CN107686990A - A kind of amino acid molybdenum disulfide composite corrosion inhibitor and its application - Google Patents
A kind of amino acid molybdenum disulfide composite corrosion inhibitor and its application Download PDFInfo
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- CN107686990A CN107686990A CN201710740879.7A CN201710740879A CN107686990A CN 107686990 A CN107686990 A CN 107686990A CN 201710740879 A CN201710740879 A CN 201710740879A CN 107686990 A CN107686990 A CN 107686990A
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- molybdenum disulfide
- amino acid
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- ethanol
- corrosion inhibitor
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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
- C23F11/08—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in other liquids
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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
- C23F11/04—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in markedly acid liquids
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Abstract
The invention discloses a kind of amino acid molybdenum disulfide composite corrosion inhibitor, and the wherein quality proportioning of amino acid and molybdenum disulfide is 10~1000:1, described amino acid is more than one or both of L serines, L arginine, cystine and methionine.The invention also discloses a kind of system with corrosion inhibition, and it is saline solns or dilute acid soln, and is dispersed with 3~30mmol/L amino acid and 10~50mg/L molybdenum disulfide.The invention also discloses the preparation method of the system with corrosion inhibition.The amino acid molybdenum disulfide composite corrosion inhibitor can effectively slow down corrosion of metal under strong acid or sea conditions, industrial copper product be particularly suitable for use in acid or sea conditions inhibition, and amino acid therein and molybdenum disulfide are the relatively low raw material of toxicity, it is ensured that the low toxic and environment-friendly of composite corrosion inhibitor.
Description
Technical field
The present invention relates to inhibiter technology field, and in particular to a kind of amino acid-molybdenum disulfide composite corrosion inhibitor, and comprising
Its system with corrosion inhibition and its collocation method and application.
Background technology
Metal material has very important status as a kind of important materials in Material Field.Since 21 century with
The continuous development of contemporary metal materialogy, metal industry, agricultural, construction industry, space flight and aviation, electronic information etc. it is multi-field should
With more and more extensive.And in chemical industry, metal material such as steel, copper etc. easily by local environment medium influence and
Chemistry or electrochemical reaction occur for metal interface so as to be damaged, and here it is metal erosion.Such as in chemical process,
Metal machinery equipment often contacts with strong corrosive media (such as acid, alkali, salt), particularly the technique in HTHP and high flow rate
Under the conditions of, etching problem seems more prominent and serious.
According to statistics, caused by the 10%~20% of the annual metal loss total amount in the whole world is corrosion, the just annual steel production of China
Measure up to for 2.2 hundreds of millions tons, equivalent to 22,000,000 tons steel disappear due to corrosion, and this substantially corresponds to a large-scale steel
The annual production of factory.The harm of metal erosion is very big, except that can damage industrial equipment, shortens its service life, and serious is also possible to
Cause the generation of the catastrophic failures such as fire, blast.This not only greatly improves industrial cost, causes huge economic losses, can also
Cause the serious wasting of resources and environmental pollution.Therefore research Process of Metallic Corrosion, principle and corrosion protection means are most important.Gold
Category corrosion process is to produce corrosion product by metal material and corrosive medium collective effect in general, and it comprises at least three bases
This process：(a) corrosive medium is migrated by diffusion and convection action to metal interface；(b) corrosive medium and metal are in boundary
React；(c) corrosion product of reaction generation forms cover layer or slave phase interfacial migration in metal surface into medium.
In recent years because the development of green corrosion inhibitor, some carbohydrate and amino acids are also gradually developed
Utilize, be used for metal coating as natural green inhibitor.Amino acid is rich content, the production of biodegradable native metabolic
Thing, but its adsorption capacity in metal surface is reduced because its is simple in construction, so as to limit amino acid as industrial inhibition
The potentiality of agent.MohammedA etc. has found natural amino acid alanine, Cys and its derivative in acid medium to gold
Category iron has preferable slow releasing function.After Deng Qiong et al. is linked together L-threonine and L-phenylalanine by Click reactions
It was found that gained bis-amino acid compound is higher to the sustained release efficiency of carbon steel in hydrochloric acid, and have compared to natural amino acid composition
And significantly improve.Furtherd investigate again afterwards, serine, threonine, phenylalanine are connected with tyrosine respectively, as a result sent out
These three existing bis-amino acid compounds have above-mentioned phenomenon.
The content of the invention
The first object of the present invention be to provide a kind of good and less toxic green amino acid of new corrosion mitigating effect-
Molybdenum disulfide composite corrosion inhibitor, the amino acid-molybdenum disulfide composite corrosion inhibitor can effectively slow down metal especially copper product and exist
Corrosion under strong acid or sea conditions.
The quality proportioning of amino acid and molybdenum disulfide is 10~1000 in the amino acid-molybdenum disulfide composite corrosion inhibitor:1
It is preferred that 40~250:1, described amino acid is Serine, L-arginine, cystine, methionine and their derivative
One or both of more than, preferably Serine or L-arginine.
When preparing the amino acid-molybdenum disulfide composite corrosion inhibitor, amino acid and molybdenum disulfide powder can be disperseed simultaneously
In a solvent, carry out compound obtaining amino acid-molybdenum disulfide composite corrosion inhibitor in a solvent.Wherein molybdenum disulfide can first pass through thing
The relatively large rough powder of particle is made in reason method, then ethanol/water mixed solvent can be used to be disperseed, and removing solvent can
The molybdenum disulfide powder that must be refined, wherein ethanol can remove under reduced pressure, and water can dry removal.Refined molybdenum disulfide powder can be compared with
It is compound by the progress of supermolecular mechanism power with amino acid to be easily dispersed in solvent.It is compound containing amino acid-molybdenum disulfide
The dispersion liquid of corrosion inhibiter can be directly added into acid, cooling circulation without amino acid-molybdenum disulfide composite corrosion inhibitor is separated
In water or seawater, the application in Industrial Metal inhibition, the especially application in copper product inhibition are realized.
Therefore, the second object of the present invention, which is that, provides a kind of system with corrosion inhibition, its for saline solns or
Dilute acid soln, and it is dispersed with 3~30mmol/L preferably 5~20mmol/L amino acid and 10~50mg/L preferably 20~40mg/L
Molybdenum disulfide.
The system can be used as process water, such as recirculated water, cooling water etc., amino acid and molybdenum disulfide therein to pass through
Supermolecular mechanism power carries out being compounded to form amino acid-molybdenum disulfide composite corrosion inhibitor, can effectively improve the corrosion inhibition of system.
Wherein, saline solns can be seawater, or other are dissolved with the solution of inorganic salts such as sodium salt, sylvite etc.；Diluted acid
Solution can be watery hydrochloric acid, dust technology and dilute sulfuric acid etc..
The system with corrosion inhibition can be configured by following steps：
(a) molybdenum disulfide powder prepared by physical method is scattered in obtained in ethanol/water the ethanol of molybdenum disulfide/
Aqueous dispersions, it is evaporated under reduced pressure at 10~50 DEG C after removing ethanol and dries, obtains refined molybdenum disulfide powder, then by refined curing
Molybdenum powder is dispersed in water, and the aqueous dispersions of molybdenum disulfide are made；
(b) aqueous dispersions of molybdenum disulfide made from quantitative amino acid solution and step (a) are mixed, then used
System solution constant volume, control final concentration of 3~30mmol/L preferably 5~20mmol/L of amino acid, the final concentration of molybdenum disulfide
It is scattered homogeneous to produce the system with corrosion inhibition for 10~50mg/L preferably 20~40mg/L；The system solution is salt solution
Or diluted acid.
Preferably, in step (a), described physical method is micromechanics stripping means.
Preferably, in step (a), the volume ratio of second alcohol and water is 1 in the mixed liquor of ethanol/water:0.5~2, preferably 1:1.
Preferably, step (a) can be specially：By the molybdenum disulfide powder prepared by micromechanics stripping method be placed in ethanol/
In the mixed liquor of water, at room temperature, ultrasound 3~72 hours, rotating speed centrifuges under the conditions of being 1000~8000 revs/min, takes upper liquid
Body, the ethanol/water dispersion liquid of molybdenum disulfide is obtained, be evaporated under reduced pressure after removing ethanol and dry at 10~50 DEG C, obtain refined two sulphur
Change molybdenum powder, then refined molybdenum disulfide powder is placed in ultra-pure water, ultrasound 5~60 minutes, the moisture that molybdenum disulfide is made dissipates
Liquid.
Preferably, it is 10~50mg/mL that molybdenum disulfide concentration in described aqueous dispersions is controlled in step (a)；Step (b)
In in used Freamine Ⅲ the solubility of amino acid be 50~200mmol/L, solvent is system solution.
Beneficial effects of the present invention：The present invention possesses Serine, L-arginine or their derivative etc. certain slow
It is compound to lose amino acid and the molybdenum disulfide powder progress of effect, forms the amino acid based on supermolecular mechanism power and is answered with molybdenum disulfide
Condensation material green corrosion inhibitor, it can effectively slow down corrosion of metal under strong acid or sea conditions, be particularly suitable for use in industrial copper product
In acid or sea conditions inhibition, and Serine in the molybdenum disulfide composite corrosion inhibitor and molybdenum disulfide are poison
The relatively low raw material of property, it is ensured that the low toxic and environment-friendly of the molybdenum disulfide composite corrosion inhibitor.
Brief description of the drawings
Fig. 1 is the transmission electron microscope picture of amino acid-molybdenum disulfide composite corrosion inhibitor of the present invention；
Fig. 2 is the electrochemical impedance spectrogram of the effect example of the present invention；
Fig. 3 is the copper sheet surface topography after pure copper samples are soaked in hydrochloric acid solution；
Fig. 4 is the copper sheet surface shape after pure copper samples are soaked in amino acid-molybdenum disulfide composite corrosion inhibitor of the present invention
Looks.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described.It should be understood that following examples are merely to illustrate this
Invention is not for restriction the scope of the present invention.
The configuration of the compound slow corrosion watery hydrochloric acid system of embodiment 1
Step：
(a) molybdenum disulfide powder prepared by micromechanics stripping means is placed in ethanol/water (v:V=1:1) mixing
In liquid, at room temperature, ultrasound 48 hours, rotating speed centrifuges under the conditions of being 4000 revs/min, takes supernatant liquid, obtains molybdenum disulfide
Ethanol/water dispersion liquid, it is evaporated under reduced pressure at 30 DEG C after removing ethanol and is put into oven for drying, obtain refined molybdenum disulfide powder, then will
Refined molybdenum disulfide powder is placed in ultra-pure water, and (resistivity is more than 18M Ω cm-1Water) in, ultrasound 20 minutes, 10mg/mL is made
Molybdenum disulfide aqueous dispersions.
(b) quantitative amino acid dilute hydrochloric acid solution (100mmol/L) mixes with molybdenum disulfide aqueous dispersions made from step (a)
Close, with 1mol/L watery hydrochloric acid constant volume, be made the dispersion liquid of amino acid-molybendum disulfide complexes, Serine it is final concentration of
20mmol/L, the final concentration of 10mg/L of molybdenum disulfide, is ultrasonically formed after homogeneous system and stands 10 minutes at room temperature, obtains two sulphur
Change molybdenum compound slow corrosion watery hydrochloric acid system.
Repeat step (b), adjusts the combined amount of molybdenum disulfide aqueous dispersions, and the final concentration for controlling molybdenum disulfide is respectively
20mg/L, 40mg/L and 50mg/L.So far two sulphur containing 10mg/L, 20mg/L, 40mg/L and 50mg/L respectively are made altogether
Change four kinds of inhibition systems using watery hydrochloric acid as system solution of molybdenum, the wherein quality proportioning of amino acid and molybdenum disulfide is 210:1,
105:1,53:Isosorbide-5-Nitrae 2:1.
Draw the compound slow corrosion watery hydrochloric acid system (Serine 20mmol/L, molybdenum disulfide 40mg/L) of the 20 above-mentioned preparations of μ L
It is added drop-wise on copper mesh.After 20 minutes, carefully solution is blotted with paper, naturally dry, its transmitted electron flying-spot microscope (TEM) is surveyed
The surface topography of examination is as shown in Figure 1.TEM tests use the model projection-type electronic scanner microscopes of JEOL 1400, equipped with
GatanOrius electric poles coupled camera and Tridiem energy filters, test voltage 200kV.
The configuration of the compound slow corrosion dust technology system of embodiment 2
With reference to embodiment 1, difference is in step (b) to replace watery hydrochloric acid using 1mol/L dust technology, and Serine is molten
The solvent of liquid also does corresponding adjustment.Three kinds of the obtained molybdenum disulfide containing 10mg/L, 20mg/L and 50mg/L respectively are with dilute
Nitric acid is the inhibition system of system solution.
The configuration of the compound slow corrosion seawer system of embodiment 3
With reference to embodiment 1, difference is to replace dilute salt using the 3.5% NaCl aqueous solution (simulated seawater) in step (b)
Acid, the solvent of Serine solution also do corresponding adjustment.The curing containing 10mg/L, 20mg/L and 50mg/L respectively is made
Inhibition system of three kinds of molybdenum using seawater as system solution.
Effect example
1st, copper sheet pre-processes
Copper strips is divided into the copper sheet that size is 1.2cm × 1.0cm × 0.2cm by being machined, and in a side perforation
So that connecting wire is used for electro-chemical test.Before the use, the working face of all copper sheets all with waterproof abrasive paper from coarse to fine step by step
1200 mesh are polishing to, then with the fine grinding again of different size abrasive paper for metallograph, the room temperature after deionized water, acetone, ethanol washing
Drying for standby.
2nd, electrochemical impedance is tested
(1) watery hydrochloric acid system
Blank group：Using 1mol/L watery hydrochloric acid as test fluid, will surveyed after above-mentioned pretreated copper sheet connecting wire
Soaked in test solution 2 hours, the open-circuit voltage then caught using system is initial value, by setting frequency range, response excursion etc.
Parameter applies sinusoidal voltage to electro-chemical systems and carries out testing impedance, determines electrochemical impedance spectrogram and polarization impedance.Survey
During examination, temperature control is 25 DEG C, and the copper sheet area being immersed in test fluid is 1.4cm2, remainder polytetrafluoroethylene (PTFE)
Band wrapping and encapsulating.
Experimental group：The compound slow corrosion watery hydrochloric acid system containing various concentrations molybdenum disulfide configured with embodiment 1 replaces dilute
Hydrochloric acid carries out electrochemical impedance test, the same blank group of testing procedure respectively as test fluid.
Control group：With the watery hydrochloric acid containing various concentrations Serine (5mmol/L, 10mmol/L, 20mmol/L)
(1mol/L) is used as test fluid, carries out electrochemical impedance test, the same blank group of testing procedure respectively.
(2) dust technology system
With reference to watery hydrochloric acid system, wherein,
The test fluid of blank group is 1mol/L dust technology；
The test fluid of experimental group is the compound slow corrosion dust technology body containing various concentrations molybdenum disulfide that embodiment 2 configures
System；
The test fluid of control group is dilute nitre containing various concentrations Serine (5mmol/L, 10mmol/L, 20mmol/L)
Sour (1mol/L).
(3) seawer system
With reference to watery hydrochloric acid system, wherein,
The test fluid of blank group is 3.5% NaCl solution；
The test fluid of experimental group is the compound slow corrosion dust technology body containing various concentrations molybdenum disulfide that embodiment 3 configures
System；
The test fluid of control group is the NaCl containing various concentrations Serine (5mmol/L, 10mmol/L, 20mmol/L)
Solution (3.5%).
Test result：
Fig. 2 is the electrochemical impedance spectrogram that measures of three kinds of test fluids of watery hydrochloric acid system, and " 1MHCl " in figure represents blank
Group (1mol/L watery hydrochloric acid), " amino acid " represents control group (Serine 20mmol/L), and " amino acid molybdenum disulfide is compound slow
Erosion agent " represents experimental group (molybdenum disulfide 40mg/L, Serine 20mmol/L).As shown in Figure 2, the present invention is dispersed with L- silk ammonia
The system of acid and molybdenum disulfide greatly improves compared to the system for being only dispersed with Serine, polarization impedance.
Table 1 show the inhibition efficiency η of above-mentioned three kinds of systems difference corrosion inhibiter, and inhibition efficiency η calculating formula is as follows：
R in formulap(0)The polarization impedance measured for blank group, RpThe polarization impedance measured for experimental group or control group.
The inhibition efficiency η test results of table 1
As seen from the results in Table 1, the present invention is dispersed with the system of Serine and molybdenum disulfide compared to being only dispersed with L- silks
The system of propylhomoserin, the inhibition efficiency of copper sheet is greatly improved, can effectively alleviate the electrochemical corrosion of copper sheet.
3rd, fine copper immersion test
By the molybdenum disulfide compound slow corrosion system that pure copper samples are separately immersed in watery hydrochloric acid (1mol/L) and prepared by embodiment 1
In (Serine 20mmol/L, molybdenum disulfide 40mg/L), observed respectively by SEM (SEM) after 0.5 hour
Its surface topography.Scanning electron microscope test uses JSM-6360LV model vacuum SEM, morphology characterization point
Not as shown in Figures 3 and 4.Understanding in watery hydrochloric acid, there is more serious corrosion in pure copper samples, and in the molybdenum disulfide of the present invention
Significantly corroding does not occur in composite corrosion inhibitor.
Claims (10)
1. a kind of amino acid-molybdenum disulfide composite corrosion inhibitor, the wherein quality proportioning of amino acid and molybdenum disulfide are 10~1000:
1, described amino acid is more than one or both of Serine, L-arginine, cystine and methionine.
2. amino acid as claimed in claim 1-molybdenum disulfide composite corrosion inhibitor, it is characterised in that described amino acid is L-
Serine or L-arginine；The quality proportioning of amino acid and molybdenum disulfide is 40~250:1.
A kind of 3. system with corrosion inhibition, it is characterised in that it is saline solns or dilute acid soln, and it is dispersed with 3~
30mmol/L amino acid and 10~50mg/L molybdenum disulfide.
4. the collocation method of system as claimed in claim 3, it is characterised in that it comprises the following steps：
(a) molybdenum disulfide powder prepared by physical method is scattered in the ethanol/water point that molybdenum disulfide is obtained in ethanol/water
Dispersion liquid, it is evaporated under reduced pressure at 10~50 DEG C after removing ethanol and dries, obtains refined molybdenum disulfide powder, then by refined molybdenum disulphide powder
End is dispersed in water, and the aqueous dispersions of molybdenum disulfide are made；
(b) aqueous dispersions of molybdenum disulfide made from quantitative Freamine Ⅲ and step (a) are mixed, it is then molten using system
Liquid constant volume, final concentration of 3~30mmol/L of amino acid, final concentration of 10~50mg/L of molybdenum disulfide are controlled, disperseed homogeneous
Produce the system with corrosion inhibition；The system solution is salt solution or diluted acid.
5. method as claimed in claim 4, it is characterised in that in step (a), described physical method is micromechanics stripping side
Method.
6. method as claimed in claim 4, it is characterised in that in step (a), second alcohol and water in the mixed liquor of ethanol/water
Volume ratio is 1:0.5~2.
7. method as claimed in claim 4, it is characterised in that step (a) is specially：By what is prepared by micromechanics stripping method
Molybdenum disulfide powder is placed in the mixed liquor of ethanol/water, and at room temperature, ultrasound 3~72 hours, rotating speed is 1000~8000 revs/min
Centrifuged under the conditions of clock, take supernatant liquid, obtained the ethanol/water dispersion liquid of molybdenum disulfide, be evaporated under reduced pressure at 10~50 DEG C and remove second
Dried after alcohol, obtain refined molybdenum disulfide powder, then refined molybdenum disulfide powder is placed in ultra-pure water, ultrasound 5~60 minutes,
The aqueous dispersions of molybdenum disulfide are made.
8. method as claimed in claim 4, it is characterised in that molybdenum disulfide in the described aqueous dispersions of control in step (a)
Concentration is 10~50mg/mL；The solubility of amino acid is 50~200mmol/L in Freamine Ⅲ used in step (b), solvent
For system solution.
9. amino acid as claimed in claim 1 or 2-application of the molybdenum disulfide composite corrosion inhibitor in corrosion inhibition for metal.
10. application as claimed in claim 9, it is characterised in that described metal is copper product.
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| CN201710740879.7A CN107686990B (en) | 2017-08-25 | 2017-08-25 | Amino acid-molybdenum disulfide composite corrosion inhibitor and application thereof |
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| CN201710740879.7A CN107686990B (en) | 2017-08-25 | 2017-08-25 | Amino acid-molybdenum disulfide composite corrosion inhibitor and application thereof |
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2017
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| DD144072A1 (en) * | 1979-05-29 | 1980-09-24 | Friedrich Lohrmann | LUBRICANTS WITH FREEZE PROTECTION |
| US20090324820A1 (en) * | 2008-06-30 | 2009-12-31 | Chartier Douglas M | Systems, Methods, and Compositions for the Inhibition of Corrosion of Metallic Surfaces |
| CN101487124A (en) * | 2008-11-18 | 2009-07-22 | 上海电力学院 | Method for forming arginine self-assembly corrosion inhibition film on copper surface |
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