CN101775176B - Polyaniline/polymerized (styrene-styrene sodium sulfonate) nuclear shell structure emulsion - Google Patents
Polyaniline/polymerized (styrene-styrene sodium sulfonate) nuclear shell structure emulsion Download PDFInfo
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Abstract
The invention discloses a polyaniline/polymerized (styrene-styrene sodium sulfonate) nuclear shell structure emulsion, which comprises the following components in parts by weight: 0.5-2 parts of styrene sodium sulfonate, 5-15 parts of styrene, 0.5-4 parts of lauryl sodium sulfate, 0.5-4 parts of nonionic surfactant, 2-8 parts of n-pentane, 7-11 parts of aniline, 3-11 parts of oxidant ammonium persulfate, 0.01-0.1 part of initiator potassium peroxydisulfate and 70-90 parts of water. The nuclear shell structure emulsion is nanometer composite colloidal particle which takes electric polyaniline is taken as shell and plastic styrene-styrene sodium sulfonate copolymer as inner core. The composite polymer particle can realize regular arrangement and compact accumulation. The nuclear shell polymer is a water dispersible microemulsion system, has good compatibility with ethoxyline resin aqueous emulsion, and can be directly mixed with the ethoxyline resin emulsion to prepare paint to obtain anticorrosive paint with good performance and environment protection.
Description
Technical field
The present invention relates to a kind of polyaniline/poly-(vinylbenzene-Sodium styrene sulfonate) nuclear shell structure emulsion, and synthetic.
Background technology
Traditional protective system is rich in heavy metals such as zinc, not only consumed a large amount of zinc resources, environment is caused serious heavy metal contamination, but also it exists that anticorrosion timeliness is short because the reason of anticorrosion mechanism makes, performance deficiency such as the easy porous of the too high coating of zinc content in the coating.
As the conductive polymers impregnating material that application prospect is arranged most, polyaniline makes the metallic surface active passivation and anticorrosion, anticorrosion medium physical isolation is limited in metallic corrosion on the membrane interface, and improves the current potential of metal, can bring into play preservative activity for a long time.Polyaniline has preservative activity, especially its distinctive anti-spot corrosion, scratch resistance ability to multiple metal such as cold-rolled steel, soft steel, aluminium, copper etc., and other protective system is incomparable especially.Therefore the environment-friendly polyaniline protective system becomes the research focus and one of main developing direction of metal anti-corrosive paint.
Though polyaniline has good corrosion prevention performance, the consistency of itself and resin is poor, has limited its use.Now polyaniline has with the ordinary method of resin-bonded: 1. dissolution method: add in the resin with special solvent dissolving back, this method can cause environmental pollution, and execution conditions are abominable, and solvent costs an arm and a leg and makes cost sharp increase; 2. physical blending method: as ball milled, expend a large amount of energy and time, and its dispersiveness and poor stability in resin, finally influenced the performance of anticorrosive polyaniline performance; 3. earlier dissolve polyaniline in amine curing agent, compound with Resins, epoxy again, this method has the defective that can't overcome: polyaniline content is low, can't reach the content of the best preservative effect of tool.
Summary of the invention
At above-mentioned prior art,, the invention provides a kind of polyaniline/poly-(vinylbenzene-Sodium styrene sulfonate) nuclear shell structure emulsion for solving the problem of polyaniline and resin compatible difference.
The present invention is achieved by the following technical solutions:
A kind of polyaniline/poly-(vinylbenzene-Sodium styrene sulfonate) nuclear shell structure emulsion, it is to make: 0.5～2 part of Sodium styrene sulfonate by the component of following weight part, 5～15 parts of vinylbenzene, 0.5～4 part of sodium lauryl sulphate, 0.5～4 part of nonionogenic tenside, 2～8 parts of Pentyl alcohols, 7～11 parts of aniline, 3～11 parts of oxygenant ammonium persulphates, 0.01～0.1 part of initiator potassium persulfate, 70～90 parts in water; For electrically conductive polyaniline is that shell, plasticity vinylbenzene-Sodium styrene sulfonate multipolymer are the nano combined micelle of kernel.
Described nonionogenic tenside is to be raw material with bisphenol-type epoxy resin and polyoxyethylene glycol, obtain through following preparation method: bisphenol-type epoxy resin and polyoxyethylene glycol are added in the there-necked flask in 1: 1～2: 1 ratios, be warming up to 60～65 ℃ of stirring and dissolving evenly after, add catalyst A lCl
3After, be warmed up to 115～125 ℃ of reaction 7～9h, obtain light yellow viscous liquid, be nonionogenic tenside.
Described Resins, epoxy is Resins, epoxy E-20 or E-44; Described polyoxyethylene glycol is Macrogol 4000 or polyethylene glycol 6000.
The preparation method of a kind of polyaniline/poly-(vinylbenzene-Sodium styrene sulfonate) nuclear shell structure emulsion is characterized in that, may further comprise the steps:
(1) preparation nonionogenic tenside: in 1: 1～2: 1 ratios bisphenol-type epoxy resin and polyoxyethylene glycol are added in the there-necked flask, be warming up to 60～65 ℃ of stirring and dissolving even after, add a spot of catalyst A lCl
3After, be warmed up to 115～125 ℃ of reaction 7～9h, obtain light yellow viscous liquid, be nonionogenic tenside;
(2) poly-(vinylbenzene-Sodium styrene sulfonate) nanometer latex of preparation: under nitrogen protection, with Sodium styrene sulfonate, vinylbenzene, sodium lauryl sulphate, nonionogenic tenside, Pentyl alcohol and distilled water is main raw material, chooses the suitable stable high-content microemulsion system of ratio preparation; Above-mentioned microemulsion system is put into 75 ℃ of waters bath with thermostatic control, add the polyreaction that initiator potassium persulfate causes vinylbenzene and Sodium styrene sulfonate, obtain poly-(vinylbenzene-Sodium styrene sulfonate) nanometer latex of high-content;
(3) under nitrogen protection; regulate pH value to 1～2 of poly-(vinylbenzene-Sodium styrene sulfonate) latex system; get aniline monomer and add in the flask; high degree of agitation to each component mixes; dropwise add ammonium persulfate aqueous solution (mass concentration is 51%～71%) then; continue stirring reaction 24 hours, promptly obtain high-content nano polyaniline/poly-(vinylbenzene-Sodium styrene sulfonate) nucleocapsid structure composite particles.
Nucleocapsid structure PANI/ of the present invention (PS-PSS) microemulsion is to be that shell, plasticity vinylbenzene-Sodium styrene sulfonate multipolymer are the nano combined micelle of kernel with the electrically conductive polyaniline.This composite polymer particle can implementation rule arrangement and tightly packed.This core-shell polymer is a water dispersible microemulsion system, and is good with the consistency of Resins, epoxy water-based emulsion, can be directly and epoxy resin latex blend preparation coating, obtain the environmental protection protective system of excellent performance.
Embodiment
The present invention is further illustrated below in conjunction with embodiment:
Embodiment 1:
(1) be that 1: 1 Resins, epoxy E-20 and Macrogol 4000 is added in the there-necked flask that agitator and thermometer are housed with mol ratio, be warming up to 60 ℃ of stirring and dissolving evenly after, add a spot of catalyst A lCl
3After be warmed up to 120 ℃ the reaction 8h, obtain light yellow viscous liquid and be nonionogenic tenside.
(2) in round-bottomed flask, add 1g sodium laurylsulfonate (SDS) and the homemade nonionogenic tenside of 1g, the 40g deionized water, high degree of agitation 1 hour is dissolved fully to sodium laurylsulfonate (SDS).Add the 0.5g Sodium styrene sulfonate then, the styrene monomer of 5.0g and 2.8g Pentyl alcohol feed a large amount of nitrogen, and high degree of agitation formed microemulsion system after 1 hour.Take by weighing 5.784g Potassium Persulphate (KPS), stand-by with the volumetric flask preparation KPS aqueous solution of 100ml.The microemulsion system for preparing put in 75 ℃ the water bath with thermostatic control, measure the above-mentioned KPS solution of 400 μ l as initiator (mol ratio of KPS and styrene monomer 1: 100), add the microemulsion system initiated polymerization, after reaction is carried out 4 hours, gathered (vinylbenzene-Sodium styrene sulfonate) nano rubber latex particle.
(3) regulate about the pH value to 2 of poly-(vinylbenzene-Sodium styrene sulfonate) latex system with hydrochloric acid.Flask is put into ice-water bath, measure a certain amount of aniline monomer (mass ratio of aniline and kernel is 9: 11) and add in the flask, high degree of agitation 2h mixes each component.The APS that takes by weighing respective amount pours in the beaker, adds 5ml distilled water, stirs and dropwise join (add half an hour) in the flask after APS dissolves fully, after reaction is carried out 24 hours, obtains high-content nucleocapsid structure PANI/ (PS-PSS) microemulsion.This process is carried out under nitrogen protection.The ratio of oxygenant ammonium persulphate and aniline monomer is (APS
(mol): An
(mol)=1: 2).
Embodiment 2:
(1) be that 1: 1 Resins, epoxy E-20 and polyethylene glycol 6000 is added in the there-necked flask that agitator and thermometer are housed with mol ratio, be warming up to 60 ℃ of stirring and dissolving evenly after, add a spot of catalyst A lCl
3After be warmed up to 120 ℃ the reaction 8h, obtain light yellow viscous liquid and be nonionogenic tenside.
(2) in round-bottomed flask, add 0.5g sodium laurylsulfonate (SDS) and the homemade nonionogenic tenside of 1g, the 40g deionized water, high degree of agitation 1 hour is dissolved fully to sodium laurylsulfonate (SDS).Add the 1g Sodium styrene sulfonate then, the styrene monomer of 5.0g and 3g Pentyl alcohol feed a large amount of nitrogen, and high degree of agitation formed microemulsion system after 1 hour.Take by weighing 5.784g Potassium Persulphate (KPS), stand-by with the volumetric flask preparation KPS aqueous solution of 100ml.The microemulsion system for preparing put in 75 ℃ the water bath with thermostatic control, measure the above-mentioned KPS solution of 400 μ l as initiator (mol ratio of KPS and styrene monomer 1: 100), add the microemulsion system initiated polymerization, after reaction is carried out 4 hours, gathered (vinylbenzene-Sodium styrene sulfonate) nano rubber latex particle.
(3) regulate about the pH value to 2 of poly-(vinylbenzene-Sodium styrene sulfonate) latex system with hydrochloric acid.Flask is put into ice-water bath, measure a certain amount of aniline monomer (mass ratio of aniline and kernel is 8: 11) and add in the flask, high degree of agitation 2h mixes each component.The APS that takes by weighing respective amount pours in the beaker, adds 5ml distilled water, stirs and dropwise join (add half an hour) in the flask after APS dissolves fully, after reaction is carried out 24 hours, obtains high-content nucleocapsid structure PANI/ (PS-PSS) microemulsion.This process is carried out under nitrogen protection.The ratio of oxygenant ammonium persulphate and aniline monomer is (APS
(mol): An
(mol)=1: 2).
Embodiment 3:
(1) be that 2: 1 Resins, epoxy E-20 and polyethylene glycol 6000 is added in the there-necked flask that agitator and thermometer are housed with mol ratio, be warming up to 60 ℃ of stirring and dissolving evenly after, add a spot of catalyst A lCl
3After be warmed up to 120 ℃ the reaction 8h, obtain light yellow viscous liquid and be nonionogenic tenside.
(2) in round-bottomed flask, add 2g sodium laurylsulfonate (SDS) and the homemade nonionogenic tenside of 1g, the 40g deionized water, high degree of agitation 1 hour is dissolved fully to sodium laurylsulfonate (SDS).Add the 0.5g Sodium styrene sulfonate then, the styrene monomer of 5.5g and 2.8g Pentyl alcohol feed a large amount of nitrogen, and high degree of agitation formed microemulsion system after 1 hour.Take by weighing 5.784g Potassium Persulphate (KPS), stand-by with the volumetric flask preparation KPS aqueous solution of 100ml.The microemulsion system for preparing put in 75 ℃ the water bath with thermostatic control, measure the above-mentioned KPS solution of 200 μ l as initiator (mol ratio of KPS and styrene monomer 1: 100), add the microemulsion system initiated polymerization, after reaction is carried out 6 hours, gathered (vinylbenzene-Sodium styrene sulfonate) nano rubber latex particle.
(3) regulate about the pH value to 2 of poly-(vinylbenzene-Sodium styrene sulfonate) latex system with hydrochloric acid.Measure a certain amount of aniline monomer (mass ratio of aniline and kernel is 10: 11) and add in the flask, high degree of agitation 2h mixes each component.The APS that takes by weighing respective amount pours in the beaker, adds 5ml distilled water, stirs and dropwise join (add half an hour) in the flask after APS dissolves fully, after room temperature reaction carries out 24 hours, obtains high-content nucleocapsid structure PANI/ (PS-PSS) microemulsion.This process is carried out under nitrogen protection.The ratio of oxygenant ammonium persulphate and aniline monomer is (APS
(mol): An
(mol)=1: 2).
Embodiment 4:
(1) be that 1: 1 epoxy resin E-44 and polyethylene glycol 6000 is added in the there-necked flask that agitator and thermometer are housed with mol ratio, be warming up to 60 ℃ of stirring and dissolving evenly after, add a spot of catalyst A lCl
3After be warmed up to 120 ℃ the reaction 8h, obtain light yellow viscous liquid and be nonionogenic tenside.
(2) in round-bottomed flask, add 1g sodium laurylsulfonate (SDS) and the homemade nonionogenic tenside of 1g, the 20g deionized water, high degree of agitation 1 hour is dissolved fully to sodium laurylsulfonate (SDS).Add the 0.5g Sodium styrene sulfonate then, the styrene monomer of 5.0g and 2g Pentyl alcohol feed a large amount of nitrogen, and high degree of agitation formed microemulsion system after 1 hour.Take by weighing 5.784g Potassium Persulphate (KPS), stand-by with the volumetric flask preparation KPS aqueous solution of 100ml.The microemulsion system for preparing put in 75 ℃ the water bath with thermostatic control, measure the above-mentioned KPS solution of 600 μ l as initiator (mol ratio of KPS and styrene monomer 1: 100), add the microemulsion system initiated polymerization, after reaction is carried out 4 hours, gathered (vinylbenzene-Sodium styrene sulfonate) nano rubber latex particle.
(3) regulate about the pH value to 2 of poly-(vinylbenzene-Sodium styrene sulfonate) latex system with hydrochloric acid.Flask is put into ice-water bath, measure a certain amount of aniline monomer (mass ratio of aniline and kernel is 10: 11) and add in the flask, high degree of agitation 2h mixes each component.The APS that takes by weighing respective amount pours in the beaker, adds 5ml distilled water, stirs and dropwise join (add half an hour) in the flask after APS dissolves fully, after reaction is carried out 12 hours, obtains high-content nucleocapsid structure PANI/ (PS-PSS) microemulsion.This process is carried out under nitrogen protection.The ratio of oxygenant ammonium persulphate and aniline monomer is (APS
(mol): An
(mol)=1: 1).
Embodiment 5:
(1) be that 1: 1 epoxy resin E-44 and Macrogol 4000 is added in the there-necked flask that agitator and thermometer are housed with mol ratio, be warming up to 60 ℃ of stirring and dissolving evenly after, add a spot of catalyst A lCl
3After be warmed up to 120 ℃ the reaction 8h, obtain light yellow viscous liquid and be nonionogenic tenside.
(2) in round-bottomed flask, add 1g sodium laurylsulfonate (SDS) and the homemade nonionogenic tenside of 2g, the 40g deionized water, high degree of agitation 1 hour is dissolved fully to sodium laurylsulfonate (SDS).Add the 0.5g Sodium styrene sulfonate then, the styrene monomer of 5.0g and 2.8g Pentyl alcohol feed a large amount of nitrogen, and high degree of agitation formed microemulsion system after 1 hour.Take by weighing 5.784g Potassium Persulphate (KPS), stand-by with the volumetric flask preparation KPS aqueous solution of 100ml.The microemulsion system for preparing put in 75 ℃ the water bath with thermostatic control, measure the above-mentioned KPS solution of 400 μ l as initiator (mol ratio of KPS and styrene monomer 1: 100), add the microemulsion system initiated polymerization, after reaction is carried out 4 hours, gathered (vinylbenzene-Sodium styrene sulfonate) nano rubber latex particle.
(3) regulate about the pH value to 2 of poly-(vinylbenzene-Sodium styrene sulfonate) latex system with hydrochloric acid.Measure a certain amount of aniline monomer (mass ratio of aniline and kernel is 9: 11) and add in the flask, high degree of agitation 2h mixes each component.The APS that takes by weighing respective amount pours in the beaker, adds 5ml distilled water, stirs and dropwise join (add half an hour) in the flask after APS dissolves fully, after room temperature reaction carries out 24 hours, obtains high-content nucleocapsid structure PANI/ (PS-PSS) microemulsion.This process is carried out under nitrogen protection.The ratio of oxygenant ammonium persulphate and aniline monomer is (APS
(mol): An
(mol)=1: 2).
Embodiment 6:
(1) be that 1: 1 Resins, epoxy E-20 and polyethylene glycol 6000 is added in the there-necked flask that agitator and thermometer are housed with mol ratio, be warming up to 60 ℃ of stirring and dissolving evenly after, add a spot of catalyst A lCl
3After be warmed up to 120 ℃ the reaction 8h, obtain light yellow viscous liquid and be nonionogenic tenside.
(2) in round-bottomed flask, add 1g sodium laurylsulfonate (SDS) and the homemade nonionogenic tenside of 1g, the 40g deionized water, high degree of agitation 1 hour is dissolved fully to sodium laurylsulfonate (SDS).Add the 0.5g Sodium styrene sulfonate then, the styrene monomer of 5.0g and 2.8g Pentyl alcohol feed a large amount of nitrogen, and high degree of agitation formed microemulsion system after 1 hour.Take by weighing 5.784g Potassium Persulphate (KPS), stand-by with the volumetric flask preparation KPS aqueous solution of 100ml.The microemulsion system for preparing put in 75 ℃ the water bath with thermostatic control, measure the above-mentioned KPS solution of 400 μ l as initiator (mol ratio of KPS and styrene monomer 1: 100), add the microemulsion system initiated polymerization, after reaction is carried out 4 hours, gathered (vinylbenzene-Sodium styrene sulfonate) nano rubber latex particle.
(3) regulate about the pH value to 2 of poly-(vinylbenzene-Sodium styrene sulfonate) latex system with hydrochloric acid.Flask is put into ice-water bath, measure a certain amount of aniline monomer (mass ratio of aniline and kernel is 7: 11) and add in the flask, high degree of agitation 2h mixes each component.The APS that takes by weighing respective amount pours in the beaker, adds 5ml distilled water, stirs and dropwise join (add half an hour) in the flask after APS dissolves fully, after reaction is carried out 24 hours, obtains high-content nucleocapsid structure PANI/ (PS-PSS) microemulsion.This process is carried out under nitrogen protection.The ratio of oxygenant ammonium persulphate and aniline monomer is (APS
(mol): An
(mol)=1: 1).
Claims (4)
1. a polyaniline/poly-(vinylbenzene-Sodium styrene sulfonate) nuclear shell structure emulsion, it is characterized in that, be to make: 0.5～2 part of Sodium styrene sulfonate, 5～15 parts of vinylbenzene, 0.5～4 part of sodium lauryl sulphate by the component of following weight part, 0.5～4 part of nonionogenic tenside, 2～8 parts of Pentyl alcohols, 7～11 parts of aniline, 3～11 parts of ammonium persulphates, 0.01～0.1 part of Potassium Persulphate, 70～90 parts in water; For electrically conductive polyaniline is that shell, plasticity vinylbenzene-Sodium styrene sulfonate multipolymer are the nano combined micelle of kernel;
Described nonionogenic tenside is to be raw material with bisphenol-type epoxy resin and polyoxyethylene glycol, obtains through following preparation method:
1: 1 in molar ratio～2: 1 ratio is added to bisphenol-type epoxy resin and polyoxyethylene glycol in the there-necked flask, be warming up to 60～65 ℃ of stirring and dissolving evenly after, add catalyst A lCl
3After, be warmed up to 115～125 ℃ of reaction 7～9h, obtain light yellow viscous liquid, be nonionogenic tenside.
2. a kind of polyaniline according to claim 1/poly-(vinylbenzene-Sodium styrene sulfonate) nuclear shell structure emulsion, it is characterized in that: described Resins, epoxy is Resins, epoxy E-20 or E-44; Described polyoxyethylene glycol is Macrogol 4000 or polyethylene glycol 6000.
3. the preparation method of the described a kind of polyaniline of claim 1/poly-(vinylbenzene-Sodium styrene sulfonate) nuclear shell structure emulsion is characterized in that, may further comprise the steps:
(1) preparation nonionogenic tenside: in 1: 1～2: 1 ratios bisphenol-type epoxy resin and polyoxyethylene glycol are added in the there-necked flask, be warming up to 60～65 ℃ of stirring and dissolving evenly after, adding catalyst A lCl
3After, be warmed up to 115～125 ℃ of reaction 7～9h, obtain light yellow viscous liquid, be nonionogenic tenside;
(2) poly-(vinylbenzene-Sodium styrene sulfonate) nanometer latex of preparation: under nitrogen protection, Sodium styrene sulfonate, vinylbenzene, sodium lauryl sulphate, nonionogenic tenside, Pentyl alcohol and water with formula ratio are main raw material, choose the nonionogenic tenside of formula ratio, put into 75 ℃ of waters bath with thermostatic control, the polyreaction that adds initiator potassium persulfate initiation vinylbenzene and Sodium styrene sulfonate obtains poly-(vinylbenzene-Sodium styrene sulfonate) nanometer latex of high-content;
(3) under nitrogen protection; regulate pH value to 1～2 of poly-(vinylbenzene-Sodium styrene sulfonate) latex system; get aniline monomer and add in the flask; high degree of agitation to each component mixes; dropwise add ammonium persulfate aqueous solution then; continue stirring reaction 24 hours, promptly obtain high-content nano polyaniline/poly-(vinylbenzene-Sodium styrene sulfonate) nucleocapsid structure composite particles.
4. the preparation method of a kind of polyaniline according to claim 3/poly-(vinylbenzene-Sodium styrene sulfonate) nuclear shell structure emulsion, it is characterized in that: the mass concentration of described ammonium persulfate aqueous solution is 51%～71%.
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| CN104335048A (en) * | 2012-03-30 | 2015-02-04 | 积水医疗株式会社 | Latex particles for agglutination assay |
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| CN102040695B (en) * | 2010-11-26 | 2012-02-29 | 中国人民解放军国防科学技术大学 | Preparation method of water-soluble polyvinylpyrrolidone grafted polyaniline (PVP-g-PANI) copolymer |
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Cited By (2)
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| CN104335048A (en) * | 2012-03-30 | 2015-02-04 | 积水医疗株式会社 | Latex particles for agglutination assay |
| CN104335048B (en) * | 2012-03-30 | 2017-05-17 | 积水医疗株式会社 | Latex particles for agglutination assay |
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