CN103232597B - 2-mercaptobenzimidazole/polyaniline anticorrosion matrix material and preparation method thereof - Google Patents
2-mercaptobenzimidazole/polyaniline anticorrosion matrix material and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to the preparation method of the organic compounds containing nitrogen for suppressing chemical transformation, being specially the preparation method of a kind of 2-mercaptobenzimidazole/anticorrosive polyaniline corrosion material.A preparation method for 2-mercaptobenzimidazole/polyaniline anticorrosion matrix material, adopts oxidative polymerization method to implement synthesis, it is characterized in that: carry out successively as follows: a. first measures acid; B. 2-mercaptobenzimidazole and aniline is dissolved in; C. ammonium persulfate solution reaction is added; D. suction filtration, completes preparation.Safe preparation process of the present invention, Corrosion Protection is strong, and mechanical property is high, is applicable to large-scale commercial production.
Description
Technical field
The present invention relates to the preparation method of the organic compounds containing nitrogen for suppressing chemical transformation, being specially the preparation method of a kind of 2-mercaptobenzimidazole/anticorrosive polyaniline corrosion material.
Background technology
Metallic substance is widely used in steamer, automobile, aircraft, buildings and various mechanical means.But by the impact of environment, metal can because of the factor such as soda acid, humidity generation corrosion phenomenon.Traditional protection to hardware is mainly to apply anticorrosive coating, the eighties in 20th century, moral hundred profit (De Berry) finds in acidic medium, can make stainless steel surface passivation with the polyaniline film of electrochemical process synthesis and have erosion resistance, after this, people start the applied research of conducting polymer film in corrosion prevention field according to this discovery.Polyaniline (i.e. PANi) is a kind of conducting polymer materials of unique properties, both there is low density and the workability of plastics, there is again the electroconductibility of metal, 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 its good environmental stability, the features such as synthesis material is easy to get, synthetic method is simple, polyaniline has become one of most widely used impregnating material.But polyaniline has bad mechanical property, solubleness weakness that is little, dispersion force difference in film as anticorrosive coating film, hinder its application in large-scale commercial production.Thus, p-poly-phenyl amine carries out modification is its problem demanding prompt solution in protection against corrosion area research.
Summary of the invention
In order to overcome the defect of prior art, providing the organic compound that a kind of preservative property are strong, the invention discloses the preparation method of a kind of 2-mercaptobenzimidazole/anticorrosive polyaniline corrosion material.
The present invention reaches goal of the invention by following technical solution:
A preparation method for 2-mercaptobenzimidazole/polyaniline anticorrosion matrix material, adopts oxidative polymerization method to implement synthesis, it is characterized in that: carry out successively as follows:
A. the acid of first measured amounts, is dissolved in deionized water and is configured to the acid solution that concentration is 0.2mol/L ~ 0.8mol/L;
B. the 2-mercaptobenzimidazole of 0.2g ~ 1.0g being added a walks in the acid solution be configured to, and after maintaining mechanical stirring 2hour ~ 6hour, adds 0.2ml ~ 1.5ml aniline and continues to stir 1hour ~ 5hour;
C. 1g ~ 6g ammonium persulphate (i.e. APS) is dissolved in deionized water, the quality of deionized water is to dissolve ammonium persulphate completely for lower limit, ammonium persulfate solution is stirred to after dissolving completely, ammonium persulfate solution dropping funnel is slowly added drop-wise to b to walk in the solution be configured to and react, temperature of reaction maintains 0 DEG C ~ 45 DEG C, reaction times 3hour ~ 12hour;
D. c step reaction products therefrom ethanol and deionized water are alternately washed till neutrality, carry out suction filtration subsequently, at suction filtration product being placed in 30 DEG C ~ 80 DEG C, implement vacuum-drying, complete the preparation of 2-mercaptobenzimidazole/polyaniline anticorrosion matrix material.
The preparation method of described 2-mercaptobenzimidazole/polyaniline anticorrosion matrix material, is characterized in that: a step time acid select in hydrochloric acid, sulfuric acid and phosphoric acid any one or several with the mixing of arbitrary proportion arbitrarily.
The preparation method of described 2-mercaptobenzimidazole/polyaniline anticorrosion matrix material, is characterized in that: described 2-mercaptobenzimidazole/polyaniline anticorrosion matrix material adopts 2-mercaptobenzimidazole p-poly-phenyl amine to carry out adulterating 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 μm ~ 20 μm.
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 completing the preparation of 2-mercaptobenzimidazole/polyaniline anticorrosion matrix material, then prepare 2-mercaptobenzimidazole/polyaniline and epoxy blend coating as follows:
Blended coating by component A and B component in mass ratio 1:1 ~ 10:1 form.Wherein, the composition of component A and B component is as follows respectively:
Component A:
Ingredient names 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;
B component:
Ingredient names mass fraction
Diethylenetriamine (as solidifying agent) 10 ~ 50;
Propyl carbinol 0.5 ~ 10.
Concrete preparation process is:
Epoxy resin, 2-mercaptobenzimidazole/polyaniline nano fiber, dispersion agent and propyl carbinol are mixed by above-mentioned mass fraction, ultrasonic mixing 2hour ~ 4hour, obtains component A; By above-mentioned mass fraction, solidifying agent and propyl carbinol are mixed, obtain B component; Component A is mixed by 1:1 ~ 10:1 with B component, is 2-mercaptobenzimidazole/polyaniline and epoxy blend coating.
By above-mentioned obtained blended paint in stainless steel surface, coating thickness controls, at 100 μm ~ 300 μm, at 45 DEG C, to solidify 12hour ~ 24hour.Corrosion Protection test can be carried out.
The present invention has the following advantages:
1. safe preparation process is pollution-free, without hazardous emission, does not almost affect surrounding enviroment;
2. the matrix material synthesized by is nanofiber, process control and uniform particle sizes, effectively can improve polyaniline solvability in the coating with dispersed, makes it blended with the coating such as resin better;
3. effectively can improve the Corrosion Protection of epoxy coating, the Corrosion Protection of metallic substance is significantly improved;
4. can improve the feature of the bad mechanical property of polyaniline own, improve its processing characteristics, be applicable to being applied to large-scale industrial production.
Embodiment
The present invention is further illustrated below by way of specific embodiment.
Embodiment 1
Get the HCl solution that the dense HCl(of 5.02mL and mass percent concentration are not less than 37%) be dissolved in 80mL deionized water, stir and make it dissolve completely.The 2-mercaptobenzimidazole taking 0.4506g joins in above-mentioned HCl solution, after mechanical stirring 2hour, adds 0.9mL aniline and continues high-speed stirring 1hour.Be dissolved in 20mL deionized water by 2.28g ammonium persulphate (i.e. APS), after being stirred to dissolving, be slowly added drop-wise in reaction system with dropping funnel, holding temperature, at about 25 DEG C, reacts 5hour.After reaction terminates, products therefrom ethanol and deionized water are alternately washed till neutrality, then suction filtration, vacuum-drying 12h at 60 DEG C, namely obtains 2-mercaptobenzimidazole/polyaniline nano fiber.
Obtained 2-mercaptobenzimidazole/polyaniline nano fiber, epoxy resin, dispersion agent and propyl carbinol are undertaken being mixed to get component A by mass fraction 8:80:2:10, solidifying agent is mixed to obtain B component with propyl carbinol in the ratio of 1:3.Component A mixed according to 1:1 with B component, be coated in stainless steel electrode surface, adopting three-electrode system test to obtain corrosion electric current density is 1.1mA/m
2.
Embodiment 2
Getting the dense HCl of 5.02mL is dissolved in 80mL deionized water, stirs and makes it dissolve completely.The 2-mercaptobenzimidazole taking 0.2253g joins in above-mentioned HCl solution, after mechanical stirring 2hour, adds 0.9mL aniline and continues high-speed stirring 1hour.Be dissolved in 20mL deionized water by 2.28g ammonium persulphate (i.e. APS), after being stirred to dissolving, be slowly added drop-wise in reaction system with dropping funnel, holding temperature, at about 25 DEG C, reacts 5hour.After reaction terminates, products therefrom ethanol and deionized water are alternately washed till neutrality, then suction filtration, vacuum-drying 12hour at 60 DEG C, namely obtains 2-mercaptobenzimidazole/Polyaniline.
Obtained 2-mercaptobenzimidazole/polyaniline nano fiber, epoxy resin, dispersion agent and propyl carbinol are undertaken being mixed to get component A by mass fraction 8:80:2:10, solidifying agent is mixed to obtain B component with propyl carbinol in the ratio of 1:3.Component A mixed according to 1:1 with B component, be coated in stainless steel electrode surface, adopting three-electrode system test to obtain corrosion electric current density is 9.5mA/m
2.
Embodiment 3
Getting the dense HCl of 7.53mL is dissolved in 80mL deionized water, stirs and makes it dissolve completely.The 2-mercaptobenzimidazole taking 0.4506g joins in above-mentioned HCl solution, after mechanical stirring 2hour, adds 0.9mL aniline and continues high-speed stirring 1hour.Be dissolved in 20mL deionized water by 2.28g ammonium persulphate (i.e. APS), after being stirred to dissolving, be slowly added drop-wise in reaction system with dropping funnel, holding temperature, at about 25 DEG C, reacts 5hour.After reaction terminates, products therefrom ethanol and deionized water are alternately washed till neutrality, then suction filtration, vacuum-drying 12hour at 60 DEG C, namely obtains 2-mercaptobenzimidazole/Polyaniline.
Obtained 2-mercaptobenzimidazole/polyaniline nano fiber, epoxy resin, dispersion agent and propyl carbinol are undertaken being mixed to get component A by mass fraction 8:80:2:10, solidifying agent is mixed to obtain B component with propyl carbinol in the ratio of 1:3.Component A mixed according to 1:1 with B component, be coated in stainless steel electrode surface, adopting three-electrode system test to obtain corrosion electric current density is 6.4mA/m
2.
Embodiment 4
Getting the dense HCl of 2.51mL is dissolved in 80mL deionized water, stirs and makes it dissolve completely.The 2-mercaptobenzimidazole taking 0.4506g joins in above-mentioned HCl solution, after mechanical stirring 2hour, adds 0.9mL aniline and continues high-speed stirring 1hour.Be dissolved in 20mL deionized water by 2.28g ammonium persulphate (i.e. APS), after being stirred to dissolving, be slowly added drop-wise in reaction system with dropping funnel, holding temperature, at about 25 DEG C, reacts 5hour.After reaction terminates, products therefrom ethanol and deionized water are alternately washed till neutrality, then suction filtration, vacuum-drying 12hour at 60 DEG C, namely obtains 2-mercaptobenzimidazole/Polyaniline.
Obtained 2-mercaptobenzimidazole/polyaniline nano fiber, epoxy resin, dispersion agent and propyl carbinol are undertaken being mixed to get component A by mass fraction 8:80:2:10, solidifying agent is mixed to obtain B component with propyl carbinol in the ratio of 1:3.Component A mixed according to 1:1 with B component, be coated in stainless steel electrode surface, adopting three-electrode system test to obtain corrosion electric current density is 14.1mA/m
2.
Embodiment 5
Getting the dense HCl of 5.02mL is dissolved in 80mL deionized water, stirs and makes it dissolve completely.The 2-mercaptobenzimidazole taking 0.4506g joins in above-mentioned HCl solution, after mechanical stirring 2hour, adds 0.9mL aniline and continues high-speed stirring 1hour.Be dissolved in 20mL deionized water by 1.14g ammonium persulphate (i.e. APS), after being stirred to dissolving, be slowly added drop-wise in reaction system with dropping funnel, holding temperature, at about 25 DEG C, reacts 5hour.After reaction terminates, products therefrom ethanol and deionized water are alternately washed till neutrality, then suction filtration, vacuum-drying 12hour at 60 DEG C, namely obtains 2-mercaptobenzimidazole/Polyaniline.
Obtained 2-mercaptobenzimidazole/polyaniline nano fiber, epoxy resin, dispersion agent and propyl carbinol are undertaken being mixed to get component A by mass fraction 8:80:2:10, solidifying agent is mixed to obtain B component with propyl carbinol in the ratio of 1:3.Component A mixed according to 1:1 with B component, be coated in stainless steel electrode surface, adopting three-electrode system test to obtain corrosion electric current density is 28.3mA/m
2.
Embodiment 6
Getting the dense HCl of 5.02mL is dissolved in 80mL deionized water, stirs and makes it dissolve completely.The 2-mercaptobenzimidazole taking 0.4506g joins in above-mentioned HCl solution, after mechanical stirring 2hour, adds 0.9mL aniline and continues high-speed stirring 1hour.Be dissolved in 20mL deionized water by 4.56g ammonium persulphate (i.e. APS), after being stirred to dissolving, be slowly added drop-wise in reaction system with dropping funnel, holding temperature, at about 25 DEG C, reacts 5hour.After reaction terminates, products therefrom ethanol and deionized water are alternately washed till neutrality, then suction filtration, vacuum-drying 12hour at 60 DEG C, namely obtains 2-mercaptobenzimidazole/Polyaniline.
Obtained 2-mercaptobenzimidazole/polyaniline nano fiber, epoxy resin, dispersion agent and propyl carbinol are undertaken being mixed to get component A by mass fraction 8:80:2:10, solidifying agent is mixed to obtain B component with propyl carbinol in the ratio of 1:3.Component A mixed according to 1:1 with B component, be coated in stainless steel electrode surface, adopting three-electrode system test to obtain corrosion electric current density is 8.9mA/m
2.
Embodiment 7
Getting the dense HCl of 5.02mL is dissolved in 80mL deionized water, stirs and makes it dissolve completely.The 2-mercaptobenzimidazole taking 0.4506g joins in above-mentioned HCl solution, after mechanical stirring 2hour, adds 0.9mL aniline and continues high-speed stirring 1hour.Be dissolved in 20mL deionized water by 2.28g ammonium persulphate (i.e. APS), after being stirred to dissolving, be slowly added drop-wise in reaction system with dropping funnel, holding temperature, at about 25 DEG C, reacts 3hour.After reaction terminates, products therefrom ethanol and deionized water are alternately washed till neutrality, then suction filtration, vacuum-drying 12hour at 60 DEG C, namely obtains 2-mercaptobenzimidazole/Polyaniline.
Obtained 2-mercaptobenzimidazole/polyaniline nano fiber, epoxy resin, dispersion agent and propyl carbinol are undertaken being mixed to get component A by mass fraction 8:80:2:10, solidifying agent is mixed to obtain B component with propyl carbinol in the ratio of 1:3.Component A mixed according to 1:1 with B component, be coated in stainless steel electrode surface, adopting three-electrode system test to obtain corrosion electric current density is 24.7mA/m
2.
Embodiment 8
By the vitriol oil and deionized water 3:40 mixing by volume, make the sulphuric acid soln of 80mL.The 2-mercaptobenzimidazole taking 0.4506g joins in above-mentioned sulphuric acid soln, after mechanical stirring 2hour, adds 0.9mL aniline and continues high-speed stirring 1hour.Slowly be added drop-wise in reaction system by the ammonium persulphate of 20mL11.4wt%, holding temperature, at about 25 DEG C, reacts 5hour.After reaction terminates, products therefrom ethanol and deionized water are alternately alternately washed till neutrality, then suction filtration, and vacuum-drying 12hour at 60 DEG C, namely obtains 2-mercaptobenzimidazole/Polyaniline.
Obtained 2-mercaptobenzimidazole/polyaniline nano fiber, epoxy resin, dispersion agent and propyl carbinol are undertaken being mixed to get component A by mass fraction 8:80:2:10, solidifying agent is mixed to obtain B component with propyl carbinol in the ratio of 1:3.Component A mixed according to 1:1 with B component, be coated in stainless steel electrode surface, adopting three-electrode system test to obtain corrosion electric current density is 12.2mA/m
2.
Embodiment 9
By the vitriol oil and deionized water 3:40 mixing by volume, make the sulphuric acid soln of 80mL, be 2-mercaptobenzimidazole in the ratio of mass fraction: polyaniline: ammonium persulphate: the ratio of sulphuric acid soln=1:3:3:9, the method that other steps are all identical with embodiment 1 prepares 2-mercaptobenzimidazole/Polyaniline.
Obtained 2-mercaptobenzimidazole/polyaniline nano fiber, epoxy resin, dispersion agent and propyl carbinol are undertaken being mixed to get component A by mass fraction 8:80:2:10, solidifying agent is mixed to obtain B component with propyl carbinol in the ratio of 1:3.Component A mixed according to 1:1 with B component, be coated in stainless steel electrode surface, adopting 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, be 2-mercaptobenzimidazole in the ratio of mass fraction: polyaniline: ammonium persulphate: the ratio of phosphoric acid solution=1:3:3:6, the method that other steps are all identical with embodiment 1 prepares 2-mercaptobenzimidazole/Polyaniline.
Obtained 2-mercaptobenzimidazole/polyaniline nano fiber, epoxy resin, dispersion agent and propyl carbinol are undertaken being mixed to get component A by mass fraction 8:80:2:10, solidifying agent is mixed to obtain B component with propyl carbinol in the ratio of 1:3.Component A mixed according to 1:1 with B component, be coated in stainless steel electrode surface, adopting three-electrode system test to obtain corrosion electric current density is 11.4mA/m
2.
Claims (5)
1. a preparation method for 2-mercaptobenzimidazole/polyaniline anticorrosion matrix material, adopts oxidative polymerization method to implement synthesis, it is characterized in that: carry out successively as follows:
A. the acid of first measured amounts, is dissolved in deionized water and is configured to the acid solution that concentration is 0.2mol/L ~ 0.8mol/L;
B. the 2-mercaptobenzimidazole of 0.2g ~ 1.0g being added a walks in the acid solution be configured to, and after maintaining mechanical stirring 2hour ~ 6hour, adds 0.2mL ~ 1.5mL aniline and continues to stir 1hour ~ 5hour;
C. 1g ~ 6g ammonium persulphate is dissolved in deionized water, the quality of deionized water is to dissolve ammonium persulphate completely for lower limit, ammonium persulfate solution is stirred to after dissolving completely, ammonium persulfate solution dropping funnel is slowly added drop-wise to b to walk in the solution be configured to and react, temperature of reaction maintains 0 DEG C ~ 45 DEG C, reaction times 3hour ~ 12hour;
D. c step reaction products therefrom ethanol and deionized water are alternately washed till neutrality, carry out suction filtration subsequently, at suction filtration product being placed in 30 DEG C ~ 80 DEG C, implement vacuum-drying, complete the preparation of 2-mercaptobenzimidazole/polyaniline anticorrosion matrix material.
2. the preparation method of 2-mercaptobenzimidazole/polyaniline anticorrosion matrix material as claimed in claim 1, is characterized in that: acid during a step select in hydrochloric acid, sulfuric acid and phosphoric acid any one or several with the mixing of arbitrary proportion arbitrarily.
3. the preparation method of 2-mercaptobenzimidazole/polyaniline anticorrosion matrix material as claimed in claim 1, is characterized in that: described 2-mercaptobenzimidazole/polyaniline anticorrosion matrix material adopts 2-mercaptobenzimidazole p-poly-phenyl amine to carry out adulterating and modification.
4. the preparation method of 2-mercaptobenzimidazole/polyaniline anticorrosion matrix material as claimed in claim 1, 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 μm ~ 20 μm.
5. the preparation method of 2-mercaptobenzimidazole/polyaniline anticorrosion matrix material as claimed in claim 1, 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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| CN106032432B (en) * | 2015-03-16 | 2018-07-27 | 同济大学 | 2-mercaptobenzimidazole/carbon nano-tube/poly aniline composite material and its preparation |
| CN108165964A (en) * | 2018-01-22 | 2018-06-15 | 唐凤骏 | A kind of polyaniline colloidal sol metal conditioner |
| CN108752927A (en) * | 2018-04-27 | 2018-11-06 | 同济大学 | A kind of preparation method of cysteine/polyaniline anticorrosion functional material |
| CN112007382B (en) * | 2020-09-03 | 2021-12-28 | 湖北医药学院 | Solid phase micro-extraction column and preparation and application method thereof |
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