CN103232597A - 2-mercapto benzimidazole/polyaniline anticorrosion composite material and preparation method thereof - Google Patents
2-mercapto benzimidazole/polyaniline anticorrosion composite material and preparation method thereof Download PDFInfo
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- CN103232597A CN103232597A CN2013101554838A CN201310155483A CN103232597A CN 103232597 A CN103232597 A CN 103232597A CN 2013101554838 A CN2013101554838 A CN 2013101554838A CN 201310155483 A CN201310155483 A CN 201310155483A CN 103232597 A CN103232597 A CN 103232597A
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- mercaptobenzimidazole
- polyaniline
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Abstract
The invention relates to a preparation method of a nitrogen-containing organic compound for inhibiting chemical change, and in particular relates to a preparation method of a 2-mercapto benzimidazole/polyaniline anticorrosion composite material. The preparation method of the 2-mercapto benzimidazole/polyaniline anticorrosion composite material is implemented by adopting an oxidization polymerization method. The preparation method is characterized by comprising the following steps of a, firstly, weighing acid; b, dissolving 2-mercapto benzimidazole/polyaniline in acid; c, adding ammonium persulfate solution to be reacted; and d, carrying out suction filtration and completing the preparation. The preparation process is safe and is suitable for large-scale industrial production, and the 2-mercapto benzimidazole/polyaniline anticorrosion composite material is strong in corrosion resistance and high in mechanical performance.
Description
Technical field
The present invention relates to the preparation method for the organic compounds containing nitrogen that suppresses chemical transformation, be specially a kind of 2-mercaptobenzimidazole/polyaniline anticorrosion preparation methods.
Background technology
Metallic substance is widely used in steamer, automobile, aircraft, buildings and various mechanical means.Yet, being subjected to the influence of environment, metal can be because of factor generation corrosion phenomenons such as soda acid, humidities.Traditional protection to hardware mainly is that to apply anticorrosive coating be main, the eighties in 20th century, moral hundred profits (De Berry) are found can make the stainless steel surface passivation and have erosion resistance with the synthetic polyaniline film of electrochemical process in acidic medium, after this, people have begun the applied research of conducting polymer film in the corrosion prevention field according to this discovery.Polyaniline (being PANi) is a kind of conducting polymer materials of unique properties, the low density and the workability that had both had plastics, the electroconductibility that has metal again, also possess chemistry and chemical property that metal and plastics are short of, all be widely used in fields such as anti-corrosion of metal corrosion material, antistatic material, electronic chemical products, add the environmental stability that it is good, characteristics such as synthesis material is easy to get, synthetic method is simple, polyaniline has become one of most widely used impregnating material.Yet polyaniline has bad mechanical property, solubleness weakness little, dispersion force difference in filming as anticorrosive coating film, has hindered its application in large-scale commercial production.Thereby it is its problem demanding prompt solution in the protection against corrosion area research that p-poly-phenyl amine carries out modification.
Summary of the invention
In order to overcome the defective of prior art, provide a kind of preservative property strong organic compound, the invention discloses a kind of 2-mercaptobenzimidazole/polyaniline anticorrosion preparation methods.
The present invention reaches goal of the invention by following technical solution:
The preparation method of a kind of 2-mercaptobenzimidazole/polyaniline anticorrosion matrix material, it is synthetic to adopt oxidative polymerization method to implement, and it is characterized in that: carry out successively as follows:
A. measure a certain amount of acid earlier, it is dissolved in deionized water is configured to the acid solution that concentration is 0.2mol/L～0.8mol/L;
B. the 2-mercaptobenzimidazole of 0.2g～1.0g is added in the acid solution that a step is configured to, keep mechanical stirring 2hour～6hour after, add 0.2ml～1.5ml aniline and continue to stir 1hour～5hour;
C. 1g～6g ammonium persulphate (being APS) is dissolved in the deionized water, the quality of deionized water is lower limit to dissolve ammonium persulphate fully, after ammonium persulfate solution is stirred to fully dissolving, ammonium persulfate solution slowly is added drop-wise in the solution that b step is configured to dropping funnel reacts, temperature of reaction maintains 0 ℃～45 ℃, reaction times 3hour～12hour;
D. c step reaction products therefrom alternately is washed till neutrality with ethanol and deionized water, carries out suction filtration subsequently, place 30 ℃～80 ℃ to implement vacuum-drying down the suction filtration product, finish the preparation of 2-mercaptobenzimidazole/polyaniline anticorrosion matrix material.
The preparation method of described 2-mercaptobenzimidazole/polyaniline anticorrosion matrix material is characterized in that: any one or several mixing with arbitrary proportion arbitrarily in hydrochloric acid, sulfuric acid and the phosphoric acid are selected in the acid in a when step for use.
The preparation method of described 2-mercaptobenzimidazole/polyaniline anticorrosion matrix material is characterized in that: described 2-mercaptobenzimidazole/polyaniline anticorrosion composite material by adopting 2-mercaptobenzimidazole p-poly-phenyl amine mixes and modification.
The preparation method of described 2-mercaptobenzimidazole/polyaniline anticorrosion matrix material, it is characterized in that: described 2-mercaptobenzimidazole/polyaniline anticorrosion matrix material is nanofiber, the diameter of nanofiber is 100nm～500nm, and the length of nanofiber is 5 μ m～20 μ m.
The preparation method of described 2-mercaptobenzimidazole/polyaniline anticorrosion matrix material, it is characterized in that: in described 2-mercaptobenzimidazole/polyaniline anticorrosion matrix material, the mass percent of 2-mercaptobenzimidazole in 2-mercaptobenzimidazole/polyaniline anticorrosion matrix material is 1%～20%.
After finishing the preparation of 2-mercaptobenzimidazole/polyaniline anticorrosion matrix material, prepare 2-mercaptobenzimidazole/polyaniline and epoxy blend coating more as follows:
Blend coating is made up of by mass ratio 1:1～10:1 A component and B component.Wherein, the composition of A component and B component is as follows respectively:
The A component:
Component title mass fraction
Propane type epoxy resin of di phenolic group 50～100;
2-mercaptobenzimidazole/polyaniline nano fiber 0.5～15;
Siliceous alkyl aryl polyether (as dispersion agent) 0.3～2;
Propyl carbinol 0.5～10;
The B component:
Component title mass fraction
Diethylenetriamine (as solidifying agent) 10～50;
Propyl carbinol 0.5～10.
Concrete preparation process is:
By above-mentioned mass fraction Resins, epoxy, 2-mercaptobenzimidazole/polyaniline nano fiber, dispersion agent and propyl carbinol are mixed, ultrasonic mixing 2hour～4hour namely gets the A component; By above-mentioned mass fraction solidifying agent and propyl carbinol are mixed, obtain the B component; A component and B component are mixed by 1:1～10:1, be 2-mercaptobenzimidazole/polyaniline and epoxy blend coating.
The above-mentioned blend coating that makes is coated on stainless steel surface, and coating thickness is controlled at 100 μ m～300 μ m, solidifies 12hour～24hour down at 45 ℃.Can carry out the Corrosion Protection test.
The present invention has the following advantages:
1. safe preparation process is pollution-free, and no hazardous emission is to almost not influence of surrounding enviroment;
2. the matrix material that is synthesized is nanofiber, and process is controlled and particle diameter is even, can improve the solvability of polyaniline in coating effectively with dispersed, make its better with coating blend such as resin;
3. can improve the Corrosion Protection of epoxy coating effectively, the Corrosion Protection of metallic substance is significantly improved;
4. can improve the characteristics of the bad mechanical property of polyaniline own, improve its processing characteristics, be fit to be applied to large-scale industrial production.
Embodiment
Below further specify the present invention by specific embodiment.
Embodiment 1
Getting the dense HCl(of 5.02mL is that mass percent concentration is not less than 37% HCl solution) be dissolved in the 80mL deionized water, stirring is dissolved it fully.The 2-mercaptobenzimidazole that takes by weighing 0.4506g joins in the above-mentioned HCl solution, behind the mechanical stirring 2hour, adds 0.9mL aniline and continues high-speed stirring 1hour.2.28g ammonium persulphate (being APS) is dissolved in the 20mL deionized water, be stirred to dissolving after, slowly be added drop-wise in the reaction system with dropping funnel, holding temperature about 25 ℃, the reaction 5hour.After reaction finishes, products therefrom alternately is washed till neutrality with ethanol and deionized water, suction filtration then, 60 ℃ of following vacuum-drying 12h namely obtain 2-mercaptobenzimidazole/polyaniline nano fiber.
With the 2-mercaptobenzimidazole/polyaniline nano fiber, Resins, epoxy, dispersion agent and the propyl carbinol that make by mass fraction 8:80:2:10 mix the A component, with solidifying agent and propyl carbinol press the mixed of 1:3 even the B component.The A component is mixed according to 1:1 with the B component, be coated in the stainless steel electrode surface, adopting the three-electrode system test to obtain corrosion electric current density is 1.1mA/m
2
Embodiment 2
Get the dense HCl of 5.02mL and be dissolved in the 80mL deionized water, stirring is dissolved it fully.The 2-mercaptobenzimidazole that takes by weighing 0.2253g joins in the above-mentioned HCl solution, behind the mechanical stirring 2hour, adds 0.9mL aniline and continues high-speed stirring 1hour.2.28g ammonium persulphate (being APS) is dissolved in the 20mL deionized water, be stirred to dissolving after, slowly be added drop-wise in the reaction system with dropping funnel, holding temperature about 25 ℃, the reaction 5hour.After reaction finishes, products therefrom alternately is washed till neutrality with ethanol and deionized water, suction filtration then, 60 ℃ of following vacuum-drying 12hour namely obtain 2-mercaptobenzimidazole/polyaniline mixture.
With the 2-mercaptobenzimidazole/polyaniline nano fiber, Resins, epoxy, dispersion agent and the propyl carbinol that make by mass fraction 8:80:2:10 mix the A component, with solidifying agent and propyl carbinol press the mixed of 1:3 even the B component.The A component is mixed according to 1:1 with the B component, be coated in the stainless steel electrode surface, adopting the three-electrode system test to obtain corrosion electric current density is 9.5mA/m
2
Embodiment 3
Get the dense HCl of 7.53mL and be dissolved in the 80mL deionized water, stirring is dissolved it fully.The 2-mercaptobenzimidazole that takes by weighing 0.4506g joins in the above-mentioned HCl solution, behind the mechanical stirring 2hour, adds 0.9mL aniline and continues high-speed stirring 1hour.2.28g ammonium persulphate (being APS) is dissolved in the 20mL deionized water, be stirred to dissolving after, slowly be added drop-wise in the reaction system with dropping funnel, holding temperature about 25 ℃, the reaction 5hour.After reaction finishes, products therefrom alternately is washed till neutrality with ethanol and deionized water, suction filtration then, 60 ℃ of following vacuum-drying 12hour namely obtain 2-mercaptobenzimidazole/polyaniline mixture.
With the 2-mercaptobenzimidazole/polyaniline nano fiber, Resins, epoxy, dispersion agent and the propyl carbinol that make by mass fraction 8:80:2:10 mix the A component, with solidifying agent and propyl carbinol press the mixed of 1:3 even the B component.The A component is mixed according to 1:1 with the B component, be coated in the stainless steel electrode surface, adopting the three-electrode system test to obtain corrosion electric current density is 6.4mA/m
2
Embodiment 4
Get the dense HCl of 2.51mL and be dissolved in the 80mL deionized water, stirring is dissolved it fully.The 2-mercaptobenzimidazole that takes by weighing 0.4506g joins in the above-mentioned HCl solution, behind the mechanical stirring 2hour, adds 0.9mL aniline and continues high-speed stirring 1hour.2.28g ammonium persulphate (being APS) is dissolved in the 20mL deionized water, be stirred to dissolving after, slowly be added drop-wise in the reaction system with dropping funnel, holding temperature about 25 ℃, the reaction 5hour.After reaction finishes, products therefrom alternately is washed till neutrality with ethanol and deionized water, suction filtration then, 60 ℃ of following vacuum-drying 12hour namely obtain 2-mercaptobenzimidazole/polyaniline mixture.
With the 2-mercaptobenzimidazole/polyaniline nano fiber, Resins, epoxy, dispersion agent and the propyl carbinol that make by mass fraction 8:80:2:10 mix the A component, with solidifying agent and propyl carbinol press the mixed of 1:3 even the B component.The A component is mixed according to 1:1 with the B component, be coated in the stainless steel electrode surface, adopting the three-electrode system test to obtain corrosion electric current density is 14.1mA/m
2
Embodiment 5
Get the dense HCl of 5.02mL and be dissolved in the 80mL deionized water, stirring is dissolved it fully.The 2-mercaptobenzimidazole that takes by weighing 0.4506g joins in the above-mentioned HCl solution, behind the mechanical stirring 2hour, adds 0.9mL aniline and continues high-speed stirring 1hour.1.14g ammonium persulphate (being APS) is dissolved in the 20mL deionized water, be stirred to dissolving after, slowly be added drop-wise in the reaction system with dropping funnel, holding temperature about 25 ℃, the reaction 5hour.After reaction finishes, products therefrom alternately is washed till neutrality with ethanol and deionized water, suction filtration then, 60 ℃ of following vacuum-drying 12hour namely obtain 2-mercaptobenzimidazole/polyaniline mixture.
With the 2-mercaptobenzimidazole/polyaniline nano fiber, Resins, epoxy, dispersion agent and the propyl carbinol that make by mass fraction 8:80:2:10 mix the A component, with solidifying agent and propyl carbinol press the mixed of 1:3 even the B component.The A component is mixed according to 1:1 with the B component, be coated in the stainless steel electrode surface, adopting the three-electrode system test to obtain corrosion electric current density is 28.3mA/m
2
Embodiment 6
Get the dense HCl of 5.02mL and be dissolved in the 80mL deionized water, stirring is dissolved it fully.The 2-mercaptobenzimidazole that takes by weighing 0.4506g joins in the above-mentioned HCl solution, behind the mechanical stirring 2hour, adds 0.9mL aniline and continues high-speed stirring 1hour.4.56g ammonium persulphate (being APS) is dissolved in the 20mL deionized water, be stirred to dissolving after, slowly be added drop-wise in the reaction system with dropping funnel, holding temperature about 25 ℃, the reaction 5hour.After reaction finishes, products therefrom alternately is washed till neutrality with ethanol and deionized water, suction filtration then, 60 ℃ of following vacuum-drying 12hour namely obtain 2-mercaptobenzimidazole/polyaniline mixture.
With the 2-mercaptobenzimidazole/polyaniline nano fiber, Resins, epoxy, dispersion agent and the propyl carbinol that make by mass fraction 8:80:2:10 mix the A component, with solidifying agent and propyl carbinol press the mixed of 1:3 even the B component.The A component is mixed according to 1:1 with the B component, be coated in the stainless steel electrode surface, adopting the three-electrode system test to obtain corrosion electric current density is 8.9mA/m
2
Embodiment 7
Get the dense HCl of 5.02mL and be dissolved in the 80mL deionized water, stirring is dissolved it fully.The 2-mercaptobenzimidazole that takes by weighing 0.4506g joins in the above-mentioned HCl solution, behind the mechanical stirring 2hour, adds 0.9mL aniline and continues high-speed stirring 1hour.2.28g ammonium persulphate (being APS) is dissolved in the 20mL deionized water, be stirred to dissolving after, slowly be added drop-wise in the reaction system with dropping funnel, holding temperature about 25 ℃, the reaction 3hour.After reaction finishes, products therefrom alternately is washed till neutrality with ethanol and deionized water, suction filtration then, 60 ℃ of following vacuum-drying 12hour namely obtain 2-mercaptobenzimidazole/polyaniline mixture.
With the 2-mercaptobenzimidazole/polyaniline nano fiber, Resins, epoxy, dispersion agent and the propyl carbinol that make by mass fraction 8:80:2:10 mix the A component, with solidifying agent and propyl carbinol press the mixed of 1:3 even the B component.The A component is mixed according to 1:1 with the B component, be coated in the stainless steel electrode surface, adopting the three-electrode system test to obtain corrosion electric current density is 24.7mA/m
2
Embodiment 8
With the vitriol oil and deionized water 3:40 mixing by volume, make the sulphuric acid soln of 80mL.The 2-mercaptobenzimidazole that takes by weighing 0.4506g joins in the above-mentioned sulphuric acid soln, behind the mechanical stirring 2hour, adds 0.9mL aniline and continues high-speed stirring 1hour.The ammonium persulphate of 20mL11.4wt% slowly is added drop-wise in the reaction system, and holding temperature is reacted 5hour about 25 ℃.After reaction finishes, products therefrom alternately alternately is washed till neutrality with ethanol and deionized water, suction filtration then, 60 ℃ of following vacuum-drying 12hour namely obtain 2-mercaptobenzimidazole/polyaniline mixture.
With the 2-mercaptobenzimidazole/polyaniline nano fiber, Resins, epoxy, dispersion agent and the propyl carbinol that make by mass fraction 8:80:2:10 mix the A component, with solidifying agent and propyl carbinol press the mixed of 1:3 even the B component.The A component is mixed according to 1:1 with the B component, be coated in the stainless steel electrode surface, adopting the three-electrode system test to obtain corrosion electric current density is 12.2mA/m
2
Embodiment 9
With the vitriol oil and deionized water 3:40 mixing by volume, make the sulphuric acid soln of 80mL, ratio in mass fraction is 2-mercaptobenzimidazole: the ratio of polyaniline: ammonium persulphate: sulphuric acid soln=1:3:3:9, other steps all prepare 2-mercaptobenzimidazole/polyaniline mixture with embodiment 1 identical method.
With the 2-mercaptobenzimidazole/polyaniline nano fiber, Resins, epoxy, dispersion agent and the propyl carbinol that make by mass fraction 8:80:2:10 mix the A component, with solidifying agent and propyl carbinol press the mixed of 1:3 even the B component.The A component is mixed according to 1:1 with the B component, be coated in the stainless steel electrode surface, adopting the three-electrode system test to obtain corrosion electric current density is 9.9mA/m
2
Embodiment 10
The phosphoric acid solution of configuration 80mL, 0.5mol/mL, ratio in mass fraction is 2-mercaptobenzimidazole: the ratio of polyaniline: ammonium persulphate: phosphoric acid solution=1:3:3:6, other steps all prepare 2-mercaptobenzimidazole/polyaniline mixture with embodiment 1 identical method.
With the 2-mercaptobenzimidazole/polyaniline nano fiber, Resins, epoxy, dispersion agent and the propyl carbinol that make by mass fraction 8:80:2:10 mix the A component, with solidifying agent and propyl carbinol press the mixed of 1:3 even the B component.The A component is mixed according to 1:1 with the B component, be coated in the stainless steel electrode surface, adopting the three-electrode system test to obtain corrosion electric current density is 11.4mA/m
2
Claims (5)
1. the preparation method of 2-mercaptobenzimidazole/polyaniline anticorrosion matrix material adopts oxidative polymerization method to implement to synthesize, and it is characterized in that: carry out successively as follows:
A. measure a certain amount of acid earlier, it is dissolved in deionized water is configured to the acid solution that concentration is 0.2mol/L～0.8mol/L;
B. the 2-mercaptobenzimidazole of 0.2g～1.0g is added in the acid solution that a step is configured to, keep mechanical stirring 2hour～6hour after, add 0.2mL～1.5mL aniline and continue to stir 1hour～5hour;
C. 1g～6g ammonium persulphate is dissolved in the deionized water, the quality of deionized water is lower limit to dissolve ammonium persulphate fully, after ammonium persulfate solution is stirred to fully dissolving, ammonium persulfate solution slowly is added drop-wise in the solution that b step is configured to dropping funnel reacts, temperature of reaction maintains 0 ℃～45 ℃, reaction times 3hour～12hour;
D. c step reaction products therefrom alternately is washed till neutrality with ethanol and deionized water, carries out suction filtration subsequently, place 30 ℃～80 ℃ to implement vacuum-drying down the suction filtration product, finish the preparation of 2-mercaptobenzimidazole/polyaniline anticorrosion matrix material.
2. the preparation method of 2-mercaptobenzimidazole as claimed in claim 1/polyaniline anticorrosion matrix material is characterized in that: any one or several mixing with arbitrary proportion arbitrarily in hydrochloric acid, sulfuric acid and the phosphoric acid are selected in the acid of a during the step for use.
3. the preparation method of 2-mercaptobenzimidazole as claimed in claim 1/polyaniline anticorrosion matrix material, it is characterized in that: described 2-mercaptobenzimidazole/polyaniline anticorrosion composite material by adopting 2-mercaptobenzimidazole p-poly-phenyl amine mixes and modification.
4. the preparation method of 2-mercaptobenzimidazole as claimed in claim 1/polyaniline anticorrosion matrix material, it is characterized in that: described 2-mercaptobenzimidazole/polyaniline anticorrosion matrix material is nanofiber, the diameter of nanofiber is 100nm～500nm, and the length of nanofiber is 5 μ m～20 μ m.
5. the preparation method of 2-mercaptobenzimidazole as claimed in claim 1/polyaniline anticorrosion matrix material, it is characterized in that: in described 2-mercaptobenzimidazole/polyaniline anticorrosion matrix material, the mass percent of 2-mercaptobenzimidazole in 2-mercaptobenzimidazole/polyaniline anticorrosion matrix material is 1%～20%.
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| CN108752927A (en) * | 2018-04-27 | 2018-11-06 | 同济大学 | A kind of preparation method of cysteine/polyaniline anticorrosion functional material |
| CN112007382A (en) * | 2020-09-03 | 2020-12-01 | 湖北医药学院 | Solid phase micro-extraction column and preparation and application method thereof |
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