperature impregnates；
Specifically, in some preferred embodiments, sample is put into 70 ± 5 DEG C of pickling solution, 3-6min is impregnated.
Wherein, the time that sample impregnates in acid solution changes according to the difference of steel grade and the difference of oxidated layer thickness.Through
Test proves that sample impregnates 3-5 minutes in pickling solution just can achieve ideal acid to the carbon steel and low-alloy steel
Effect is washed, without further being detected to its pickling effect again.
Iron oxide (the main component FeO+Fe of blue will be generated in sample cutting process on cut surface2O3), pickling solution
Middle hydrochloric acid can react (FeO+2HCl=FeCl with FeO2+H2O) keep oxide layer loose, and then hydrochloric acid penetration to matrix aoxidizes
Reduction reaction (Fe+HCl=FeCl2+H2↑) cause oxide layer stripping.Wherein, pickling temperature is maintained at 70 DEG C ± 5 DEG C, Ke Yijia
Speed reaction is gone on smoothly.
(2) it is washed and is dried after taking out sample；
Specifically, in some preferred embodiments, being adopted 5 times wash with distilled water after taking out sample, and use hair dryer
Drying.
(3) ethyl alcohol cleaning sample and drying are used after drying.
Specifically, in some preferred embodiments, used washes of absolute alcohol sample 2 times after distilling washing and drying,
And it is dried up with hair dryer.
Wherein, ethyl alcohol is miscible with water very competent, and has stronger volatility and environment-protecting and non-poisonous characteristic, relies on
The carrying of ethyl alcohol, volatilization, it is dry after sample through washes of absolute alcohol twice after, hair dryer is dried again, can remove
The moisture of remaining extremely trace.
Specifically, sample selected in a kind of carbon steel of the invention and low-alloy steel cut surface oxide layer acid washing method
For surface without visible physical imperfection (such as crackle is mingled with, shrinkage cavity) and non-excessive oxidation particle (it is non-instant cutting generate,
Outmoded oxide skin).
Specifically, in one preferred embodiment, carbon steel of the invention and low-alloy steel cut surface oxide layer acid
Washing method the following steps are included:
(1) surface is put into 70 ± 5 DEG C of pickling solution without the granulated samples of visible physical imperfection and non-excessive oxidation, is soaked
Steep 5min；
(2) it is adopted 5 times wash with distilled water after taking out sample, and dries 1.5min with Hairdryer；
(3) it uses washes of absolute alcohol sample 2 times, and dries 0.5min with Hairdryer.
Of the invention a kind of carbon steel and low-alloy steel cut surface oxide layer acid washing method, pass through pickling → washing → drying
→ ethyl alcohol washes → the acid cleaning process flow processing of re-dry through the particulate samples of cutting preparation, can obtain meeting oxygen, nitrogen standard scores
The bright and clean sample that analysis method requires, surface are remained without oxygen-containing, nitrogen substance.Sample after cleaning can be used for survey while oxygen, nitrogen
Fixed, that is, two constituent contents can be detected simultaneously by weighing a sample, do not needed to prepare respectively, be surface-treated for measuring two
The sample of element.
Wherein, carbon steel of the invention and low-alloy steel cut surface oxide layer pickling solution and acid washing method, can be used for cleaning
Including carbon content be less than or equal to 0.70% or less all trades mark carbon steel and/or low-alloy steel, such as: construction(al)steel, air bottle steel,
Structural steel, part mould steel and all kinds of wheels, axle steel sample.Sample after pickling solution of the present invention and acid cleaning process cleaning
Product, it is ensured that detection accuracy is good when oxygen content is down to 0.0005%, nitrogen content down to 0.002%.
The present invention within specified temperatures, by the reproducibility of acid, gets rid of the oxide layer of sample cutting surfaces, adds simultaneously
The good organic additive of adding water soluble is configured to the pickling solution of suitable proportion and concentration using its corrosion inhibition.Through the solution
Cleaning, sample surfaces oxide layer remove rapidly, dissolves, and keeps steel sample matrix exposed, and sample surfaces are bright and clean after ensuring cleaning.Acid
After washing, the pickling solution adhered to using a small amount of, multiple distilled water cleaning sample surface, hair dryer is dry, removes sample surfaces
Large quantity of moisture.Then, extremely strong using ethyl alcohol property miscible with water, and there is stronger volatility and environment-protecting and non-poisonous characteristic,
Sample after drying through washes of absolute alcohol twice after, hair dryer is dried again, carrying, volatilization by ethyl alcohol, removal
Fall the moisture of remaining extremely trace.Invention achieves sample surfaces without the remaining purpose of oxygen-containing, nitrogen substance, is quasi- simultaneously
Really, trace oxygen in carbon steel and/or low-alloy steel is quickly measured, nitrogen provides clean particulate samples.
Embodiment
The present invention is further illustrated below by the mode of embodiment, but does not therefore limit the present invention to the reality
It applies among a range.In the following examples, the experimental methods for specific conditions are not specified, according to conventional methods and conditions.Following implementation
Raw material used in example is that regular market purchase obtains.
Granulated samples of sum of the surface without visible physical imperfection without excessive oxidation processed are chosen, wherein the quality of sample
About 0.6g, sample steel grade are S355NL.It is put into the pickling solution of 20ml heat, constant temperature impregnates.Sample is clamped with tweezers, according to
Secondary put into the 50ml small beaker that 5 fill distilled water is cleaned 5 times, the dry about 1.5min of Hairdryer.By dry sample
Continuous immerse in the tool lid bottle that two fill dehydrated alcohol is cleaned, and is washed and is covered lid immediately, prevents water and sundries in air
Pollution to ethyl alcohol, the dry 0.5min of Hairdryer, obtains clean granulated samples to be detected.Wherein, sour in each embodiment
Washing lotion constituent content, see Table 1 for details for acid cleaning process parameter.
The pickling solution component content and pickling parameter of 1 embodiment 1-5 of table
| Hydrochloric acid (mol/L) | Hexamethylenetetramine (%) | Pickling time (min) | Pickling temperature (DEG C) | |
| Embodiment 1 | 1.2 | 1.0 | 5 | 70 |
| Embodiment 2 | 1.8 | 1.5 | 3 | 75 |
| Embodiment 3 | 1.2 | 0.5 | 4 | 65 |
| Embodiment 4 | 2.4 | 3 | 3 | 68 |
| Embodiment 5 | 1.5 | 1.5 | 5 | 72 |
In order to examine the pickling effect of granulated samples cutting surfaces, inventor carries out the sample after embodiment 1-5 pickling
Detection.Specifically, being detected using roughmeter to sample cutting surface roughness, using scanning electron microscope+energy disperse spectroscopy to sample
Product cut surface cleanliness is detected, and testing result is shown in Table 2.
2 embodiment 1-5 pickling effect of table summarizes
| Cut surface roughness Ra (μm) | Cut surface cleanliness | |
| Embodiment 1 | 0.8 | Energy spectrum diagram has no the pulse of oxygen, nitrogen |
| Embodiment 2 | 1.6 | Energy spectrum diagram has no the pulse of oxygen, nitrogen |
| Embodiment 3 | 0.8 | Energy spectrum diagram has no the pulse of oxygen, nitrogen |
| Embodiment 4 | 1.6 | Energy spectrum diagram has no the pulse of oxygen, nitrogen |
| Embodiment 5 | 1.6 | Energy spectrum diagram has no the pulse of oxygen, nitrogen |
In addition, inventor according to embodiment 2 pickling formula of liquid and acid cleaning process parameter to the ER7 of quality about 0.6g,
The granulated samples of DZ2,42CrMo, Q345B, LZ50, R260 steel grade are handled.Then, it is detected using oxygen nitrogen analyzer
Nitrogen oxygen content in granulated samples, testing result are shown in Table 3 after pickling.
3 embodiment 6-11 pickling effect of table summarizes
| Embodiment | Steel grade | Oxygen % | Nitrogen % |
| 6 | ER7 | 0.00073、0.00084 | 0.0022、0.0021 |
| 7 | Q345B | 0.00168、0.00181 | 0.0027、0.0025 |
| 8 | DZ2 | 0.00092、0.00097 | 0.0024、0.0023 |
| 9 | LZ50 | 0.00045、0.00056 | 0.0023、0.0022 |
| 10 | R260 | 0.0023、0.0025 | 0.0025、0.0027 |
| 11 | 42CrMo | 0.0016、0.0015 | 0.0019、0.0021 |
It can be seen from the above embodiments that, pickling solution of the invention and acid washing method are, it can be achieved that quickly remove carbon steel
The oxide layer generated with low-alloy steel due to cutting, keeps sample surfaces bright and clean, and without oxygen-containing, nitrogen substance is remaining, meets GB/
The requirement of T11261-2006, GB/T 20124-2006 analysis method to sample.
The present invention is hereinbefore disclosed with preferred embodiment, but it should be understood by those skilled in the art that, these
Embodiment is only used for describing the present invention, but should not be understood as limiting the scope of the invention.It should be noted that all implement with these
Example equivalent variation and displacement, should all be set as being covered by scope of the presently claimed invention.Therefore, protection scope of the present invention
It should be subject to range defined in claims.
Claims (10)
1. a kind of carbon steel and low-alloy steel cut surface oxide layer pickling solution, which is characterized in that the pickling solution by dilute hydrochloric acid and
Hexamethylenetetramine composition.
2. pickling solution according to claim 1, which is characterized in that the concentration of the dilute hydrochloric acid is 1.2-2.4mol/L.
3. pickling solution according to claim 2, which is characterized in that the concentration of the dilute hydrochloric acid is 1.2-1.8mol/L.
4. pickling solution according to claim 1, which is characterized in that quality of the hexamethylenetetramine in pickling solution is dense
Degree is 0.5%-3%.
5. pickling solution according to claim 4, which is characterized in that quality of the hexamethylenetetramine in pickling solution is dense
Degree is 0.8%-1.2%.
6. a kind of carbon steel and low-alloy steel cut surface oxide layer acid washing method, which comprises the following steps:
(1) sample is put into the pickling solution of heat, constant temperature impregnates；
(2) it is washed and is dried after taking out sample；
(3) after dry, using ethyl alcohol cleaning sample and drying.
7. acid washing method according to claim 6, which is characterized in that the sample is carbon content less than or equal to 0.70%
Carbon steel and/or low-alloy steel.
8. acid washing method according to claim 6, which is characterized in that the step (1) is that sample is put into 70 ± 5 DEG C
In pickling solution, 3-6min is impregnated.
9. acid washing method according to claim 6, which is characterized in that the step (2) is after taking out sample using distillation
Water cleans 5 times, and is dried up with hair dryer.
10. acid washing method according to claim 6, which is characterized in that after the step (3) is dry, using anhydrous second
Alcohol cleaning sample 2 times, and dried up with hair dryer.
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| CN113740142A (en) * | 2020-05-27 | 2021-12-03 | 宝山钢铁股份有限公司 | Method for obtaining hydrogen content of galvanized sheet matrix |
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