CN108752927A - A kind of preparation method of cysteine/polyaniline anticorrosion functional material - Google Patents
A kind of preparation method of cysteine/polyaniline anticorrosion functional material Download PDFInfo
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- CN108752927A CN108752927A CN201810395969.1A CN201810395969A CN108752927A CN 108752927 A CN108752927 A CN 108752927A CN 201810395969 A CN201810395969 A CN 201810395969A CN 108752927 A CN108752927 A CN 108752927A
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- cysteine
- polyaniline
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- functional material
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/36—Sulfur-, selenium-, or tellurium-containing compounds
- C08K5/37—Thiols
- C08K5/372—Sulfides, e.g. R-(S)x-R'
- C08K5/3725—Sulfides, e.g. R-(S)x-R' containing nitrogen
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/02—Polyamines
- C08G73/026—Wholly aromatic polyamines
- C08G73/0266—Polyanilines or derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
Abstract
The present invention relates to a kind of preparation method of cysteine/polyaniline anticorrosion functional material, synthetic method is in-situ oxidizing-polymerizing method, is comprised the concrete steps that：Aniline and ethylbenzene are uniformly mixed and are used as hydrophobe, lauryl sodium sulfate dissolving is regard as emulsifier in deionized water, emulsifier is added in hydrophobe, while inhibitor cysteine is added；The mixed solution is sufficiently stirred, makes to be uniformly mixed, ultrasound is carried out during ice bath later, makes emulsifying soln；Adding the aqueous solution of polyvinyl alcohol and being added in mixed solution as stabilizer, after ammonium sulfate is fully dissolved makes its oxidation polymerization, finally by solution centrifugation, washing, the drying after polymerization, obtains product.The method of the present invention can synthesize the nanometer spherical structure of cysteine/polyaniline, the defects of improving bad polyaniline mechanical performance and bad dispersibility, improve the dispersion degree of inhibitor, the release process control of inhibitor, raising anti-corrosion capability is made to be conducive to industrial production.
Description
Technical field
The invention belongs to technical field of material, more particularly, to a kind of cysteine/polyaniline anticorrosion work(
The preparation method of energy material.
Background technology
The considerations of carbon steel is due to economic aspect and excellent performance, such as higher structural strength and mechanical strength,
It is used widely in many industries.But the if feelings that carbon steel touches corrosive solution and do not protect when in use
Under condition, it may occur that heavy corrosion.Corrosion process can cause much to lose, even more so especially in industrial environment.Corrosion is
One continual process, the best approach for solving the problems, such as this are exactly to prevent.
Most universal and cost-effectiveness the best way for corrosion of steel structure protection is to use organic coating, forms one
Physical barriers prevent aggressive substances to be diffused into metal surface, delay its corrosion.In recent years, polyaniline (PANI) is considered as
One of most promising anticorrosion material.Because the better heat stability of polyaniline, machinability and electric conductivity are also fairly good；From
From the point of view of economic angle, polyaniline is more notable to be better than other conducting polymers, because aniline monomer is than other conducting polymers
Monomer is cheap, and the synthesis of polyaniline is very simple, performance is easily adjusted, has many potential application possibilities.But
Polyaniline also has very important defect：Conductivity opposing metallic is relatively low, and their solubilities in all common solvents
Difference and solubility are low.Therefore, by it is modified make polyaniline be preferably applied for anticorrosion field be current research hotspot it
One.
In order to enable organic matter coating to obtain reinforcing and long-term corrosion protection ability, a kind of effective ways are to apply
Inhibition component is mixed in material.Amino acid is easy to produce, is biodegradable, relatively cheap and complete as nontoxic compound
It is dissolved in aqueous medium, therefore is attracted attention as the potential corrosion inhibitor of iron and its alloy.This is because this kind of organise
It closes and is rich in lone pair electrons/pi-electron in object so that it can be adsorbed on metal surface, blocking activity site, to mitigate metal erosion
Harm.One of its reaction mechanism is adsorbed on the metal surface by nitrogen-atoms.If in a kind of structure memory of amino acid
In aromatic rings and hetero atom, such as sulphur atom and nitrogen-atoms, it will dramatically increase its efficiency for inhibiting corrosion.But it is current anti-
Rotten material preparation process process is complex, and Corrosion Protection is to be improved.
Chinese patent CN102732128A discloses a kind of nano polyaniline anticorrosive coating, and matter is pressed by component A and B component
Measure ratio 1~5：1 composition；Wherein, component A：60~95 parts of corrosion-resistant epoxy paint；0.5~10 part of doped polyaniline nanoparticle；
0.5~5 part of diluent；0.5~10 part of dispersant；B component：10~40 parts of curing agent；0.5~5 part of diluent, which passes through
H2O/FeCl2/H2O2System prepares polyaniline, and major defect is little to improving the effect of polyaniline mechanical performance itself, and not
Conducive to the dispersion of inhibitor, the migration of inhibitor is hindered, has certain reduction to the barrier property of polyaniline itself.
Invention content
The purpose of the present invention is improving polyaniline property, solves the problems, such as above, propose a kind of preparation method simply, anti-corrosion
Erosion excellent result and inhibitor discharge the preparation method of controllable cysteine/polyaniline composite nanometer particle, pass through addition
Inhibitor cysteine is modified material, due to the structure with nano particle, is conducive to dispersion and the fortune of inhibitor
It is defeated, discharge process control during anticorrosion.
The purpose of the present invention is achieved through the following technical solutions：
A kind of preparation method of cysteine/polyaniline anticorrosion functional material, using in-situ oxidizing-polymerizing method into
Row synthesis, specifically includes following steps：
(1) aniline and ethylbenzene are uniformly mixed as hydrophobe, make lauryl sodium sulfate dissolving in deionized water
For emulsifier, emulsifier is added in hydrophobe, using cysteine as inhibitor, while being added in mixed solution；
(2) it is thoroughly mixed solution, it is ultrasonic during ice bath after mixing, make its emulsification, obtains microemulsion；
(3) it is added in polyvinyl alcohol water solution and ammonium sulfate solution to microemulsion, carries out oxidation polymerization；
(4) solution after polymerization is centrifuged, washing, dry reaction product are to get to product.
Preferably, mass fraction of the inhibitor cysteine in combination product described in step (1) is 1~5%.Emulsification
Agent lauryl sodium sulfate quality is 62.5mg, and ethylbenzene takes 1.23mL, aniline to take 0.49mL in hydrophobe, is sufficiently mixed uniformly.
Preferably, the ratio between amount of substance of ethylbenzene and aniline is 2 in hydrophobe described in step (1):1.
Preferably, step (2) is stirred at room temperature, time 60-80min, speed of agitator 1000-1300rpm, in ice
It is ultrasonic under the conditions of bath, time 240-300s.
Preferably, the weight percentage of step (3) polyvinyl alcohol water solution is 15wt%, adds 1mL, oxidant over cure
Sour ammonium quality be 1.23g, in 1.67ml deionized waters fully dissolving prepared by.
Preferably, the centrifugation time of step (4) solution is 20-30min, rotating speed 6000-8000rpm, using deionization
Water and the multiple washing reaction product of absolute ethyl alcohol, until supernatant liquid is clarified, then product is true at a temperature of 40-70 DEG C
Sky is dry for 24 hours.
Preferably, step (4) product is the nanosphere of compound, and the diameter range of nanosphere is in 100~300nm.
The present invention is modified material by adding cysteine, is because amino acid is it is verified that in a variety of erosions
Property medium in, can have good and safety corrosion-suppressing effect to various metals, and itself it is nontoxic, biodegradable and
Price is relatively cheap.Cysteine contains the atoms such as N, S, O, in addition to amino and carboxylic group, also having sulfydryl-SH bases
Group.Molecule is anchored to metal surface by sulfydryl by forming mercaptan sat linkage, can delay the cathode of metal erosion by the mechanism
Process.Cysteine and its derivative show excellent corrosion-suppressing effect, and can pass through amino or carboxyl and-SH
It is coordinated, is adsorbed as bidentate ligand.
Compared with prior art, the present invention has the following advantages：
1, preparation process of the present invention is simple, safe, does not generate pollution, harmful substance, does not influence surrounding enviroment.
2, the advanced composite material (ACM) synthesized by the present invention is nanoparticle structure, and preparation process is controllable, uniform particle sizes, can
Certain degree improves the dissolubility of polyaniline in the coating and dispersibility, and it is more preferable that effect is blended with coatings such as resins.
3, the advanced composite material (ACM) for preparing of the present invention, be conducive to the dispersion of inhibitor in the coating, and inhibitor is released
Process control is put, the corrosion protection effect for improving epoxy coating is conducive to.
4, nanometer spherical particle compound material prepared by the present invention, can be effectively improved the defect of polyaniline bad mechanical property,
Improve processing performance so that it can which large-scale application is in industrial production.
Description of the drawings
Fig. 1 is the shape appearance figure of new material prepared by the method for the present invention.
Specific implementation mode
With reference to specific embodiment, the present invention is described in detail, but should be in no way restrictive.
Embodiment 1
0.49mL aniline and 1.23mL ethylbenzene are measured respectively, are mixed evenly, as hydrophobe, are weighed 62.5mg ten
Sodium dialkyl sulfate fully dissolves in 6ml deionized waters, as emulsifier, emulsifier is added in hydrophobic mixture, simultaneously
It weighs 7.5mg cysteines to be added thereto, as inhibitor.Mixed solution is sufficiently stirred at room temperature, and speed of agitator is
1200rpm, mixing time 70min, it is then that mixture is cooling in ice bath, and be ultrasonically treated, the time is 300 seconds, is made
It is emulsified.The polyvinyl alcohol water solution of 15wt% is added into microemulsion, then weighs 1.23g ammonium persulfates, is gone in 1.67mL
It dissolves completely in ionized water, is added dropwise in microemulsion at ambient temperature.After the completion of reaction, repeatedly washed with deionized water,
Until upper solution is clarified.By above-mentioned solution in centrifuge, with the rotating speed high speed centrifugation 25min of 7000rpm, using going
Ionized water and absolute ethyl alcohol clean reaction product repeatedly, are finally dried in vacuo for 24 hours at a temperature of 50 DEG C, you can obtain product.
By the cysteine/polyaniline metal anticorrosion erosion new material and epoxy blend, it is coated in steel disc electrode table
Corrosion Protection is tested in face using three-electrode system, and it is 3.02 × 10 to measure corrosion electric current density-10A/cm2。
Embodiment 2
0.49mL aniline and 1.23mL ethylbenzene are measured respectively, are mixed evenly, as hydrophobe, are weighed 62.5mg ten
Sodium dialkyl sulfate fully dissolves in 6ml deionized waters, as emulsifier, emulsifier is added in hydrophobic mixture, simultaneously
It weighs 15mg cysteines to be added thereto, as inhibitor.Mixed solution is sufficiently stirred at room temperature, and speed of agitator is
1200rpm, mixing time 70min, it is then that mixture is cooling in ice bath, and be ultrasonically treated, the time is 300 seconds, is made
It is emulsified.The polyvinyl alcohol water solution of 15wt% is added into microemulsion, then weighs 1.23g ammonium persulfates, is gone in 1.67mL
It dissolves completely in ionized water, is added dropwise in microemulsion at ambient temperature.After the completion of reaction, repeatedly washed with deionized water,
Until upper solution is clarified.By above-mentioned solution in centrifuge, with the rotating speed high speed centrifugation 25min of 7000rpm, using going
Ionized water and absolute ethyl alcohol clean reaction product repeatedly, are finally dried in vacuo for 24 hours at a temperature of 50 DEG C, you can obtain product.
By the cysteine/polyaniline metal anticorrosion erosion new material and epoxy blend, it is coated in steel disc electrode table
Corrosion Protection is tested in face using three-electrode system, and it is 4.74 × 10 to measure corrosion electric current density-10A/cm2。
Embodiment 3
0.49mL aniline and 1.23mL ethylbenzene are measured respectively, are mixed evenly, as hydrophobe, are weighed 62.5mg ten
Sodium dialkyl sulfate fully dissolves in 6ml deionized waters, as emulsifier, emulsifier is added in hydrophobic mixture, simultaneously
It weighs 22.5mg cysteines to be added thereto, as inhibitor.Mixed solution is sufficiently stirred at room temperature, and speed of agitator is
1200rpm, mixing time 70min, it is then that mixture is cooling in ice bath, and be ultrasonically treated, the time is 300 seconds, is made
It is emulsified.The polyvinyl alcohol water solution of 15wt% is added into microemulsion, then weighs 1.23g ammonium persulfates, is gone in 1.67mL
It dissolves completely in ionized water, is added dropwise in microemulsion at ambient temperature.After the completion of reaction, repeatedly washed with deionized water,
Until upper solution is clarified.By above-mentioned solution in centrifuge, with the rotating speed high speed centrifugation 25min of 7000rpm, using going
Ionized water and absolute ethyl alcohol clean reaction product repeatedly, are finally dried in vacuo for 24 hours at a temperature of 50 DEG C, you can obtain product.
By the cysteine/polyaniline metal anticorrosion erosion new material and epoxy blend, it is coated in steel disc electrode table
Corrosion Protection is tested in face using three-electrode system, and it is 2.75 × 10 to measure corrosion electric current density-9A/cm2。
Embodiment 4
0.49mL aniline and 1.23mL ethylbenzene are measured respectively, are mixed evenly, as hydrophobe, are weighed 62.5mg ten
Sodium dialkyl sulfate fully dissolves in 6ml deionized waters, as emulsifier, emulsifier is added in hydrophobic mixture, simultaneously
It weighs 30mg cysteines to be added thereto, as inhibitor.Mixed solution is sufficiently stirred at room temperature, and speed of agitator is
1200rpm, mixing time 70min, it is then that mixture is cooling in ice bath, and be ultrasonically treated, the time is 300 seconds, is made
It is emulsified.The polyvinyl alcohol water solution of 15wt% is added into microemulsion, then weighs 1.23g ammonium persulfates, is gone in 1.67mL
It dissolves completely in ionized water, is added dropwise in microemulsion at ambient temperature.After the completion of reaction, repeatedly washed with deionized water,
Until upper solution is clarified.By above-mentioned solution in centrifuge, with the rotating speed high speed centrifugation 25min of 7000rpm, using going
Ionized water and absolute ethyl alcohol clean reaction product repeatedly, are finally dried in vacuo for 24 hours at a temperature of 50 DEG C, you can obtain product.
By the cysteine/polyaniline metal anticorrosion erosion new material and epoxy blend, it is coated in steel disc electrode table
Corrosion Protection is tested in face using three-electrode system, and it is 7.72 × 10 to measure corrosion electric current density-10A/cm2。
Embodiment 5
0.49mL aniline and 1.23mL ethylbenzene are measured respectively, are mixed evenly, as hydrophobe, are weighed 62.5mg ten
Sodium dialkyl sulfate fully dissolves in 6ml deionized waters, as emulsifier, emulsifier is added in hydrophobic mixture, simultaneously
It weighs 37.5mg cysteines to be added thereto, as inhibitor.Mixed solution is sufficiently stirred at room temperature, and speed of agitator is
1200rpm, mixing time 70min, it is then that mixture is cooling in ice bath, and be ultrasonically treated, the time is 300 seconds, is made
It is emulsified.The polyvinyl alcohol water solution of 15wt% is added into microemulsion, then weighs 1.23g ammonium persulfates, is gone in 1.67mL
It dissolves completely in ionized water, is added dropwise in microemulsion at ambient temperature.After the completion of reaction, repeatedly washed with deionized water,
Until upper solution is clarified.By above-mentioned solution in centrifuge, with the rotating speed high speed centrifugation 25min of 7000rpm, using going
Ionized water and absolute ethyl alcohol clean reaction product repeatedly, are finally dried in vacuo for 24 hours at a temperature of 50 DEG C, you can obtain product.
By the cysteine/polyaniline metal anticorrosion erosion new material and epoxy blend, it is coated in steel disc electrode table
Corrosion Protection is tested in face using three-electrode system, and it is 4.97 × 10 to measure corrosion electric current density-10A/cm2。
Claims (7)
1. a kind of preparation method of cysteine/polyaniline anticorrosion functional material, which is characterized in that use in-situ oxidation
Polymerization is synthesized, and following steps are specifically included：
(1) aniline and ethylbenzene are uniformly mixed as hydrophobe, regard lauryl sodium sulfate dissolving as breast in deionized water
Emulsifier is added in hydrophobe, using cysteine as inhibitor, while being added in mixed solution by agent；
(2) it is thoroughly mixed solution, it is ultrasonic during ice bath after mixing, make its emulsification, obtains microemulsion；
(3) it is added in polyvinyl alcohol water solution and ammonium sulfate solution to microemulsion, carries out oxidation polymerization；
(4) solution after polymerization is centrifuged, washing, dry reaction product are to get to product.
2. a kind of preparation method of cysteine according to claim 1/polyaniline anticorrosion functional material, special
Sign is that mass fraction of the cysteine in combination product described in step (1) is 1~5%.
3. a kind of preparation method of cysteine according to claim 1/polyaniline anticorrosion functional material, special
Sign is that the ratio between amount of substance of ethylbenzene and aniline is 2 in hydrophobe described in step (1):1.
4. a kind of preparation method of cysteine according to claim 1/polyaniline anticorrosion functional material, special
Sign is that step (2) is stirred at room temperature, time 60-80min, speed of agitator 1000-1300rpm, under condition of ice bath
Ultrasound, time 240-300s.
5. a kind of preparation method of cysteine according to claim 1/polyaniline anticorrosion functional material, special
Sign is that the weight percentage of step (3) polyvinyl alcohol water solution is 15wt%.
6. a kind of preparation method of cysteine according to claim 1/polyaniline anticorrosion functional material, special
Sign is, the centrifugation time of step (4) solution is 20-30min, rotating speed 6000-8000rpm, using deionized water and anhydrous
The multiple washing reaction product of ethyl alcohol, until supernatant liquid is clarified, then product is dried in vacuo at a temperature of 40-70 DEG C
24h。
7. a kind of preparation method of cysteine according to claim 1/polyaniline anticorrosion functional material, special
Sign is that step (4) product is nanosphere, and the diameter range of nanosphere is in 100~300nm.
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| CN102702518A (en) * | 2012-06-28 | 2012-10-03 | 山东大学 | Method for preparing composite material of stannic oxide/polyaniline |
| CN102732128A (en) * | 2012-07-04 | 2012-10-17 | 苏州义创新材料科技有限公司 | Nanometer polyaniline anticorrosive coating and preparation method therefor |
| CN103232597A (en) * | 2013-04-28 | 2013-08-07 | 同济大学 | 2-mercapto benzimidazole/polyaniline anticorrosion composite material and preparation method thereof |
| CN103849295A (en) * | 2014-03-27 | 2014-06-11 | 四川理工学院 | Phthalocyanine-based sulfonic acid-doped polyaniline anticorrosive paint |
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2018
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| WO2008143735A2 (en) * | 2007-03-05 | 2008-11-27 | Scott Hayes | Multi-layer and composite corrosion resistant coatings |
| CN101497755A (en) * | 2009-02-24 | 2009-08-05 | 山东大学 | Environment friendly anti-corrosive paint and preparation thereof |
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Application publication date: 20181106 |