CN107236086B - Conductive polymerization dispersion liquid and high-voltage solid-state capacitance conductive polymer emulsion - Google Patents
Conductive polymerization dispersion liquid and high-voltage solid-state capacitance conductive polymer emulsion Download PDFInfo
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F265/00—Macromolecular compounds obtained by polymerising monomers on to polymers of unsaturated monocarboxylic acids or derivatives thereof as defined in group C08F20/00
- C08F265/04—Macromolecular compounds obtained by polymerising monomers on to polymers of unsaturated monocarboxylic acids or derivatives thereof as defined in group C08F20/00 on to polymers of esters
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- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/14—Methyl esters, e.g. methyl (meth)acrylate
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- C08L2201/52—Aqueous emulsion or latex, e.g. containing polymers of a glass transition temperature (Tg) below 20°C
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Abstract
The invention provides a conductive polymerization dispersion liquid and a high-voltage solid-state capacitance conductive polymer emulsion, which comprise the following steps: adding acrylic ester, acrylamide and an emulsifier into a sodium polystyrene sulfonate aqueous solution, and performing emulsion polymerization by taking ammonium persulfate as an initiator; then adding an EDOT monomer into the polymerized emulsion, taking ferric sulfate as a catalyst, and simultaneously dropwise adding sodium persulfate as an oxidant to obtain a mixed solution; removing residual unreacted organic monomers and inorganic salt components in the liquid from the mixed liquid; then polyglycerol, wetting agent and conductivity enhancer are added into the mixture, and homogenization is carried out under high pressure. The invention also comprises the application of the dispersion obtained by the method to the preparation of the solid electrolytic capacitor. The invention synthesizes the water dispersion of the conductive polymer, then purifies and removes the impurity, then impregnates and dries as the electrolyte of the capacitor, there is no impurity damaging the oxide film in the impregnation liquid, the leakage current of the capacitor is reduced, and the withstand voltage of the product is improved.
Description
Technical Field
The invention belongs to the technical field of solid electrolytic capacitor preparation, and particularly relates to a conductive polymer dispersion with high solid content in a solid electrolytic capacitor.
Background
The conductive polymer solid-state capacitor has excellent high-frequency low-resistance characteristics, has wider application fields in various applications, and has the trend of gradually replacing the original liquid electrolytic capacitor along with the reduction of cost. However, under the superior impedance characteristic and life characteristic, the solid capacitor has obvious disadvantages compared with the traditional liquid electrolytic capacitor, because the solid capacitor is prepared by adopting monomers and oxidants to polymerize in situ in a capacitor core bag, and strong acid iron p-toluenesulfonate is adopted as the oxidants and dopants to damage the oxide film of the anode foil, the leakage current is large, the product leakage current is usually in the range of 100 mu A-300 mu A, the leakage current of the liquid capacitor is usually below 1 mu A, and the difference of the two is very large; and the voltage endurance is not high, so that the voltage endurance can only be used for products below 35V at present, and products with higher voltage are difficult to achieve products above 100V, and more particularly products above 400V due to the characteristics of the conductive polymer.
The existing conductive polymer dispersion has low solid content and high viscosity, is introduced into a capacitor core package in a soaking and drying mode, and is difficult to improve the filling rate of the conductive polymer in the core package, so that the characteristics of capacity extraction, ESR and the like are poor, and particularly the low-temperature performance is difficult to reach the standard. The present invention has found in the study that the existing conductive polymer dispersion is different from the conventional polymer emulsion (emulsion synthesized by emulsion polymerization, the solid content can often reach 30%, the viscosity is moderate, and the viscosity stability is good), and the solid content tends to rise very fast along with the viscosity. The viscosity becomes very high after the solid content reaches 2.5%, and although the viscosity can be reduced by high-pressure homogenization, the viscosity stability is insufficient, the viscosity can be greatly increased in the placing process until the fluidity is lost, and the capacitor core bag cannot be used. According to analysis, the conductive polymer PEDOT/PSSA presents a string shape in water, the doped dispersing agent is polystyrene sulfonic acid, the water solubility is good, the conductive polymer PEDOT/PSSA presents a stretching state in water, the interface of latex particles is not obvious, hydrophilic groups are in a diastole state in water phase, and the hydrophilic groups are entangled with each other, so that the viscosity of the system is high and aggregation is easy to cause a severe increase of the viscosity. However, conventional emulsions tend to form granular emulsions in which the hydrophobic polymer is surrounded by hydrophilic groups which, because of their encapsulation, stabilize the emulsion and do not spread in the free state in water, and thus have a relatively low viscosity.
However, the conductive polymer dispersion has the defects of low solid content and high viscosity; the conductive polymer is introduced into the capacitor core package in an impregnation drying mode, so that the filling rate of the conductive polymer in the core package is difficult to improve, the characteristics of capacity extraction, ESR and the like are poor, and particularly the low-temperature performance is difficult to reach the standard.
Disclosure of Invention
The invention aims to: in order to solve the defects in the prior art, the invention provides a conductive polymer dispersion liquid and a high-voltage solid capacitor conductive polymer emulsion, which have lower viscosity, and are used for improving the ESR (equivalent series resistance) characteristic and reducing the electric leakage quantity of a solid capacitor, so that the integral performance of the solid capacitor is improved.
The technical scheme is as follows: in order to solve the technical problems, the invention adopts the following technical scheme: a method for preparing a conductive polymeric dispersion comprising the steps of:
(1) Sodium polystyrene sulfonate is used as an emulsifier, acrylic ester and acrylamide are used as comonomers, a compound emulsifier is added, and polymerization reaction is carried out under the action of an initiator ammonium persulfate to obtain polyacrylate emulsion; the reaction temperature is 70-90 degrees, and the reaction time is 2-8 hours;
(2) Adding the polyacrylate emulsion obtained in the step (1) into a container subjected to nitrogen replacement and taking the polyacrylate emulsion as a core material, then adding an EDOT monomer and deionized water, stirring and dispersing to form emulsion, continuously adding an oxidant sodium persulfate and a catalyst ferric sulfate to react for at least 24 hours, and obtaining a crude product of the conductive polymerization dispersion liquid with the solid content of 2-5 percent after the reaction is finished;
(3) Purifying the crude product of the conductive polymerization dispersion liquid obtained in the step (2) to remove unreacted organic monomers and inorganic salts, thereby obtaining a purified conductive polymerization dispersion liquid product.
Preferably, the acrylate is methacrylate, acrylate or acrylonitrile.
Preferably, the compound emulsifier is an anionic emulsifier or a cationic emulsifier.
Preferably, the anionic emulsifier is sodium dodecyl sulfonate, sodium ricinoleate or JS-20; the cationic emulsifier is alkyl ammonium salt or quaternary ammonium salt.
Preferably, the mass ratio of the emulsifier to the compound emulsifier is 500-2000:1.
Preferably, the mass ratio of the emulsifier to the polyacrylate is 1-20:1.
Preferably, the mass ratio of the EDOT monomer to the polyacrylate in the step (2) is 1:1-10.
Preferably, the molar ratio of the oxidant sodium persulfate to the EDOT monomer in the step (2) is 1-2:1.
Preferably, the ammonium persulfate initiator in the step (1) is added in an amount of 0.1 to 1% by weight based on the total weight of the comonomer.
The invention also provides a high-voltage solid-state capacitance conductive polymer emulsion based on the conductive polymerization dispersion liquid, which comprises the following components in parts by mass:
and adjusting the pH to be within the range of 6+/-0.5, homogenizing under high pressure, and ending.
The beneficial effects are that: the invention synthesizes the water dispersion of the conductive polymer, purifies and removes the impurity harmful to the capacitor, then impregnates and dries as the electrolyte of the capacitor, because the impurity damaging the oxide film does not exist in the impregnation liquid, the leakage of the capacitor is reduced, and the withstand voltage of the product is improved. The acrylate emulsion as the inner core plays a role of a binder, and in the process of the aqueous dispersion polymerization, the monomer is adsorbed inside the acrylate emulsion, and the doping agent PSSA is wrapped outside the emulsion, so that the oxidation polymerization reaction is accelerated. The obtained PEDOT/PSSA is used as a hydrophilic shell layer, the hydrophobic polyacrylate is used as a stable emulsion system of an inner core, the viscosity is greatly reduced compared with that of a single solid-containing PEDOT/PSSA, the system is more stable, and the solid-state capacitor is used in a solid-state capacitor, so that various performance indexes of the capacitor are greatly improved.
Detailed Description
The present invention is further described below with reference to specific embodiments, which are to be understood as being merely illustrative of the present invention and not limiting to the scope of the present invention, and various equivalent modifications of the present invention will fall within the scope of the appended claims to the person skilled in the art after reading the present invention.
The invention adopts acrylic ester emulsion as the inner core, and the hydrophilic dispersing agent is coated outside the acrylic ester emulsion to form stable emulsion. The acrylate emulsion as the inner core can not only play a role of a binder, but also adsorb monomers in the acrylate emulsion in the process of aqueous dispersion polymerization, and PSSA as a doping agent is wrapped outside the emulsion, so that the oxidation polymerization reaction can be accelerated. The obtained PEDOT/PSSA is used as a hydrophilic shell layer, the hydrophobic polyacrylate is used as a stable emulsion system of an inner core, the viscosity is greatly reduced compared with the pure PEDOT/PSSA with the same solid content, the system is more stable, and the solid-state capacitor is used for solid-state capacitors, so that various performance indexes are greatly improved. The preparation process comprises the following steps:
example 1
Preparation of polystyrene sulfonic acid coated polyacrylate emulsion:
2000 g of aqueous solution of 10% sodium polystyrene sulfonate is added into a three-mouth bottle after nitrogen replacement, the temperature is raised to 80 ℃, 40 g of methyl methacrylate and 10 g of acrylamide are added, 0.2 g of emulsifying agent JS-20 is added to form emulsion, 0.3 g of ammonium persulfate is added to react for 4 hours, after the mixture is cooled to room temperature, 50mL of cation exchange resin is added, stirring is carried out for 1 hour, and the exchange resin is removed by filtration, thus obtaining 2000mL of polyacrylate emulsion coated with polystyrene sulfonic acid, the solid content is measured to be 10%, and the particle size of the emulsion is 0.2um.
Preparation of conductive polymer dispersion liquid with acrylate emulsion as core:
1000 g of polyacrylic emulsion with the solid content of 10% is added into a three-mouth bottle replaced by nitrogen, 20 g of EDOT monomer is added, the mixture is stirred and dispersed to be emulsion, and 1500 g of deionized water is added to obtain mixed emulsion. 40 g of sodium persulfate and 0.1 g of ferric sulfate are taken and added into 480 g of deionized water, after stirring and dissolving, the mixture is fully replaced by nitrogen, and all the mixture is dropwise added into the mixed emulsion in 2 hours, and stirring and reaction are continued for 24 hours. After the reaction was completed, 500mL of anion exchange resin and 300mL of cation exchange resin were added, and the mixture was stirred for 4 hours, followed by filtration to obtain a conductive polymer dispersion.
Preparing high-pressure impregnation liquid:
1000mL of the conductive polymer dispersion was taken, 200 g of polyglycerol, 25 g of acrylamide and 1 g of wetting dispersant were added, the pH of the mixed liquid was adjusted to 6, and then high-pressure homogenization was performed by a high-pressure homogenizer to obtain a stable conductive polymer emulsion having a particle size of 0.2 to 0.3. Mu.m.
Example 2
Preparation of polystyrene sulfonic acid coated polyacrylate emulsion:
2000 g of aqueous solution of 10% sodium polystyrene sulfonate is added into a three-mouth bottle after nitrogen replacement, the temperature is raised to 80 ℃, 15 g of methyl methacrylate and 8 g of acrylamide are added, 0.3 g of sodium ricinoleate serving as a compound emulsifier is added to form emulsion, 0.2 g of ammonium persulfate is added to react for 4 hours, 50mL of quaternary ammonium salt cation exchange resin is added after the mixture is cooled to room temperature, stirring is carried out for 1 hour, and the exchange resin is filtered to obtain 2000mL of polyacrylate emulsion coated with polystyrene sulfonic acid, the solid content is determined to be 8%, and the particle size of the emulsion is 0.2um.
Preparation of conductive polymer dispersion liquid with acrylate emulsion as core:
1000 g of polyacrylic emulsion with the solid content of 8% is added into a three-mouth bottle replaced by nitrogen, 15 g of EDOT monomer is added, the mixture is stirred and dispersed to be emulsion, and 1500 g of deionized water is added to obtain mixed emulsion. 35 g of sodium persulfate and 0.1 g of ferric sulfate are taken and added into 480 g of deionized water, after stirring and dissolving, the mixture is fully replaced by nitrogen, and all the mixture is dropwise added into the mixed emulsion in 2 hours, and stirring and reaction are continued for 24 hours. After the reaction was completed, 500mL of anion exchange resin and 300mL of cation exchange resin were added, and the mixture was stirred for 4 hours, followed by filtration to obtain a conductive polymer dispersion.
Preparing high-pressure impregnation liquid:
1000mL of the conductive polymer dispersion was taken, 200 g of polyglycerol, 25 g of acrylamide and 1 g of wetting dispersant were added, the pH of the mixed liquid was adjusted to 6, and then high-pressure homogenization was performed by a high-pressure homogenizer to obtain a stable conductive polymer emulsion having a particle size of 0.2 to 0.3. Mu.m.
Example 3
Preparation of polystyrene sulfonic acid coated polyacrylate emulsion:
2000 g of aqueous solution of 10% sodium polystyrene sulfonate is added into a three-mouth bottle after nitrogen replacement, the temperature is raised to 80 ℃, 65 g of methyl methacrylate and 12 g of acrylamide are added, 0.5 g of sodium ricinoleate serving as a compound emulsifier is added to form emulsion, 0.2 g of ammonium persulfate is added to react for 4 hours, 50mL of quaternary ammonium salt cation exchange resin is added after the mixture is cooled to room temperature, stirring is carried out for 1 hour, and the exchange resin is filtered to obtain 2000mL of polyacrylate emulsion coated with polystyrene sulfonic acid, the solid content is determined to be 11%, and the particle size of the emulsion is 0.2um.
Preparation of conductive polymer dispersion liquid with acrylate emulsion as core:
1000 g of polyacrylic emulsion with 11% solid content is added into a three-mouth bottle replaced by nitrogen, 30 g of EDOT monomer is added, the mixture is stirred and dispersed to be emulsion, and 1500 g of deionized water is added to obtain mixed emulsion. 35 g of sodium persulfate and 0.1 g of ferric sulfate are taken and added into 480 g of deionized water, after stirring and dissolving, the mixture is fully replaced by nitrogen, and all the mixture is dropwise added into the mixed emulsion in 2 hours, and stirring and reaction are continued for 24 hours. After the reaction was completed, 500mL of anion exchange resin and 300mL of cation exchange resin were added, and the mixture was stirred for 4 hours, followed by filtration to obtain a conductive polymer dispersion.
Preparing high-pressure impregnation liquid:
1000mL of the conductive polymer dispersion was taken, 200 g of polyglycerol, 25 g of acrylamide and 1 g of wetting dispersant were added, the pH of the mixed liquid was adjusted to 6, and then high-pressure homogenization was performed by a high-pressure homogenizer to obtain a stable conductive polymer emulsion having a particle size of 0.2 to 0.3. Mu.m.
Preparing a high-voltage solid capacitor by the conductive polymer emulsion: cutting, nailing, welding, forming and carbonizing the aluminum foil to obtain capacitor elements, immersing the capacitor elements in the high-pressure immersion liquid to fully absorb the liquid medicine to form a high polymer, filling the high polymer into an aluminum shell, sealing the aluminum shell with a girdle, sealing and assembling, aging and repairing the electric performance by high Wen Tongdian, testing various large characteristic parameters of the capacitor by 100%, and finally cutting feet, packaging and warehousing.
Comparative example: and directly immersing the capacitor element into the polymer-containing PEDOT/PSSA for in-situ polymerization, and sequentially carrying out procedures of assembly packaging, aging, pin cutting, packaging, warehousing and the like to obtain the high-molecular conductive polymer solid capacitor. The performance of the prepared high-voltage solid capacitor is tested, and the test results are shown in the following table 1:
Claims (10)
1. a method for preparing a conductive polymeric dispersion comprising the steps of:
(1) Sodium polystyrene sulfonate is used as an emulsifier, acrylic ester and acrylamide are used as comonomers, a compound emulsifier is added, and polymerization reaction is carried out under the action of an initiator ammonium persulfate to obtain polyacrylate emulsion; the reaction temperature is 70-90 degrees, and the reaction time is 2-8 hours;
(2) Adding the polyacrylate emulsion obtained in the step (1) into a container subjected to nitrogen replacement and taking the polyacrylate emulsion as a core material, then adding an EDOT monomer and deionized water, stirring and dispersing to form emulsion, continuously adding an oxidant sodium persulfate and a catalyst ferric sulfate to react for at least 24 hours, and obtaining a crude product of the conductive polymerization dispersion liquid with the solid content of 2-5 percent after the reaction is finished;
(3) Purifying the crude product of the conductive polymerization dispersion liquid obtained in the step (2) to remove unreacted organic monomers and inorganic salts, thereby obtaining a purified conductive polymerization dispersion liquid product.
2. The method for producing a conductive polymer dispersion according to claim 1, wherein: the acrylic ester is methyl acrylic ester, acrylic ester or acrylonitrile.
3. The method for producing a conductive polymer dispersion according to claim 1, wherein: the compound emulsifier is an anionic emulsifier or a cationic emulsifier.
4. A method for producing a conductive polymeric dispersion according to claim 3, characterized in that: the anionic emulsifier is sodium dodecyl sulfonate, sodium ricinoleate or JS-20; the cationic emulsifier is alkyl ammonium salt or quaternary ammonium salt.
5. The method for producing a conductive polymer dispersion according to any one of claims 1 to 4, characterized in that: the mass ratio of the emulsifier to the compound emulsifier is 500-2000:1.
6. The method for producing a conductive polymer dispersion according to claim 5, wherein: the mass ratio of the emulsifier to the polyacrylate is 1-20:1.
7. The method for producing a conductive polymer dispersion according to claim 5, wherein: in the step (2), the mass ratio of the EDOT monomer to the polyacrylate is 1:1-10.
8. The method for producing a conductive polymer dispersion according to claim 5, wherein: in the step (2), the molar ratio of the oxidant sodium persulfate to the EDOT monomer is 1-2:1.
9. A method for producing a conductive polymeric dispersion according to claim 3, characterized in that: the addition amount of the ammonium persulfate initiator in the step (1) is 0.1-1% of the total weight of the comonomer.
10. A high voltage solid state capacitive conductive polymer emulsion based on the conductive polymeric dispersion of claim 1 comprising the following mass components:
and adjusting the pH to be within the range of 6+/-0.5, homogenizing under high pressure, and ending.
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| CN112759996B (en) * | 2020-12-31 | 2022-03-15 | 江苏富琪森新材料有限公司 | PEDOT/polyacrylate modified polythiophene antistatic material and preparation method thereof |
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| CN101977960A (en) * | 2008-01-22 | 2011-02-16 | H.C.斯达克克莱维欧斯有限公司 | Method for the production of conductive polymers |
| CN104211969A (en) * | 2014-09-10 | 2014-12-17 | 万星光电子(东莞)有限公司 | Preparation method of PEDOT/PSS dispersion liquid and preparation method of high pressure solid capacitor |
| CN105143302A (en) * | 2013-03-11 | 2015-12-09 | 昭和电工株式会社 | Method for producing conductive polymer-containing dispersion |
| CN105884955A (en) * | 2014-12-15 | 2016-08-24 | 江南大学 | Preparation method of waterborne dispersant and conductive dispersion liquid |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101977960A (en) * | 2008-01-22 | 2011-02-16 | H.C.斯达克克莱维欧斯有限公司 | Method for the production of conductive polymers |
| CN105143302A (en) * | 2013-03-11 | 2015-12-09 | 昭和电工株式会社 | Method for producing conductive polymer-containing dispersion |
| CN104211969A (en) * | 2014-09-10 | 2014-12-17 | 万星光电子(东莞)有限公司 | Preparation method of PEDOT/PSS dispersion liquid and preparation method of high pressure solid capacitor |
| CN105884955A (en) * | 2014-12-15 | 2016-08-24 | 江南大学 | Preparation method of waterborne dispersant and conductive dispersion liquid |
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| 以聚苯乙烯磺酸钠接枝聚乙二醇为模板的聚3,4-二氧乙烯噻吩水分散体的制备及性能;顾佳欢等;高分子材料科学与工程(第07期);147-152 * |
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