CN103741146B - The method of changeable valence rare earth composite corrosion inhibitor efficiency is improved in strong acid medium - Google Patents
The method of changeable valence rare earth composite corrosion inhibitor efficiency is improved in strong acid medium Download PDFInfo
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- CN103741146B CN103741146B CN201410008372.9A CN201410008372A CN103741146B CN 103741146 B CN103741146 B CN 103741146B CN 201410008372 A CN201410008372 A CN 201410008372A CN 103741146 B CN103741146 B CN 103741146B
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- corrosion inhibitor
- composite corrosion
- strong acid
- acid medium
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Abstract
The invention discloses the method improving changeable valence rare earth composite corrosion inhibitor efficiency in strong acid medium, comprise successively: take Ce (NO
3)
3and Na
2moO
4be dissolved in distilled water, Ce (NO
3)
3and Na
2moO
4mass ratio be 1:1 ~ 1:5, mass concentration total in solution is 0.12 ~ 0.20%, is made into Mo-Ce composite corrosion inhibitor; Oxygenant is added, oxygenant and Ce (NO in Mo-Ce composite corrosion inhibitor
3)
3mol ratio be 1:20 ~ 1:30, regulator solution pH value is 1, under the constant temperature of 303K, stir at least 20 minutes, obtains oxidizing Mo-Ce composite corrosion inhibitor; Obtained product is used for anticorrosion in strong acid medium of steel.Part changeable valence rare earth element by changing high price at a low price into, is solved the problem of the low and corrosion mitigating effect instability of changeable valence rare earth composite corrosion inhibitor inhibition efficiency in strong acid medium by the present invention.
Description
Technical field
The present invention relates to a kind of for changeable valence rare earth composite corrosion inhibitor, add the method that special oxygenant improves ferrous materials preservative efficiency in strong acid medium, the method can improve its inhibition efficiency can realize environmental friendliness again.
Background technology
Anti-corrosion have use equipment simple, easy to operate, invest the features such as little, effective, instant effect.Therefore, anti-corrosion erosion technology is used widely at industrial sectors such as petroleum chemical industry, heavy machinery industry, the energy, metallurgy.At present, ripely in industrial practice to use and the inhibiter being applied to carbon steel mainly contains following a few class: chromate inhibiter, mercury salt class inhibiter, nitrites inhibiter and alkynol class inhibiter, although these inhibiter have good inhibition efficiency, but there is the shortcoming that is common: poisonous to human body, to bad environmental.Especially chromic salt, can be carcinogenic.
The inhibiter that exploitation has features such as efficient, nontoxic, non-environmental-pollution has become the research main flow of this area.Due to the advantage such as nontoxic, inexpensive, resource is wide, rare earth inhibiter is expected to the leader becoming green corrosion inhibitor field.The research application major part of current rare earth inhibiter concentrates in neutral medium.The research that is inorganic, organic inhibitor compound use in acidic medium rare earth inhibiter and other being had strong coordination ability is at present reported, mainly for Rare-Earth Ce
4+ion, this is due to Ce
4+ion can form the better title complex ion of stability with negatively charged ion in the solution, matrix and corrosive medium is more effectively kept apart, plays better corrosion-resisting function.In addition, shown by calculation of thermodynamics and pH-Electric Potential Graph, Ce
4+ion can also form insoluble compound in corresponding system, and the active site of covered cathode reaction, contributes to the raising of inhibition efficiency.Also there are some researches show, Rare-Earth Ce
4+ion and sodium molybdate corrosion inhibitor compound use in strong acid medium, not only can not play Synergistic Effect of Corrosion Inhibition to steel, shows obvious antagonistic effect (i.e. anti-corrosion inhibition) on the contrary.On the one hand, due to Ce
4+ion, with four positive charges, has strong repulsive interaction with positively charged steel surface, therefore is difficult to form protectiveness film at steel surface; On the other hand, from Nernst equation, Ce in strong acid medium
4+the oxidisability of ion can obviously strengthen, and reason is Ce
4+/ Ce
3+the right electropotential of electricity can improve a lot, much larger than Fe
2+the electropotential that/Fe electricity is right, therefore Ce
4+ion is easy to capture electronics from metallic iron and make steel accelerated corrosion.
According to the literature; in the protective membrane that changeable valence rare earth element inhibiter is formed at steel specimen surface; there is (namely a part for same element there occurs valent transformation in mechanism) in the compound no longer formed with single chemical valence state; cause the compactness of surface protection film and corrosion mitigating effect to become better, inhibiter shows higher inhibition efficiency.Therefore, realize partial routine to the inhibiter containing changeable valence rare earth element to appraise at the current rate conversion (RE
3+→ RE
4+), the inhibition efficiency of this inhibiter can be improved to a great extent.
At present, in neutral medium to Ce
3+the process of carrying out appraise at the current rate conversion technique relative maturity and be used widely, expand Rare-Earth Ce
3+the application of inhibiter in neutral medium.But because the stability of a lot of oxygenant in acidic medium (especially strong acid medium) and existence change, cause in strong acid medium Rare-Earth Ce
3+the ion process of carrying out appraise at the current rate conversion target be difficult to realize, limit Rare-Earth Ce
3+the application of ion inhibiter in strong acid medium, thus reduce the range of application in engineering reality.Therefore, only have the inhibition system preparing a kind of correspondence, find a kind of appropriate oxygenant, in strong acid medium, the effect of appraising at the current rate of Rare-Earth Ce element can be played by stability and high efficiency, could Rare-Earth Ce be expanded
3+the application of ion inhibiter in strong acid medium.
Summary of the invention
The object of the present invention is to provide the method improving changeable valence rare earth composite corrosion inhibitor efficiency in strong acid medium, the method is taked in strong acid medium, use special strong oxidizer, realize part changeable valence rare earth element by changing high price at a low price into, thus improve changeable valence rare earth composite corrosion inhibitor efficiency, solve the problem of the low and corrosion mitigating effect instability of changeable valence rare earth composite corrosion inhibitor inhibition efficiency in strong acid medium.
For reaching above technical purpose, the invention provides following technical scheme.
The present invention adopts the oxygenant in strong acid medium with strong oxidizing property, carry out partial routine to changeable valence rare earth element to appraise at the current rate conversion, composite corrosion inhibitor is formed with molybdate, form and have easily and the complex bound composite inorganic molecule in metallic surface, bonding force between enhancing and steel interface atoms and adsorption, reach the object improving changeable valence rare earth composite corrosion inhibitor efficiency.
First, with the Ce (NO of different mass
3)
3and Na
2moO
4be made into the Mo-Ce composite corrosion inhibitor of different ratio, by adding appropriate different types of strong oxidizer, be dissolved in distilled water, slow dropping saturated HCl regulator solution pH value is 1, under magnetic stirring apparatus, constant temperature (303K) stirs half an hour, treat that several compound fully reacts in aqueous, obtain (Mo-Ce) composite corrosion inhibitor of different oxidizing formation, adopt the Mo-Ce composite corrosion inhibitor of the different oxidizing formation of weight-loss method calculating in strong acid medium to the inhibition efficiency of ferrous materials, thus obtain the Mo-Ce composite corrosion inhibitor of the strong oxidizer oxidation of efficiency the best.
In strong acid medium, improve the method for changeable valence rare earth composite corrosion inhibitor efficiency, comprise the following steps successively:
(1) Ce (NO of different mass is taken
3)
3and Na
2moO
4be dissolved in distilled water, Ce (NO
3)
3and Na
2moO
4mass ratio be 1:1 ~ 1:5, mass concentration total in solution is 0.12 ~ 0.20%, is made into Mo-Ce composite corrosion inhibitor;
(2) in Mo-Ce composite corrosion inhibitor, add oxygenant, described oxygenant is persulphate (ammonium persulphate, Potassium Persulphate or Sodium Persulfate), potassium permanganate or hydrogen peroxide, oxygenant and Ce (NO
3)
3mol ratio be 1:20 ~ 1:30, slowly dripping saturated HCl regulator solution pH value is 1, stirs at least 20 minutes, treats that several compound fully reacts in aqueous, obtain oxidizing Mo-Ce composite corrosion inhibitor with magnetic stirring apparatus under the constant temperature of 303K;
(3) product obtained in step (2) is used for anticorrosion in strong acid medium of steel.
Ce (NO
3)
3and Na
2moO
4respectively as the inhibiter of steel in strong acid medium, when being used alone, consumption is large, efficiency is low; The inhibition efficiency of the Mo-Ce composite corrosion inhibitor of different dosage is far longer than efficiency when these two kinds of inhibiter are used alone or adds and efficiency, illustrates that these two kinds of inhibiter exist obvious Synergistic Effect of Corrosion Inhibition to steel when compound shares in strong acid medium.Ce (the NO used in the present invention
3)
3and Na
2moO
4be analytical pure.
Oxygenant is added in Mo-Ce composite corrosion inhibitor, even if when oxygenant dosage is very little, larger impact is had on the inhibition efficiency of Mo-Ce composite corrosion inhibitor, the persulphate of especially appropriate concentration can significantly improve the inhibition efficiency of composite corrosion inhibitor, and different persulfate oxidation agent to affect the rule of efficiency change substantially identical, as persulfate oxidation agent consumption and Ce (NO
3)
3molar concentration rate when being 1:25, there is maximum value in inhibition efficiency, especially (NH4) 2S2O8 can make inhibition efficiency reach 90%, and this illustrates to have and only have the changeable valence rare earth ion of tiny segment to achieve process and to appraise at the current rate conversion (Ce
3+→ Ce
4+) good corrosion mitigating effect could be obtained.
Realize appraising at the current rate conversion in the process of strong acid medium Rare Earth Ion, selected oxygenant not only self will have stronger oxidisability and stability, more needs to consider that kinetic factor and the condition of selective reaction occur these oxygenants in system.In strong acid medium, persulphate and Ce
3+there is redox reaction
realize part Ce
3+ion to be appraised at the current rate conversion by the process changing high price at a low price into.
Mo-Ce composite corrosion inhibitor produces thin film at steel specimen surface, and this is that steel sample corrosion reaction apparent activation energy increases, the major cause that corrosion difficulty increases.And the Mo-Ce composite corrosion inhibitor that different persulfate oxidation agent oxidation is formed in strong acid medium at the film that specimen surface is formed, more smooth densification, increases the surface coverage of film to sample, thus enhances corrosion mitigating effect.
Compared with prior art, the present invention has following beneficial effect: the present invention guarantees to realize a changeable valence rare earth element part by changing high price at a low price in strong acid medium, while raising changeable valence rare earth composite corrosion inhibitor inhibition efficiency, too increase the stability of changeable valence rare earth composite corrosion inhibitor corrosion mitigating effect, the present invention also has eco-friendly characteristic.
Accompanying drawing explanation
Fig. 1 is Ce (NO
3)
3, Na
2moO
4with Mo-Ce composite corrosion inhibitor inhibition efficiency curve to steel in strong acid medium.
Fig. 2 be oxidizing Mo-Ce composite corrosion inhibitor in strong acid medium to the inhibition efficiency curve of steel.
Fig. 3 is that (condition is the macro surface shape appearance figure of steel sample in different inhibition system after immersion corrosion experiment: 2molL
-1hCl, 303K)
The valent existence of Ce elements difference in the protective membrane that Fig. 4 is Mo-Ce composite corrosion inhibitor, the Mo-Ce composite corrosion inhibitor of ammonium persulphate oxidation is formed at specimen surface.
Embodiment
The present invention is further illustrated below in conjunction with embodiment and accompanying drawing.
One, utilize oxygenant in strong acid medium, improve the efficiency of changeable valence rare earth composite corrosion inhibitor
Embodiment 1:
The preparation of Mo-Ce composite corrosion inhibitor in strong acid medium:
Take the Ce (NO that mass ratio is 1:2
3)
3and Na
2moO
4be dissolved in distilled water, the total mass concentration of solution is 0.15%, and slowly drip saturated HCl in the solution, regulator solution pH value is 1, and under magnetic stirring apparatus, constant temperature (303K) stirs half an hour, obtains Mo-Ce composite corrosion inhibitor.
With (NH in strong acid medium
4)
2s
2o
8oxidation Mo-Ce composite corrosion inhibitor:
In the Mo-Ce composite corrosion inhibitor of above-mentioned preparation, add oxygenant (NH
4)
2s
2o
8, oxygenant and Ce (NO
3)
3mol ratio be 1:25, slowly drip saturated HCl in the solution, regulator solution pH value is 1, and under magnetic stirring apparatus, constant temperature (303K) stirs half an hour, obtains (NH
4)
2s
2o
8the Mo-Ce composite corrosion inhibitor of oxidation.
Obtained product is used for anticorrosion in strongly-acid etchant solution of steel sample.
Two, the performance test of the Mo-Ce composite corrosion inhibitor of oxidation
Steel sample pretreating: polished with 400#, 600#, 800# sand paper successively by the steel sample of 30mm × 20mm × 2mm, then uses acetone and ethanol purge to remove the grease of specimen surface, finally in drying basin, carries out drying.For guaranteeing the reliability of testing, carry out parallel extension sample.
Strongly-acid etchant solution: use saturated HCl and distilled water preparation 2molL
-1hCl solution.
(1) inhibition efficiency of weight-loss method test inhibiter
Steel sample after process is accurately weighed, is suspended from not containing inhibiter with containing Ce (NO
3)
3, Na
2moO
4, in the etchant solution of Mo-Ce composite corrosion inhibitor that is oxidized of Mo-Ce composite corrosion inhibitor, strong oxidizer (ammonium persulphate, Potassium Persulphate, Sodium Persulfate, potassium permanganate and hydrogen peroxide), immersion corrosion through 72h takes out steel sample after testing (constant temperature 303K), cleaning, dry up, accurately weigh, calculate the average weightless Δ W of steel sample.
Inhibition efficiency calculates:
Δ W in formula
0, Δ W be respectively not containing and containing the average weight loss of steel sample during inhibiter.
Fig. 1 is Ce (NO
3)
3, Na
2moO
4with Mo-Ce composite corrosion inhibitor inhibition efficiency curve to steel in strong acid medium, Ce (NO
3)
3and Na
2moO
4respectively as the inhibiter of steel in strong acid medium, when being used alone, consumption is large, efficiency is low; The inhibition efficiency of the Mo-Ce composite corrosion inhibitor of different dosage is far longer than efficiency when these two kinds of inhibiter are used alone or adds and efficiency, illustrates that these two kinds of inhibiter exist obvious Synergistic Effect of Corrosion Inhibition to steel when compound shares in strong acid medium.Wherein Ce (NO
3)
3and Na
2moO
4mass ratio be 1:2, concentration of polymer solution is when being 0.15%, synergistic effect is the most obvious between the two, has best corrosion mitigating effect.
Fig. 2 be oxidizing Mo-Ce composite corrosion inhibitor in strong acid medium to the inhibition efficiency curve of steel.The data presentation of Fig. 2, even if when oxygenant addition is very little, have larger impact to the inhibition efficiency of Mo-Ce composite corrosion inhibitor, wherein the persulphate of appropriate concentration (comprises (NH
4)
2s
2o
8, K
2s
2o
8and Na
2s
2o
8) inhibition efficiency of Mo-Ce composite corrosion inhibitor can be significantly improved, as persulfate oxidation agent consumption and Ce (NO
3)
3molar concentration rate when being 1:25, all there is maximum value (IE%>80%) in inhibition efficiency, wherein (NH
4)
2s
2o
8inhibition efficiency can be made to bring up to 90%.
(2) polarization curve test
Adopt three-electrode system, bare area is the steel sample of 10mm × 10mm is working electrode, and platinum electrode is supporting electrode, and saturated calomel electrode (SCE) is reference electrode, and in measuring process, all current potentials are all relative to SCE.Measuring parameter is set to: sweep velocity is 0.2mVs
-1, sweep interval is-300 ~ 300mVvs.E
corr(corrosion potential).
Inhibition efficiency calculates:
I in formula
blank, I
inhibitorbe respectively the corrosion electric current density of steel sample in strong acid medium when not containing and contain inhibiter.
The contrast of table 1 polarization curve test electrochemical parameter
From the electrochemical parameter of table 1, add ammonium persulfate oxidizing agent in Mo-Ce composite corrosion inhibitor after, the corrosion current density that corrosion reaction occurs steel sample in strong acid medium reduces (54mA/cm further
2be reduced to 19mA/cm
2), the corrosion speed of steel sample reduces, and inhibition efficiency improves (being increased to 87.66% by 64.94%).Because ammonium persulphate reduces anode retardation while increase negative electrode retardation, while the corrosion current density of steel sample is reduced, corrosion potential is also made to reduce.
(3) surface film pattern test
Take out the steel sample through the experiment of 72h immersion corrosion in the strongly-acid etchant solution not containing inhibiter and the Mo-Ce composite corrosion inhibitor containing Mo-Ce composite corrosion inhibitor, ammonium persulphate oxidation, with tap water washed samples surface, natural air drying in air, stereomicroscope observation.
The film morphology of specimen surface shown in Fig. 3 shows, the film that the existence of ammonium persulphate makes Mo-Ce composite corrosion inhibitor be formed at steel specimen surface is finer and close smooth, and increase the coverage of film, the possibility that corrosive medium contacts with steel specimen surface reduces.(4) surface film component valence state test
Take out at the steel sample of Mo-Ce composite corrosion inhibitor in strongly-acid etchant solution after the experiment of 72h immersion corrosion containing Mo-Ce composite corrosion inhibitor, ammonium persulphate oxidation, with tap water washed samples surface, natural air drying in air, adopts photoelectron spectrograph to test film element and valence state.
Fig. 4 shows, in the film formed by Mo-Ce composite corrosion inhibitor, Ce elements is with Ce
3+state exists, and in the film that the Mo-Ce composite corrosion inhibitor be oxidized by ammonium persulphate is formed, Ce elements is with Ce
3+, Ce
4+two kinds of valent states coexist.The existence of ammonium persulphate achieves part Ce elements in Corrosion Inhibition by a low price to the conversion of appraising at the current rate that high price changes, and therefore improves inhibition efficiency.
(5) environmental-protecting performance test
The Mo-Ce composite corrosion inhibitor that ammonium persulphate is oxidized is formulated as the aqueous solution of 1%, listed by table 2, detection method measures eight environmental protection indexs such as arsenic, lead, chromium, cadmium, mercury, sexavalent chrome, petroleum-type and bio-toxicity.
Table 2 environmental-protecting performance detection method and result
Table 2 environmental protection index detects and shows, the indexs such as arsenic, lead, chromium, cadmium, mercury, sexavalent chrome, petroleum-type all do not detect, and bio-toxicity is nontoxic, shows good environmental-protecting performance.
Claims (2)
1. in strong acid medium, improve the method for changeable valence rare earth composite corrosion inhibitor efficiency, comprise the following steps successively:
(1) Ce (NO of different mass is taken
3)
3and Na
2moO
4be dissolved in distilled water, Ce (NO
3)
3and Na
2moO
4mass ratio be 1:1 ~ 1:5, mass concentration total in solution is 0.12 ~ 0.20%, is made into Mo-Ce composite corrosion inhibitor;
(2) in Mo-Ce composite corrosion inhibitor, add oxygenant, described oxygenant is persulphate, oxygenant and Ce (NO
3)
3mol ratio be 1:20 ~ 1:30, slowly dripping saturated HCl regulator solution pH value is 1, stirs at least 20 minutes, treats that several compound fully reacts in aqueous, obtain oxidizing Mo-Ce composite corrosion inhibitor with magnetic stirring apparatus under the constant temperature of 303K;
(3) product obtained in step (2) is used for anticorrosion in strong acid medium of steel.
2. the method improving changeable valence rare earth composite corrosion inhibitor efficiency as claimed in claim 1, is characterized in that, in described step (2), persulphate is ammonium persulphate, Potassium Persulphate or Sodium Persulfate.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6716370B2 (en) * | 2001-07-25 | 2004-04-06 | The Boeing Company | Supramolecular oxo-anion corrosion inhibitors |
| CN101914775A (en) * | 2010-06-29 | 2010-12-15 | 青岛大学 | Water-soluble anthranilic acid polymer carbon steel acid cleaning inhibitor and application thereof |
-
2014
- 2014-01-08 CN CN201410008372.9A patent/CN103741146B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6716370B2 (en) * | 2001-07-25 | 2004-04-06 | The Boeing Company | Supramolecular oxo-anion corrosion inhibitors |
| CN101914775A (en) * | 2010-06-29 | 2010-12-15 | 青岛大学 | Water-soluble anthranilic acid polymer carbon steel acid cleaning inhibitor and application thereof |
Non-Patent Citations (2)
| Title |
|---|
| Research on anti-corrosion property of rare earth inhibitor for X70 steel;朱艳华 等;《Journal of Rare Earths》;20130731;第31卷(第7期);第735页左栏第27行-右栏第9行、第736页右栏第8-31行，图1-2 * |
| 不锈钢表面稀土铈化学转化膜耐蚀性能的研究;杜康;《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》;20090715(第7期);正文第16页20-21行、第28页第19行-第29页第28行、第49页第1-6行、第53页第2行-第54页第19行，表4.1-4.2、图5.1 * |
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