CN104059225A - Chemical polymerization process for preparing polypyrrole - Google Patents
Chemical polymerization process for preparing polypyrrole Download PDFInfo
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- CN104059225A CN104059225A CN201410288713.2A CN201410288713A CN104059225A CN 104059225 A CN104059225 A CN 104059225A CN 201410288713 A CN201410288713 A CN 201410288713A CN 104059225 A CN104059225 A CN 104059225A
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Abstract
The invention provides a chemical polymerization process for preparing polypyrrole. The monomer concentration of a monomer solution used for chemical polymerization is relatively stable, the pH value of the monomer solution is controlled within the range of 0.5-2.0, the temperature is controlled within the range of 10-50 DEG C, and the immersion time of the monomer solution is controlled within the range of 1-2min. The temperature of an oxidation solution used for chemical polymerization is controlled within the range of 5-35 DEG C, the immersion time of the oxidation solution is controlled within the range of 0.5-1min, and the number of cycles is controlled within 2-4 times. By using the process provided by the invention, the leak current property of a prepared solid polymer aluminum electrolytic capacitor and characteristics of the prepared solid polymer aluminum electrolytic capacitor under high temperature and high humidity environments are more excellent.
Description
Technical field
The present invention relates to a kind of chemical polymerization process of preparing polypyrrole of solid electrolytic capacitor.
Background technology
We know, under high temperature and super-humid conditions, work long hours, and solid capacitor easily causes performance degradation, cause capacity to reduce, and equivalent series resistance (ESR) increases, and leakage current value increases.In order to address the above problem, in way in the past, have, by increasing the wall thickness of potting resin of pin one side of electrical condenser, extend the distance between potting resin outer end and capacitor cathode and anode; Or at electrical condenser pin, carry out coated with resins again with the gap that contacts of potting resin, delay entering of airborne oxygen and steam, thereby the capacitor performance improving under hot and humid condition is deteriorated.
The problem existing in above-mentioned way is in the past, by increasing the method for potting resin wall thickness, will cause the physical dimension of electrical condenser to increase, and result causes being difficult to realize miniaturization, can not meet especially the demand of current miniaturization of electronic products.And by the way that coated with resins is carried out again in gap that contacts with potting resin at electrical condenser pin, on equipment, be difficult to realize automatization, and be unfavorable for the production in enormous quantities technique of industrialization,, capacitor product outward appearance is also had a certain impact meanwhile.
Summary of the invention
The technical problem to be solved in the present invention, is to provide a kind of chemical polymerization process of preparing polypyrrole, makes leakage current characteristic and the characteristic under hot and humid environment of the solid polymer aluminium electrolutic capacitor for preparing better.
The present invention is achieved in that a kind of chemical polymerization process of preparing polypyrrole, the monomer concentration of the monomer solution that chemical polymerization is used is stable, the pH value of monomer solution is controlled at 0.5-2.0, the temperature of monomer solution is controlled at 10-50 ℃, the immersion liquid time of monomer solution is 1-2 minute, the temperature of the oxidation solution that chemical polymerization is used is controlled at 5-35 ℃, and the immersion liquid time of oxidation solution is 0.5-1 minute, and cycle index is 2-4 time.
Further, the pH value of described monomer concentration and monomer solution is added and is contained monomer and doping agent mixed solution is controlled by timing.
Further, described timing is added to every 5-10min and adds once.
Further, described monomer solution comprises pyrrole monomer and doping agent.
Further, described doping agent comprises any in p-methyl benzenesulfonic acid and salt, Witco 1298 Soft Acid and salt thereof, dodecyl sodium sulfonate and salt thereof, camphorsulfonic acid and salt thereof, Phenylsulfonic acid and salt thereof, naphthene sulfonic acid and salt thereof, dibutyl naphthalene sulfonic acid and salt thereof, phenol sulfonic acid and salt, sulphosalicylic acid and salt thereof, sulfosalicylic acid and salt thereof, naphthalene disulfonic acid and salt thereof, benzene disulfonic acid and salt thereof, anthraquinone disulfonic acid and salt thereof.
Tool of the present invention has the following advantages: the present invention, without increasing potting resin wall thickness, without the physical dimension that increases electrical condenser, is conducive to miniaturization development; The present invention, without increasing new equipment and Automation of Manufacturing Process, is conducive to the production in enormous quantities of industrialization; Under leakage current characteristic and hot and humid environment in end properties of the present invention, the characteristic of (85 ℃, 85%RH, after 1000h) product is obviously better; Features simple and practical process of the present invention, has significant economic benefit.
Embodiment
Embodiment 1:
In chemical polymerization operation, aluminium foil cathode portion is placed in to the KMnO of 0.35M
4in the aqueous solution, soak 1 minute, take out and dry, then in monomer solution, soak 2 minutes, described monomer solution is Py (pyrrole monomer) and the p-methyl benzenesulfonic acid of 0.5M and the mixed aqueous solution of salt thereof containing 0.45M, take out and dry, repeat aluminium foil cathode portion to be placed in KMnO
4the aqueous solution, in monomer solution, soak 2 times after cleaning, drying at cathode surface, form pre-conductive layer.Wherein, in monomer solution, by adjusting the ratio of p-methyl benzenesulfonic acid and salt thereof, the mixing solutions of Py of 5min interpolation simultaneously and p-methyl benzenesulfonic acid and salt thereof, the pH value that makes solution is 0.5; The temperature of controlling monomer solution by water-bath is 30 ℃, and the temperature of oxidizing solution is 25 ℃.
Embodiment 2:
Remove at KMnO
4in the aqueous solution, soak 0.5 minute, soak 1 minute in monomer solution, described monomer solution, for the mixed aqueous solution containing Py and dodecyl sodium sulfonate and salt thereof, repeats aluminium foil cathode portion to be placed in KMnO
4the aqueous solution, soaks in monomer solution 3 times.Wherein, in monomer solution, by adjusting the ratio of dodecyl sodium sulfonate and salt thereof, the mixing solutions of Py of 5min interpolation simultaneously and dodecyl sodium sulfonate and salt thereof, the pH value that makes solution is 0.8; The temperature of monomer solution is 35 ℃, and the temperature of oxidizing solution is outside 30 ℃, and all the other are with embodiment 1.
Embodiment 3:
Remove at KMnO
4in the aqueous solution, soak 0.7 minute, soak 1.5 minutes in monomer solution, described monomer solution, for the mixed aqueous solution containing Py and Witco 1298 Soft Acid and salt thereof, repeats aluminium foil cathode portion to be placed in KMnO
4the aqueous solution, soaks in monomer solution 2 times.Wherein, in monomer solution, by adjusting the ratio of Witco 1298 Soft Acid and salt thereof, the mixing solutions of Py of 5min interpolation simultaneously and Witco 1298 Soft Acid and salt thereof, the pH value that makes solution is 1.5; The temperature of monomer solution is 25 ℃, and the temperature of oxidizing solution is outside 35 ℃, and all the other are with embodiment 1.
Embodiment 4:
Remove at KMnO
4in the aqueous solution, soak 0.8 minute, soak 1.5 minutes in monomer solution, described monomer solution, for the mixed aqueous solution containing Py and benzene disulfonic acid and salt thereof, repeats aluminium foil cathode portion to be placed in KMnO
4the aqueous solution, soaks in monomer solution 4 times.Wherein, in monomer solution, by adjusting the ratio of benzene disulfonic acid and salt thereof, the mixing solutions of Py of 8min interpolation simultaneously and benzene disulfonic acid and salt thereof, the pH value that makes solution is 2.0; The temperature of monomer solution is 15 ℃, and the temperature of oxidizing solution is outside 15 ℃, and all the other are with embodiment 1.
Embodiment 5:
Remove at KMnO
4in the aqueous solution, soak 0.9 minute, soak 1.8 minutes in monomer solution, described monomer solution, for the mixed aqueous solution containing Py and camphorsulfonic acid and salt thereof, repeats aluminium foil cathode portion to be placed in the KMnO4 aqueous solution, soaks 3 times in monomer solution.Wherein, in monomer solution, by adjusting the ratio of camphorsulfonic acid and salt thereof, the mixing solutions of Py of 5min interpolation simultaneously and camphorsulfonic acid and salt thereof, the pH value that makes solution is 1.8; The temperature of monomer solution is 50 ℃, and the temperature of oxidizing solution is outside 5 ℃, and all the other are with embodiment 1.
Embodiment 6:
Remove at KMnO
4in the aqueous solution, soak 0.6 minute, soak 1.5 minutes in monomer solution, described monomer solution, for the mixed aqueous solution containing Py and Phenylsulfonic acid and salt thereof, repeats aluminium foil cathode portion to be placed in KMnO
4the aqueous solution, soaks in monomer solution 2 times.Wherein, in monomer solution, by adjusting the ratio of Phenylsulfonic acid and salt thereof, the mixing solutions of Py of 5min interpolation simultaneously and Phenylsulfonic acid and salt thereof, the pH value that makes solution is 1.0; The temperature of monomer solution is 10 ℃, and the temperature of oxidizing solution is outside 5 ℃, and all the other are with embodiment 1.
Embodiment 7:
Remove at KMnO
4in the aqueous solution, soak 0.6 minute, soak 1.5 minutes in monomer solution, described monomer solution, for the mixed aqueous solution containing Py and naphthene sulfonic acid and salt thereof, repeats aluminium foil cathode portion to be placed in KMnO
4the aqueous solution, soaks in monomer solution 2 times.Wherein, in monomer solution, by adjusting the ratio of naphthene sulfonic acid and salt thereof, the mixing solutions of Py of 5min interpolation simultaneously and naphthene sulfonic acid and salt thereof, the pH value that makes solution is 1.8; The temperature of monomer solution is 10 ℃, and the temperature of oxidizing solution is outside 5 ℃, and all the other are with embodiment 1.
Embodiment 8:
Remove at KMnO
4in the aqueous solution, soak 0.6 minute, soak 1.5 minutes in monomer solution, described monomer solution, for the mixed aqueous solution containing Py and dibutyl naphthalene sulfonic acid and salt thereof, repeats aluminium foil cathode portion to be placed in KMnO
4the aqueous solution, soaks in monomer solution 3 times.Wherein, in monomer solution, by adjusting the ratio of dibutyl naphthalene sulfonic acid and salt thereof, the mixing solutions of Py of 5min interpolation simultaneously and dibutyl naphthalene sulfonic acid and salt thereof, the pH value that makes solution is 1.8; The temperature of monomer solution is 20 ℃, and the temperature of oxidizing solution is outside 25 ℃, and all the other are with embodiment 1.
Embodiment 9:
Remove at KMnO
4in the aqueous solution, soak 0.6 minute, soak 1.5 minutes in monomer solution, described monomer solution, for the mixed aqueous solution containing Py and phenol sulfonic acid and salt thereof, repeats aluminium foil cathode portion to be placed in KMnO
4the aqueous solution, soaks in monomer solution 3 times.Wherein, in monomer solution, by adjusting the ratio of phenol sulfonic acid and salt thereof, the mixing solutions of Py of 5min interpolation simultaneously and phenol sulfonic acid and salt thereof, the pH value that makes solution is 1.5; The temperature of monomer solution is 30 ℃, and the temperature of oxidizing solution is outside 35 ℃, and all the other are with embodiment 1.
Embodiment 10:
Remove at KMnO
4in the aqueous solution, soak 0.6 minute, soak 1.5 minutes in monomer solution, described monomer solution, for the mixed aqueous solution containing Py and anthraquinone disulfonic acid and salt thereof, repeats aluminium foil cathode portion to be placed in KMnO
4the aqueous solution, soaks in monomer solution 3 times.Wherein, in monomer solution, by adjusting the ratio of anthraquinone disulfonic acid and salt thereof, the mixing solutions of Py of 5min interpolation simultaneously and anthraquinone disulfonic acid and salt thereof, the pH value that makes solution is 1.8; The temperature of monomer solution is 20 ℃, and the temperature of oxidizing solution is outside 15 ℃, and all the other are with embodiment 1.
Embodiment 11:
Remove at KMnO
4in the aqueous solution, soak 0.6 minute, soak 1.5 minutes in monomer solution, described monomer solution, for the mixed aqueous solution containing Py and sulfosalicylic acid and salt thereof, repeats aluminium foil cathode portion to be placed in KMnO
4the aqueous solution, soaks in monomer solution 3 times.Wherein, in monomer solution, by adjusting the ratio of sulfosalicylic acid and salt thereof, the mixing solutions of Py of 5min interpolation simultaneously and sulfosalicylic acid and salt thereof, the pH value that makes solution is 1.2; The temperature of monomer solution is 25 ℃, and the temperature of oxidizing solution is outside 25 ℃, and all the other are with embodiment 1.
Embodiment 12:
Remove at KMnO
4in the aqueous solution, soak 0.6 minute, soak 1.5 minutes in monomer solution, described monomer solution, for the mixed aqueous solution containing Py and naphthalene disulfonic acid and salt thereof, repeats aluminium foil cathode portion to be placed in KMnO
4the aqueous solution, soaks in monomer solution 3 times.Wherein, in monomer solution, by adjusting the ratio of naphthalene disulfonic acid and salt thereof, the mixing solutions of Py of 5min interpolation simultaneously and naphthalene disulfonic acid and salt thereof, the pH value that makes solution is 1.5; The temperature of monomer solution is 15 ℃, and the temperature of oxidizing solution is outside 15 ℃, and all the other are with embodiment 1.
Embodiment 13:
Remove at KMnO
4in the aqueous solution, soak 0.6 minute, soak 1.5 minutes in monomer solution, described monomer solution, for the mixed aqueous solution containing Py and sulphosalicylic acid and salt thereof, repeats aluminium foil cathode portion to be placed in KMnO
4the aqueous solution, soaks in monomer solution 3 times.Wherein, in monomer solution, by adjusting the ratio of sulphosalicylic acid and salt thereof, the mixing solutions of Py of 10min interpolation simultaneously and sulphosalicylic acid and salt thereof, the pH value that makes solution is 1.0; The temperature of monomer solution is 20 ℃, and the temperature of oxidizing solution is outside 15 ℃, and all the other are with embodiment 1.
Comparative example one:
In chemical polymerization operation, aluminium foil cathode portion is placed in to the KMnO of 0.35M
4in the aqueous solution, soak 1 minute, take out and dry, then in monomer solution, soak 2 minutes, described monomer solution is Py (pyrrole monomer) and the Witco 1298 Soft Acid of 0.5M and the mixed aqueous solution of salt thereof containing 0.45M, take out and dry, repeat aluminium foil cathode portion to be placed in KMnO
4, in the mixed aqueous solution of Py (pyrrole monomer) and p-methyl benzenesulfonic acid and salt thereof, soak 5 times after cleaning, drying at cathode surface, form pre-conductive layer.Wherein, in monomer solution, by adjusting the ratio of Witco 1298 Soft Acid and salt thereof, the mixing solutions of Witco 1298 Soft Acid of 10min interpolation simultaneously and salt thereof, the pH value that makes solution is 2.5; The temperature of controlling monomer solution by water-bath is 55 ℃, and the temperature of oxidizing solution is 40 ℃.
Comparative example two:
In chemical polymerization operation, aluminium foil cathode portion is placed in to the KMnO of 0.35M
4in the aqueous solution, soak 3 minutes, take out and dry, then in monomer solution, soak 3 minutes, described monomer solution is Py (pyrrole monomer) and the camphorsulfonic acid of 0.5M and the mixed aqueous solution of salt thereof containing 0.45M, take out and dry, repeat aluminium foil cathode portion to be placed in KMnO
4, in the mixed aqueous solution of Py (pyrrole monomer) and p-methyl benzenesulfonic acid and salt thereof, soak 8 times after cleaning, drying at cathode surface, form pre-conductive layer.Wherein, in monomer solution, by adjusting the ratio of camphorsulfonic acid and salt thereof, the mixing solutions of camphorsulfonic acid of 8min interpolation simultaneously and salt thereof, the pH value that makes solution is 3.5; The temperature of controlling monomer solution by water-bath is 5 ℃, and the temperature of oxidizing solution is 45 ℃.
Comparative example three:
In chemical polymerization operation, aluminium foil cathode portion is placed in to the KMnO of 0.35M
4in the aqueous solution, soak 4 minutes, take out and dry, then in monomer solution, soak 6 minutes, described monomer solution is Py (pyrrole monomer) and the p-methyl benzenesulfonic acid of 0.5M and the mixed aqueous solution of salt thereof containing 0.45M, take out and dry, repeat aluminium foil cathode portion to be placed in KMnO
4, in the mixed aqueous solution of Py (pyrrole monomer) and p-methyl benzenesulfonic acid and salt thereof, soak 10 times after cleaning, drying at cathode surface, form pre-conductive layer.Wherein, in monomer solution, by adjusting the ratio of p-methyl benzenesulfonic acid and salt thereof, the mixing solutions of p-methyl benzenesulfonic acid of 5min interpolation simultaneously and salt thereof, the pH value that makes solution is 0.3; The temperature of controlling monomer solution by water-bath is 60 ℃, and the temperature of oxidizing solution is 40 ℃.
After above-mentioned chemical polymerization process completes, by electrochemical polymerization, after pre-conductive layer carries out electrolytic polymerization outward again, to the cathode portion of formation electroconductive polymer layer successively coated graphite and silver slurry, by anode and negative electrode are set, form capacitor body; Finally with epoxy resin by capacitor body molded packages.
Effect comparison
By upper Biao Ke get, the embodiment of the present invention is compared with comparative example, and leakage current characteristic and the characteristic under hot and humid environment of the solid polymer aluminium electrolutic capacitor preparing are better.
Although more than described the specific embodiment of the present invention; but being familiar with those skilled in the art is to be understood that; our described specific embodiment is illustrative; rather than for the restriction to scope of the present invention; those of ordinary skill in the art are in equivalent modification and the variation done according to spirit of the present invention, all should be encompassed in the scope that claim of the present invention protects.
Claims (5)
1. a chemical polymerization process of preparing polypyrrole, it is characterized in that: chemical polymerization adopts the stable monomer solution of monomer concentration, and the pH value of monomer solution is controlled at 0.5-2.0, and the temperature of monomer solution is controlled at 10-50 ℃, the immersion liquid time of monomer solution is 1-2 minute; The temperature of the oxidation solution that chemical polymerization is used is controlled at 5-35 ℃, and the immersion liquid time of oxidation solution is 0.5-1 minute, and cycle index is 2-4 time.
2. a kind of chemical polymerization process of preparing polypyrrole according to claim 1, is characterized in that: the pH value of described monomer concentration and monomer solution is added and contained monomer and doping agent mixed solution is controlled by timing.
3. the chemical polymerization process of preparing polypyrrole according to claim 2, is characterized in that: described timing is added to every 5-10min to be added once.
4. a kind of chemical polymerization process of preparing polypyrrole according to claim 2, is characterized in that: described monomer solution comprises pyrrole monomer and doping agent.
5. a kind of chemical polymerization process of preparing polypyrrole according to claim 4, is characterized in that: described doping agent comprises any in p-methyl benzenesulfonic acid and salt, Witco 1298 Soft Acid and salt thereof, dodecyl sodium sulfonate and salt thereof, camphorsulfonic acid and salt thereof, Phenylsulfonic acid and salt thereof, naphthene sulfonic acid and salt thereof, dibutyl naphthalene sulfonic acid and salt thereof, phenol sulfonic acid and salt, sulphosalicylic acid and salt thereof, sulfosalicylic acid and salt thereof, naphthalene disulfonic acid and salt thereof, benzene disulfonic acid and salt thereof, anthraquinone disulfonic acid and salt thereof.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113444365A (en) * | 2021-07-13 | 2021-09-28 | 浙江科技学院 | Hybrid doped polypyrrole paper-based flexible electrode material and preparation method thereof |
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| CN113444365A (en) * | 2021-07-13 | 2021-09-28 | 浙江科技学院 | Hybrid doped polypyrrole paper-based flexible electrode material and preparation method thereof |
| CN113444365B (en) * | 2021-07-13 | 2022-05-31 | 浙江科技学院 | Hybrid doped polypyrrole paper-based flexible electrode material and preparation method thereof |
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Application publication date: 20140924 |