CN109825836A - A kind of derusting and anti-corrosion protection method of bronze ware - Google Patents
A kind of derusting and anti-corrosion protection method of bronze ware Download PDFInfo
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- CN109825836A CN109825836A CN201910096492.1A CN201910096492A CN109825836A CN 109825836 A CN109825836 A CN 109825836A CN 201910096492 A CN201910096492 A CN 201910096492A CN 109825836 A CN109825836 A CN 109825836A
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Abstract
The present invention provides a kind of derusting of bronze ware and anti-corrosion protection methods, comprising: S1, prepare corrosion inhibitor solution: the corrosion inhibitor solution includes aminotrimethylenephosphonic acid, acylate, azole heterocyclic compound, and solvent is second alcohol and water；S2, bronze ware is immersed into the ethanol solution that mass fraction is 10~30% surfactants, 10~30min of ultrasound in ultrasonic oscillator；S3, bronze ware is taken out, corrosion inhibitor solution is sprayed to bronze surface using aerosol dispenser, with 20~200mL/m2The speed of/min sprays；S4, bronze ware after reaction is cleaned with ethanol solution, dried.Method is easy to operate, derusting speed is fast, does not damage the bronze part surface-brightening after bronze part substrate, derusting, and antirust time can meet historical relic's protection and the requirement of archaeological circle up to 3 months or more.
Description
Technical field
The invention belongs to historical relic's protection fields, are related to metal product aseptic technic more particularly to a kind of derusting of bronze ware
And anti-corrosion protection method.
Background technique
Bronze ware is a great invention in human history, has very high artistic value and historical value.However, by
Corrosion is easy to happen in humid air in bronze material itself, bronze ware, which is unearthed, in addition goes to toward in land burial centuries
Or even more than one thousand years, make it by different degrees of damage and corrosion, wherein bronzed disease is that the maximum a kind of Special Corrosion of harm is existing
As, it is harmful patina on bronze ware and air and moisture interaction cyclic corrosion makes bronze ware corrosion until dusting, and
With infectiousness.Bronze ware once catches bronzed disease, and sprawling and development will be difficult to control, and gently then causes the inscription of bronze surface
The important history archaeological information such as text, pattern destroys and keeps antique value severely damaged, heavy then so that implements is festered and perforate very
Disintegrate to complete, this makes bronze ware be faced with severe anti-corrosion protection problem.
For the processing of rust removing of bronze surface, there are three types of modes at present: mechanical derusting, chemical derusting, electrochemistry derust.
Wherein, chemical derusting is handled because its easy to operate, at low cost and effect is good, using than wide.But current usedization
It learns in derusting method, largely uses acid solution, rust removing solution that can cause to damage to bronze ware itself, and the surface after derusting holds very much
Easily it is corroded again.Chinese patent CN201610928827.8 discloses a kind of surface hydrophobicity rust-proofing method of bronze bronze drum,
The based superhydrophobic thin films of bronze bronze drum surface building layer of transparent, have preferable anti-corrosion effect.But this method need to be super in building
Mechanical grinding first is carried out to bronze bronze drum before hydrophobic film, Film forming operations are comparatively laborious, and time-consuming.Chinese patent
CN201410570635.5 discloses a kind of chemical polishing agent and its application, and speed is fast, polishing effect is good, rust-proof life is longer, but
Catalyst need to be added and promote the progress of derusting polishing process using a large amount of auxiliary agent.
Summary of the invention
It is an object of the invention to: in view of the above-mentioned problems, proposing the derusting and anti-corrosion protection method of a kind of bronze ware, inhibition
Agent solution ingredient is simple, and this method can effectively remove rapidly the harmful patina of bronze surface, and be formed on its surface colorless and transparent
Protective film, effectively prevent bronze surface to be further corroded.
The technical solution adopted by the invention is as follows:
A kind of derusting and anti-corrosion protection method of bronze ware, comprising the following steps:
S1, prepare corrosion inhibitor solution: the corrosion inhibitor solution includes aminotrimethylenephosphonic acid, acylate, azole heterocycle
Compound, solvent are second alcohol and water；
S2, bronze ware is immersed into the ethanol solution that mass fraction is 10~30% surfactants, in ultrasonic oscillator
Middle ultrasonic 10~30min；
S3, bronze ware is taken out, corrosion inhibitor solution is sprayed to bronze surface using aerosol dispenser, with 20~200mL/
m2The speed of/min sprays；
S4, bronze ware after reaction is cleaned with ethanol solution, dried.
The present invention matches aminotrimethylenephosphonic acid, acylate, azole heterocyclic compound, utilizes three methene of amino
Phosphonic acids, acylate to the chelation of metal and its ion, the hetero atoms such as N, O, S contained in conjunction with azole heterocyclic compound with
Metal forms stable conjugation complex compound, and each component plays synergistic effect, forms one layer of fine and close transparent guarantor in bronze surface
Cuticula.Bronze surface is handled using surfactant first, provides more active sites for subsequent corrosion inhibiter；Fortune
Corrosion inhibiter, is atomized into small drop, the corrosion and surface-active with bronze surface by the method sprayed with aerosol dispenser
The active site that agent provides comes into full contact with, and shortens the reaction time, forms more closer protective films in bronze surface.Make
It uses ethanol solution as the solvent of corrosion inhibiter, the solubility of corrosion inhibiter on the one hand can be improved, on the other hand can also improve slow
The stability for losing agent, keeps the effect of derusting anti-corrosive.Corrosion inhibiter provided by the invention and method, collective effect improve remove at double
Corrosion-resistant speed of becoming rusty and ability.
Further, the acylate include one of sodium citrate, sodium gluconate, sodium lactate, sodium acetate or
It is a variety of.
Further, the azole heterocyclic compound includes 2- heptadecyl imidazole, methyl benzotriazazole, carboxyl benzo
One of triazole, benzothiazole, 2-mercaptobenzothiazole, 2- mercaptobenzoxazole are a variety of.
Further, each material mass score in the corrosion inhibitor solution: aminotrimethylenephosphonic acid 1~8%, acylate
5~10%, azole heterocyclic compound 0.5~5%, surplus is solvent.
Further, each material mass score in the corrosion inhibitor solution: aminotrimethylenephosphonic acid 2~5%, acylate
6~8%, azole heterocyclic compound 1~2.6%, surplus is solvent.
Further, the preparation method of the corrosion inhibitor solution are as follows: weigh aminotrimethylenephosphonic acid by weight percentage, have
Machine hydrochlorate, azole heterocyclic compound, second alcohol and water, are then heated to 30~60 DEG C, accelerate the dissolution of corrosion inhibiter.
Further, the mass fraction of ethyl alcohol is 10%~50% in solvent described in step S1.
Further, lemon acid for adjusting pH is added to 6.0~7.0 in the corrosion inhibitor solution.
Further, the surfactant is nonylphenol polyoxyethylene ether and/or nonylphenol polyoxyethylene ether sulfuric acid
Ammonium and/or fatty alcohol polyoxyethylene ether ammonium sulfate, while being activated to bronze surface, moreover it is possible to play emulsification, dispersion inhibition
The effect of agent promotes the removal of bronze surface rusty stain and the formation of rust-preventing film.
Further, the ultrasonic oscillator power is 200~300W.
It is obtained by the present invention to have the beneficial effect that:
1, aminotrimethylenephosphonic acid, acylate, a variety of corrosion inhibitor compounds of azole heterocyclic compound match, and accelerate
The complexing of bronze surface corrosion, and react mild, derusting ability promoted at double；
2, bronze ware is pre-processed using surfactant, imparts the more active sites of bronze surface, it can
It is reacted with more corrosion inhibiter；
3, corrosion inhibitor solution is atomized into tiny drop, increases the contact area of corrosion inhibiter and bronze surface, adds
The progress of speed reaction, corrosion inhibitor solution dosage reduce, and derust more thorough, and can form finer and close protective film；
4, the protective film that transparent light is formed on the surface of bronze ware can also play polishing while playing passivation anti-corrosion
Effect；By the processed bronze ware of the method for the present invention, surface-brightening, the anti-corrosion time is long, the anti-corrosion phase can reach 3 months with
On；
5, corrosion inhibiter stability of the invention is strong, and method is simple, strong operability, will not cause to damage to bronze substrate,
Descaling process is environment friendly and pollution-free.
6, the present invention can easily and quickly remove the harmful patina of Bronze Relics, and transparent its inscription and decorative pattern can be kept clear
As it can be seen that historical relic's protection and the requirement of archaeological circle can be met.
Specific embodiment
The technical solution in the embodiment of the present invention will be clearly and completely described below, it is clear that described reality
Applying example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is general
Logical technical staff every other embodiment obtained without making creative work belongs to what the present invention protected
Range.
The bronze sample preparation of simulation band rust: size is cut from from casting bronze test specimen modelled after an antique using electro-spark cutting machine are as follows:
10cm × 10cm × 1cm sample is several, by its surface respectively in order with 80 mesh, 180 mesh, 240 mesh, 320 mesh sand paper into
Row polishing, after surface is polished light, is cleaned with acetone, uses dehydrated alcohol degreasing afterwards, dry.Then it is dripped on sample
Add a certain amount of 0.1mol/L HCl+2mol/L H2O2Mixed aqueous solution then obtained in air with 28 DEG C of heating water bath 18h
The bronze sample of band rust.
Embodiment 1:
A kind of derusting and anti-corrosion protection method of bronze ware, comprising the following steps:
S1, prepare corrosion inhibitor solution: weighing 0.1kg aminotrimethylenephosphonic acid, 0.5kg sodium citrate, 0.2kg 2- 17
Alkyl imidazole, 0.5kg ethyl alcohol and 4.1kg water are then heated to 30 DEG C and stirring and dissolving, and lemon acid for adjusting pH is added to 6.5；
S2, the nonylphenol polyoxyethylene ether ethanol solution that mass fraction is 10% will be immersed with the bronze sample that becomes rusty, in ultrasound
Ultrasound 30min makes sample surfaces activate to form active group in wave oscillator；
Corrosion inhibitor solution is sprayed to sample surfaces using aerosol dispenser by S3, taking-up sample, with the speed of 30mL/min
Spray 25min；
S4, sample after reaction is cleaned with ethanol solution, remove the corrosion inhibitor solution of surface attachment, be subsequently placed in certainly
Right ventilation is dried, i.e., forms colorless and transparent film in sample surfaces.
Historical relic bronze ware will be changed into the bronze sample that becomes rusty, handled according to the above method.
Embodiment 2:
A kind of derusting and anti-corrosion protection method of bronze ware, comprising the following steps:
S1, prepare corrosion inhibitor solution: weighing 0.45kg aminotrimethylenephosphonic acid, 0.3kg sodium citrate, 0.05kg 2- ten
Seven alkyl imidazoles, 0.05kg methyl benzotriazazole, 2.5kg ethyl alcohol and 2.5kg water are heated in 40 DEG C of water-bath and are stirred molten
Lemon acid for adjusting pH is added to 6.0 in solution；
S2, the nonylphenol polyoxyethylene ether ammonium sulfate ethanol solution that mass fraction is 20% will be immersed with the bronze sample that becomes rusty,
It activates sample surfaces to form active group with 300W power ultrasound 10min in ultrasonic oscillator；
S3, sample is taken out, using aerosol dispenser with 50mL/m2The speed of/min, which is sprayed, is sprayed to sample for corrosion inhibitor solution
Product surface sprays 20min；
S4, sample after reaction is cleaned with ethanol solution, remove the corrosion inhibitor solution of surface attachment, be subsequently placed in certainly
Right ventilation is dried, i.e., forms colorless and transparent film in sample surfaces.
Historical relic bronze ware will be changed into the bronze sample that becomes rusty, handled according to the above method.
Embodiment 3:
A kind of derusting and anti-corrosion protection method of bronze ware, comprising the following steps:
S1, prepare corrosion inhibitor solution: weighing 0.15kg aminotrimethylenephosphonic acid, 0.45kg sodium citrate, 0.025kg carboxyl
Benzotriazole, 0.025kg 2- mercaptobenzoxazole, 2kg ethyl alcohol and 3.2kg water, heat in 50 DEG C of water-bath and stir molten
Lemon acid for adjusting pH is added to 6.5 in solution；
S2, nonylphenol polyoxyethylene ether, the nonyl that surfactant total mass fraction is 30% will be immersed with the bronze sample that becomes rusty
Base phenol polyethenoxy ether ammonium sulfate, fatty alcohol polyoxyethylene ether ammonium sulfate (three's mass ratio is 1:1:1) ethanol solution, in ultrasound
It activates sample surfaces to form active group with 200W power ultrasound 20min in wave oscillator；
S3, sample is taken out, using aerosol dispenser with 100mL/m2Corrosion inhibitor solution is sprayed to sample by the speed of/min
Surface sprays 10min；
S4, sample after reaction is cleaned with ethanol solution, remove the corrosion inhibitor solution of surface attachment, be subsequently placed in certainly
Right ventilation is dried, i.e., forms colorless and transparent film in sample surfaces.
Historical relic bronze ware will be changed into the bronze sample that becomes rusty, handled according to the above method.
Embodiment 4:
A kind of derusting and anti-corrosion protection method of bronze ware, comprising the following steps:
S1, prepare corrosion inhibitor solution: weighing 0.25kg aminotrimethylenephosphonic acid, 0.35kg sodium citrate, 0.05kg benzo
Thiazole, 0.05kg 2-mercaptobenzothiazole, 0.05kg 2- mercaptobenzoxazole, 1.05kg ethyl alcohol and 4.05kg water, at 55 DEG C
Water-bath in heating and stirring and dissolving, lemon acid for adjusting pH is added to 6.2；
S2, the nonylphenol polyoxyethylene ether sulfuric acid that surfactant total mass fraction is 25% will be immersed with the bronze sample that becomes rusty
Ammonium, fatty alcohol polyoxyethylene ether ammonium sulfate (the two mass ratio is 2:1) ethanol solution, with 250W power in ultrasonic oscillator
Ultrasonic 15min makes sample surfaces activate to form active group；
S3, sample is taken out, using aerosol dispenser with 80mL/m2Corrosion inhibitor solution is sprayed to sample table by the speed of/min
Face sprays 15min；
S4, sample after reaction is cleaned with ethanol solution, remove the corrosion inhibitor solution of surface attachment, be subsequently placed in certainly
Right ventilation is dried, i.e., forms colorless and transparent film in sample surfaces.
Historical relic bronze ware will be changed into the bronze sample that becomes rusty, handled according to the above method.
Embodiment 5:
A kind of derusting and anti-corrosion protection method of bronze ware, comprising the following steps:
S1, prepare corrosion inhibitor solution: weighing 0.2kg aminotrimethylenephosphonic acid, 0.41kg sodium citrate, 0.12kg methylbenzene
And triazole, 0.06kg benzothiazole, 0.05kg 2-mercaptobenzothiazole, 0.06kg2- mercaptobenzoxazole, 1.55kg ethyl alcohol
With 3.55kg water, lemon acid for adjusting pH is added to 6.8 in heating and stirring and dissolving in 45 DEG C of water-bath；
S2, nonylphenol polyoxyethylene ether, the rouge that surfactant total mass fraction is 15% will be immersed with the bronze sample that becomes rusty
Fat alcohol polyoxyethylene ether ammonium sulfate (the two mass ratio is 1.5:1) ethanol solution is super with 220W power in ultrasonic oscillator
Sound 12min makes sample surfaces activate to form active group；
S3, sample is taken out, using aerosol dispenser with 150mL/m2The speed of/min uses aerosol dispenser by corrosion inhibiter
Solution spraying sprays 5min to sample surfaces；
S4, sample after reaction is cleaned with ethanol solution, remove the corrosion inhibitor solution of surface attachment, be subsequently placed in certainly
Right ventilation is dried, i.e., forms colorless and transparent film in sample surfaces.
Historical relic bronze ware will be changed into the bronze sample that becomes rusty, handled according to the above method.
Embodiment 6:
A kind of derusting and anti-corrosion protection method of bronze ware, comprising the following steps:
S1, prepare corrosion inhibitor solution: weighing 0.13kg aminotrimethylenephosphonic acid, 0.42kg sodium citrate, 0.02kg methyl
Benzotriazole, 0.02kg carboxy benzotriazole, 0.02kg benzothiazole, 0.03kg2- mercaptobenzothiazoler, 0.03kg 2-
Mercaptobenzoxazole, 1.3kg ethyl alcohol and 3.9kg water, heating and stirring and dissolving in 35 DEG C of water-bath, are added lemon acid for adjusting pH
To 7.0, and keep the temperature spare；
S2, nonylphenol polyoxyethylene ether, the nonyl that surfactant total mass fraction is 18% will be immersed with the bronze sample that becomes rusty
Base phenol polyethenoxy ether ammonium sulfate (the two mass ratio is 1:1) ethanol solution, with 200W power ultrasound in ultrasonic oscillator
18min makes sample surfaces activate to form active group, dries；
S3, sample is taken out, using aerosol dispenser with 90mL/m2Corrosion inhibitor solution is sprayed to sample table by the speed of/min
Face sprays 8min；
S4, sample after reaction is cleaned with ethanol solution, remove the corrosion inhibitor solution of surface attachment, be subsequently placed in certainly
Right ventilation is dried, i.e., forms colorless and transparent film in sample surfaces.
Historical relic bronze ware will be changed into the bronze sample that becomes rusty, handled according to the above method.
Following comparative example is carried out according to the experiment parameter of embodiment 5.
Comparative example 1:
Bronze sample is become rusty as experimental subjects using band, removes step S2, other experiment parameters are the same as embodiment 5.
Comparative example 2:
Bronze sample is become rusty as experimental subjects using band, and step S3 is changed to sample immersing 5min in corrosion inhibitor solution, other realities
Parameter is tested with embodiment 5.
Comparative example 3:
Bronze sample is become rusty as experimental subjects using band, removes step S2, step S3 is changed to sample immersing corrosion inhibitor solution
5min, other experiment parameters are the same as embodiment 5.
Comparative example 4:
Bronze sample is become rusty as experimental subjects using band, removal step S2, sprays surfactant addition corrosion inhibitor solution together
Leaching, other experiment parameters are the same as embodiment 5.
Comparative example 5:
Bronze sample is become rusty as experimental subjects using band, removes the aminotrimethylenephosphonic acid in step S1, other experiment parameters are same
Embodiment 5.
Comparative example 6:
Bronze sample is become rusty as experimental subjects using band, removes the sodium citrate in step S1, the same embodiment of other experiment parameters
5。
Comparative example 7:
Bronze sample is become rusty as experimental subjects using band, removes the azole compounds in step S1, other experiment parameters are same to be implemented
Example 5.
In neutral salt spray test method (GBT2015-1997) to the bronze ware antirust of Examples 1 to 6 and comparative example 1~7
Performance is tested, and experimental data is listed in table 1.
Table 1
Table 1 statistics indicate that, Examples 1 to 6 can to bronze part derust completely, cannot derust with comparative example 1~6
Entirely, comparative example 7 can derust completely but rust-proof life is shorter than method of the invention very much.Lack surfactant (comparative example 1),
Without using aerosol dispenser spraying (comparative example 2), not only lacks surfactant but also do not use aerosol dispenser spraying (comparative example
3), surfactant is not submerged initially in bronze part surface (comparative example 4) can influence derusting effect to a certain extent；Especially go
In addition to step S2 and do not use aerosol dispenser spray corrosion inhibiter comparative example 3 method, handle after bronze part there are still big
Rusty stain is measured, illustrates first to be used in combination and could effectively derust rapidly with surfactant ultrasound, again with aerosol dispenser spray, and
It is long-term to keep derusting effect；Lack aminotrimethylenephosphonic acid (comparative example 5), lack azole compounds (comparative example 7) can be one
Determine to influence derusting effect in degree, lacks organic salt (comparative example 6) although can also derust complete its anti-corrosion effect decline very
More, illustrating that aminotrimethylenephosphonic acid, organic salt, azole compounds need to match can be only achieved optimal derusting anti-corrosive effect.
Statistics indicate that method of the invention has, easy to operate, derusting speed is fast, rust-proof life is long, does not damage bronze part substrate, removes for these
The characteristics of bronze part surface-brightening after rust, antirust time transparent can make its inscription and decorative pattern clearly may be used up to 3 months or more
See, historical relic's protection and the requirement of archaeological circle can be met.
Finally, it should be noted that the foregoing is only a preferred embodiment of the present invention, it is not intended to restrict the invention,
Although the present invention is described in detail referring to the foregoing embodiments, for those skilled in the art, still may be used
To modify the technical solutions described in the foregoing embodiments or equivalent replacement of some of the technical features,
All within the spirits and principles of the present invention, any modification, equivalent replacement, improvement and so on should be included in of the invention
Within protection scope.
Claims (10)
1. the derusting and anti-corrosion protection method of a kind of bronze ware, which comprises the following steps:
S1, prepare corrosion inhibitor solution: the corrosion inhibitor solution includes aminotrimethylenephosphonic acid, acylate, azole heterocyclic compound
Object, solvent are second alcohol and water；
S2, bronze ware is immersed into the ethanol solution that mass fraction is 10~30% surfactants, surpassed in ultrasonic oscillator
10~30min of sound；
S3, bronze ware is taken out, using aerosol dispenser with 20~200mL/m2Corrosion inhibitor solution is sprayed to bronze by the speed of/min
Device surface；
S4, bronze ware after reaction is cleaned with ethanol solution, dried.
2. the derusting and anti-corrosion protection method of bronze ware as described in claim 1, which is characterized in that the acylate includes
One of sodium citrate, sodium gluconate, sodium lactate, sodium acetate are a variety of.
3. the derusting and anti-corrosion protection method of bronze ware as described in claim 1, which is characterized in that the azole heterocyclic compound
Object includes 2- heptadecyl imidazole, methyl benzotriazazole, carboxy benzotriazole, benzothiazole, 2-mercaptobenzothiazole, 2-
One of mercaptobenzoxazole is a variety of.
4. the derusting and anti-corrosion protection method of bronze ware as described in claim 1, which is characterized in that in the corrosion inhibitor solution
Each material mass score: aminotrimethylenephosphonic acid 1~8%, acylate 5~10%, azole heterocyclic compound 0.5~5% are remaining
Amount is solvent.
5. the derusting and anti-corrosion protection method of bronze ware as claimed in claim 4, which is characterized in that in the corrosion inhibitor solution
Each material mass score: aminotrimethylenephosphonic acid 2~5%, acylate 6~8%, azole heterocyclic compound 1~2.6% are remaining
Amount is solvent.
6. the derusting and anti-corrosion protection method of bronze ware as described in claim 1, which is characterized in that the corrosion inhibitor solution
Preparation method are as follows: weigh aminotrimethylenephosphonic acid, acylate, azole heterocyclic compound, second alcohol and water by mass percentage, so
After be heated to 30~60 DEG C and make it dissolve.
7. the derusting and anti-corrosion protection method of bronze ware as described in claim 1, which is characterized in that solvent described in step S1
The mass fraction of middle ethyl alcohol is 10%~50%.
8. the derusting and anti-corrosion protection method of bronze ware as described in claim 1, which is characterized in that the corrosion inhibitor solution adds
Enter lemon acid for adjusting pH to 6.0~7.0.
9. the derusting and anti-corrosion protection method of bronze ware as described in claim 1, which is characterized in that the surfactant is
Nonylphenol polyoxyethylene ether and/or nonylphenol polyoxyethylene ether ammonium sulfate and/or fatty alcohol polyoxyethylene ether ammonium sulfate.
10. the derusting and anti-corrosion protection method of bronze ware as claimed in any one of claims 1-9 wherein, which is characterized in that described
Ultrasonic oscillator power is 200~300W.
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| CN112626532A (en) * | 2020-12-09 | 2021-04-09 | 苏州帝航防护设施有限公司 | Metal surface degreasing agent and treatment process thereof |
| CN113106460A (en) * | 2021-04-15 | 2021-07-13 | 深圳市钝化技术有限公司 | High-temperature-resistant conductive copper alloy protective agent, preparation method and copper alloy passivation method |
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| CN114086191A (en) * | 2021-11-11 | 2022-02-25 | 浙江福达合金材料科技有限公司 | Soaking agent for preventing copper from being adhered to surface of rivet electrical contact and application of soaking agent |
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