CN108048853B - Polyaniline/salicylide modification of chitosan corrosion inhibiter preparation method - Google Patents
Polyaniline/salicylide modification of chitosan corrosion inhibiter preparation method Download PDFInfo
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- CN108048853B CN108048853B CN201810000400.0A CN201810000400A CN108048853B CN 108048853 B CN108048853 B CN 108048853B CN 201810000400 A CN201810000400 A CN 201810000400A CN 108048853 B CN108048853 B CN 108048853B
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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
- C23F11/10—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 using organic inhibitors
- C23F11/14—Nitrogen-containing compounds
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Abstract
Polyaniline/salicylide modification of chitosan corrosion inhibiter preparation method, a certain amount of chitosan is dissolved in acetic acid solution first, then, a certain amount of salicylide ethanol solution is added thereto, under conditions of heating and stirring, the regular hour is reacted up to salicylide modification of chitosan；Sequentially add a certain amount of aniline and a certain amount of sulfamic acid thereto again, after the solution is stirred and evenly mixed, the acetic acid solution of a certain amount of ammonium persulfate is added in the mixed liquor, after reaction, it is filtered, washed, filtration cakes torrefaction, polyaniline/salicylide modification of chitosan corrosion inhibiter can be obtained.
Description
Technical field
The invention belongs to metal corrosion and protection fields, and in particular to the technology of preparing of corrosion inhibiter, i.e. polyaniline/salicylide
The technology of preparing of modification of chitosan corrosion inhibiter.
Background technique
Currently, addition corrosion inhibiter is a kind of effective, anti-corrosion means of remarkable in economical benefits.Early stage is common inorganic slow
Losing agent can form one layer of insoluble protective film in metal surface and then hinder destruction of the corrosive medium to metal.But it is inorganic slow
The disadvantage of erosion agent maximum is exactly that the harm to environment and human body is larger and the required concentration that works is larger, and early stage is common organic slow
Losing agent is mainly organic phosphorus compound, and the environment such as eutrophication are also caused while bad to metal coating in practical applications and are asked
Topic, therefore find the research hotspot that green natural organic inhibitor has become corrosion science.
Chitosan is a kind of natural polymer, includes hetero atom (N and O) in structure, provided orphan is to electricity
Son has stronger adsorption capacity to metal, but since its molecular weight is larger, so that its dissolubility in water is poor.
Summary of the invention
The present invention is polyaniline/salicylide modification of chitosan corrosion inhibiter preparation method, be the steps include:
(1) at room temperature, 0.35mol/L acetic acid solution is added chitosan into first, so that chitosan and acetic acid solution
Mass ratio is 1:120 ~ 250, and under stirring, chitosan is dissolved 1 ~ 4h in acetic acid solution；Then, molten to the acetic acid of the chitosan
The ethanol solution containing salicylide is added in liquid, makes mass ratio 1:4 ~ 8 of chitosan and salicylide, controls and speed is added, 0.5
It is added in ~ 1h, then, is heated to 30 ~ 80oC, reacts 4 ~ 8h, obtain salicylide modification of chitosan；
(2) then, aniline, sulfamic acid at 5 DEG C, are sequentially added in Xiang Shangshu reaction system, makes chitosan and aniline
Mass ratio be 1:5 ~ 10, make molar ratio 1:1 ~ 5 of aniline and sulfamic acid, add the acetic acid solution containing ammonium persulfate
As initiator mixed solution, make molar ratio 1:0.5 ~ 2 of aniline and ammonium persulfate, control is added speed, adds in 0.5 ~ 1h
It is complete, then, 4 ~ 8h is reacted, polyaniline/salicylide modification of chitosan corrosion inhibiter is obtained.
Usefulness of the present invention is: preparing corrosion inhibiter by salicylide modification of chitosan, on the one hand solves chitosan
On the other hand the shortcomings that poorly water-soluble, improves the corrosion inhibiter to the anticorrosion efficiency of metal.Contained electricity is negative in polyaniline structure
Property biggish N polar group, the pi-electron in lone pair electrons and conjugated structure provided can form with metal sky d track and be coordinated
Key is adsorbed on metal surface, while the non-polar group in polyaniline structure forms hydrophobic layer in metal surface and then hinders metal
Corrosion rate.Therefore by the way that polyaniline and salicylide modification of chitosan are carried out the compound chitosan dissolubility difference of both having solved
Disadvantage combines the excellent corrosion inhibition of polyaniline again, so that composite corrosion inhibitor has good guarantor to metal under low concentration
Shield effect, at the same it is very little to the harm of environment, it is a kind of environmentally friendly green corrosion inhibitor.Therefore the corrosion inhibiter is to metal
Protection have biggish application market and researching value.
Specific embodiment
The present invention is polyaniline/salicylide modification of chitosan corrosion inhibiter preparation method, be the steps include:
(1) at room temperature, 0.35mol/L acetic acid solution is added chitosan into first, so that chitosan and acetic acid solution
Mass ratio is 1:120 ~ 250, and under stirring, chitosan is dissolved 1 ~ 4h in acetic acid solution；Then, molten to the acetic acid of the chitosan
The ethanol solution containing salicylide is added in liquid, makes mass ratio 1:4 ~ 8 of chitosan and salicylide, controls and speed is added, 0.5
It is added in ~ 1h, then, is heated to 30 ~ 80oC, reacts 4 ~ 8h, obtain salicylide modification of chitosan；
(2) then, aniline, sulfamic acid at 5 DEG C, are sequentially added in Xiang Shangshu reaction system, makes chitosan and aniline
Mass ratio be 1:5 ~ 10, make molar ratio 1:1 ~ 5 of aniline and sulfamic acid, add the acetic acid solution containing ammonium persulfate
As initiator mixed solution, make molar ratio 1:0.5 ~ 2 of aniline and ammonium persulfate, control is added speed, adds in 0.5 ~ 1h
It is complete, then, 4 ~ 8h is reacted, polyaniline/salicylide modification of chitosan corrosion inhibiter is obtained.
The present invention is further spread out below by embodiment.
Embodiment 1:
At room temperature, 0.2g chitosan is added in 48.0g 0.35mol/L acetic acid solution, under stirring, chitosan is existed
1h is dissolved in acetic acid solution,；Then, the ethanol solution containing 1.0g salicylide, control are added into the chitosan acetic acid solution
Speed is added, adds in 0.5h, then, is heated to 50 DEG C, reacts 5h, after reaction terminating, obtains salicylide modification of chitosan.So
Afterwards, at 5 DEG C, 1.1g aniline, 1.0g sulfamic acid are sequentially added into the solution, are added in advance that 4.6g ammonium persulfate is molten
Solution controls and speed is added, add in 0.5h in the initiator mixed liquor of 10.0g 0.35mol/L acetic acid solution, then, reaction
6h after reaction terminating, obtains polyaniline/salicylide modification of chitosan corrosion inhibiter.
Embodiment 2:
At room temperature, 0.1g chitosan is added in 25.0g 0.35mol/L acetic acid solution, under stirring, chitosan is existed
1h is dissolved in acetic acid solution,；Then, the ethanol solution containing 0.4g salicylide, control are added into the chitosan acetic acid solution
Speed is added, adds in 0.5h, then, is heated to 50 DEG C, reacts 4h, after reaction terminating, obtains salicylide modification of chitosan.So
Afterwards, at 5 DEG C, 1.1g aniline, 3.9g sulfamic acid are sequentially added into the solution, are added in advance that 4.6g ammonium persulfate is molten
Solution controls and speed is added, add in 0.5h in the initiator mixed liquor of 10.0g 0.35mol/L acetic acid solution, then, reaction
5h after reaction terminating, obtains polyaniline/salicylide modification of chitosan corrosion inhibiter.
Embodiment 3:
At room temperature, 0.2g chitosan is added in 48.0g 0.35mol/L acetic acid solution, under stirring, chitosan is existed
1h is dissolved in acetic acid solution,；Then, the ethanol solution containing 1.6g salicylide, control are added into the chitosan acetic acid solution
Speed is added, adds in 0.5h, then, is heated to 40 DEG C, reacts 5h, after reaction terminating, obtains salicylide modification of chitosan.So
Afterwards, at 5 DEG C, 1.1g aniline, 1.0g sulfamic acid are sequentially added into the solution, are added in advance that 4.6g ammonium persulfate is molten
Solution controls and speed is added, add in 0.5h in the initiator mixed liquor of 10.0g 0.35mol/L acetic acid solution, then, reaction
8h after reaction terminating, obtains polyaniline/salicylide modification of chitosan corrosion inhibiter.
Embodiment 4:
At room temperature, 0.2g chitosan is added in 48.0g 0.35mol/L acetic acid solution, under stirring, chitosan is existed
1h is dissolved in acetic acid solution,；Then, the ethanol solution containing 1.0g salicylide, control are added into the chitosan acetic acid solution
Speed is added, adds in 0.5h, then, is heated to 60 DEG C, reacts 7h, after reaction terminating, obtains salicylide modification of chitosan.So
Afterwards, at 5 DEG C, 2.2g aniline, 5.8g sulfamic acid are sequentially added into the solution, are added in advance that 6.8g ammonium persulfate is molten
Solution controls and speed is added, add in 0.5h in the initiator mixed liquor of 10.0g 0.35mol/L acetic acid solution, then, reaction
6h after reaction terminating, obtains polyaniline/salicylide modification of chitosan corrosion inhibiter.
Embodiment 5:
At room temperature, 0.1g chitosan is added in 16.0g 0.35mol/L acetic acid solution, under stirring, chitosan is existed
1h is dissolved in acetic acid solution,；Then, the ethanol solution containing 0.4g salicylide, control are added into the chitosan acetic acid solution
Speed is added, adds in 0.5h, then, is heated to 70 DEG C, reacts 6h, after reaction terminating, obtains salicylide modification of chitosan.So
Afterwards, at 5 DEG C, 2.2g aniline, 4.8g sulfamic acid are sequentially added into the solution, are added in advance that 3.6g ammonium persulfate is molten
Solution controls and speed is added, add in 0.5h in the initiator mixed liquor of 10.0g 0.35mol/L acetic acid solution, then, reaction
5h after reaction terminating, obtains polyaniline/salicylide modification of chitosan corrosion inhibiter.
Embodiment 6:
At room temperature, 0.2g chitosan is added in 30.0g 0.35mol/L acetic acid solution, under stirring, chitosan is existed
1h is dissolved in acetic acid solution,；Then, the ethanol solution containing 1.0g salicylide, control are added into the chitosan acetic acid solution
Speed is added, adds in 0.5h, then, is heated to 60 DEG C, reacts 5h, after reaction terminating, obtains salicylide modification of chitosan.So
Afterwards, at 5 DEG C, 1.1g aniline, 3.9g sulfamic acid are sequentially added into the solution, are added in advance that 3.4g ammonium persulfate is molten
Solution controls and speed is added, add in 0.5h in the initiator mixed liquor of 10.0g 0.35mol/L acetic acid solution, then, reaction
7h after reaction terminating, obtains polyaniline/salicylide modification of chitosan corrosion inhibiter.
Embodiment 7:
At room temperature, 0.2g chitosan is added in 30.0g 0.35mol/L acetic acid solution, under stirring, chitosan is existed
1h is dissolved in acetic acid solution,；Then, the ethanol solution containing 1.0g salicylide, control are added into the chitosan acetic acid solution
Speed is added, adds in 0.5h, then, is heated to 50 DEG C, reacts 6h, after reaction terminating, obtains salicylide modification of chitosan.So
Afterwards, at 5 DEG C, 1.1g aniline, 2.4g sulfamic acid are sequentially added into the solution, are added 11.4g ammonium persulfate in advance
It is dissolved in the initiator mixed liquor of 10.0g 0.35mol/L acetic acid solution, control is added speed, adds in 0.5h, then, reaction
4h after reaction terminating, obtains polyaniline/salicylide modification of chitosan corrosion inhibiter.
Embodiment 8:
At room temperature, 0.2g chitosan is added in 48.0g 0.35mol/L acetic acid solution, under stirring, chitosan is existed
1h is dissolved in acetic acid solution,；Then, the ethanol solution containing 1.6g salicylide, control are added into the chitosan acetic acid solution
Speed is added, adds in 0.5h, then, is heated to 70 DEG C, reacts 5h, after reaction terminating, obtains salicylide modification of chitosan.So
Afterwards, at 5 DEG C, 1.1g aniline, 1.0g sulfamic acid are sequentially added into the solution, are added in advance that 1.8g ammonium persulfate is molten
Solution controls and speed is added, add in 0.5h in the initiator mixed liquor of 10.0g 0.35mol/L acetic acid solution, then, reaction
6h after reaction terminating, obtains polyaniline/salicylide modification of chitosan corrosion inhibiter.
Embodiment 9:
At room temperature, 0.1g chitosan is added in 16.0g 0.35mol/L acetic acid solution, under stirring, chitosan is existed
1h is dissolved in acetic acid solution,；Then, the ethanol solution containing 0.4g salicylide, control are added into the chitosan acetic acid solution
Speed is added, adds in 0.5h, then, is heated to 40 DEG C, reacts 4h, after reaction terminating, obtains salicylide modification of chitosan.So
Afterwards, at 5 DEG C, 2.2g aniline, 2.0g sulfamic acid are sequentially added into the solution, are added in advance that 9.2g ammonium persulfate is molten
Solution controls and speed is added, add in 0.5h in the initiator mixed liquor of 10.0g 0.35mol/L acetic acid solution, then, reaction 4
H after reaction terminating, obtains polyaniline/salicylide modification of chitosan corrosion inhibiter.
Embodiment 10:
At room temperature, 0.2g chitosan is added in 30.0g 0.35mol/L acetic acid solution, under stirring, chitosan is existed
1h is dissolved in acetic acid solution,；Then, the ethanol solution containing 1.6g salicylide, control are added into the chitosan acetic acid solution
Speed is added, adds in 0.5h, then, is heated to 60 DEG C, reacts 5h, after reaction terminating, obtains salicylide modification of chitosan.So
Afterwards, at 5 DEG C, 1.1g aniline, 3.9g sulfamic acid are sequentially added into the solution, are added in advance that 4.6g ammonium persulfate is molten
Solution controls and speed is added, add in 0.5h in the initiator mixed liquor of 10.0g 0.35mol/L acetic acid solution, then, reaction
5h after reaction terminating, obtains polyaniline/salicylide modification of chitosan corrosion inhibiter.
Embodiment 11:
At room temperature, 0.1g chitosan is added in 25.0g 0.35mol/L acetic acid solution, under stirring, chitosan is existed
1h is dissolved in acetic acid solution,；Then, the ethanol solution containing 0.4g salicylide, control are added into the chitosan acetic acid solution
Speed is added, adds in 0.5h, then, is heated to 70 DEG C, reacts 8h, after reaction terminating, obtains salicylide modification of chitosan.So
Afterwards, at 5 DEG C, 1.1g aniline, 3.9g sulfamic acid are sequentially added into the solution, are added in advance that 3.4g ammonium persulfate is molten
Solution controls and speed is added, add in 0.5h in the initiator mixed liquor of 10.0g 0.35mol/L acetic acid solution, then, reaction
6h after reaction terminating, obtains polyaniline/salicylide modification of chitosan corrosion inhibiter.
Embodiment 12:
At room temperature, 0.2g chitosan is added in 30.0g 0.35mol/L acetic acid solution, under stirring, chitosan is existed
1h is dissolved in acetic acid solution,；Then, the ethanol solution containing 1.6g salicylide, control are added into the chitosan acetic acid solution
Speed is added, adds in 0.5h, then, is heated to 80 DEG C, reacts 4h, after reaction terminating, obtains salicylide modification of chitosan.So
Afterwards, at 5 DEG C, 1.1g aniline, 2.9g sulfamic acid are sequentially added into the solution, are added in advance that 3.6g ammonium persulfate is molten
Solution controls and speed is added, add in 0.5h in the initiator mixed liquor of 10.0g 0.35mol/L acetic acid solution, then, reaction
8h after reaction terminating, obtains polyaniline/salicylide modification of chitosan corrosion inhibiter.
The test of polyaniline/salicylide modification of chitosan corrosion inhibiter corrosion inhibition:
Polyaniline/salicylide modification of chitosan corrosion inhibiter is prepared according to 2 preparation method of embodiment, is ground using electrochemical method
Study carefully polyaniline/salicylide modification of chitosan corrosion inhibiter corrosion inhibition, and slow to the polyaniline of preparation/salicylide modification of chitosan
Erosion agent carries out analysis verifying.
Electro-chemical test use CHI660E electrochemical workstation (Shanghai Chen Hua), use three-electrode system (working electrode for
Using the Q235 steel disc of epoxy resin encapsulation process, bare area is 1 × 1cm2, reference electrode is saturated calomel electrode, to electricity
Extremely platinum plate electrode), potentiodynamic polarization scanning range are as follows: -0.8 ~ -0.1V, sweep speed 1mV/s, electrochemical AC impedance
Spectral frequency variation range are as follows: 0.01 ~ 100kHz, response excursion are as follows: 5mV；
Electro-chemical test is divided into four groups, and first group of corrosive medium is the hydrochloric acid solution (100mL) of 1mol/L, and inhibition is not added
Agent；Second group of corrosive medium is the hydrochloric acid solution (100mL) of 1mol/L, adds 100ppm(0.0105g) corrosion inhibiter；Third group
Corrosive medium be 1mol/L hydrochloric acid solution (100mL), add 300ppm(0.0304g) corrosion inhibiter；4th group of corrosion is situated between
Matter is the hydrochloric acid solution (100mL) of 1mol/L, adds 500ppm(0.0504g) corrosion inhibiter.
Dynamic potential polarization curve test:
Gained polarization curve data are as shown in table 1:
1 dynamic potential polarization curve test result of table
Electrochemical AC impedance test:
Gained AC impedance modal data is as shown in table 2:
2 ac impedance spectroscopy test result of table
Claims (1)
1. polyaniline/salicylide modification of chitosan corrosion inhibiter preparation method, which is characterized in that the steps include:
(1) at room temperature, 0.35mol/L acetic acid solution is added chitosan into first, so that the quality of chitosan and acetic acid solution
Than under stirring, chitosan is dissolved 1 ~ 4h in acetic acid solution for 1:120 ~ 250；Then, into the acetic acid solution of the chitosan
The ethanol solution containing salicylide is added, makes mass ratio 1:4 ~ 8 of chitosan and salicylide, speed, 0.5 ~ 1h is added in control
It inside adds, then, is heated to 30 ~ 80oC, reacts 4 ~ 8h, obtain salicylide modification of chitosan；
(2) then, aniline, sulfamic acid at 5 DEG C, are sequentially added in Xiang Shangshu reaction system, makes the matter of chitosan and aniline
Amount than be 1:5 ~ 10, make molar ratio 1:1 ~ 5 of aniline and sulfamic acid, add the acetic acid solution containing ammonium persulfate as
Initiator mixed solution, makes molar ratio 1:0.5 ~ 2 of aniline and ammonium persulfate, and control is added speed, adds in 0.5 ~ 1h, so
Afterwards, 4 ~ 8h is reacted, polyaniline/salicylide modification of chitosan corrosion inhibiter is obtained.
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| RU2769376C1 (en) * | 2020-08-03 | 2022-03-31 | Саусвест Петролиэм Юниверсити (СВПЮ) | Method of producing modified corrosion inhibitor by acidification of chitosan |
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| CN102558568B (en) * | 2011-12-26 | 2013-06-26 | 北京理工大学 | Method for preparing chitosan bearing cyclodextrin derivative |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| RU2769376C1 (en) * | 2020-08-03 | 2022-03-31 | Саусвест Петролиэм Юниверсити (СВПЮ) | Method of producing modified corrosion inhibitor by acidification of chitosan |
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