CN111524709A - Working electrolyte for flame-retardant high-voltage aluminum electrolytic capacitor and preparation method thereof - Google Patents
Working electrolyte for flame-retardant high-voltage aluminum electrolytic capacitor and preparation method thereof Download PDFInfo
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- CN111524709A CN111524709A CN202010342008.1A CN202010342008A CN111524709A CN 111524709 A CN111524709 A CN 111524709A CN 202010342008 A CN202010342008 A CN 202010342008A CN 111524709 A CN111524709 A CN 111524709A
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- 239000003063 flame retardant Substances 0.000 title claims abstract description 88
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title claims abstract description 87
- 239000003990 capacitor Substances 0.000 title claims abstract description 81
- 239000003792 electrolyte Substances 0.000 title claims abstract description 70
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 68
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 68
- 238000002360 preparation method Methods 0.000 title abstract description 16
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 46
- 239000002904 solvent Substances 0.000 claims abstract description 42
- 239000002994 raw material Substances 0.000 claims abstract description 32
- 150000007522 mineralic acids Chemical class 0.000 claims abstract description 26
- 239000000654 additive Substances 0.000 claims abstract description 20
- 230000000996 additive effect Effects 0.000 claims abstract description 20
- 150000007524 organic acids Chemical class 0.000 claims abstract description 19
- 239000000203 mixture Substances 0.000 claims description 58
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical group OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 30
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical group OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 30
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 24
- -1 carbon chain carboxylic acid ammonium salt Chemical class 0.000 claims description 21
- 238000001816 cooling Methods 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 12
- 239000005543 nano-size silicon particle Substances 0.000 claims description 12
- 235000012239 silicon dioxide Nutrition 0.000 claims description 12
- 239000013538 functional additive Substances 0.000 claims description 11
- OTLNPYWUJOZPPA-UHFFFAOYSA-N 4-nitrobenzoic acid Chemical compound OC(=O)C1=CC=C([N+]([O-])=O)C=C1 OTLNPYWUJOZPPA-UHFFFAOYSA-N 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 229920000642 polymer Polymers 0.000 claims description 5
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 claims description 5
- OTRAYOBSWCVTIN-UHFFFAOYSA-N OB(O)O.OB(O)O.OB(O)O.OB(O)O.OB(O)O.N.N.N.N.N.N.N.N.N.N.N.N.N.N.N Chemical compound OB(O)O.OB(O)O.OB(O)O.OB(O)O.OB(O)O.N.N.N.N.N.N.N.N.N.N.N.N.N.N.N OTRAYOBSWCVTIN-UHFFFAOYSA-N 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- AFPHTEQTJZKQAQ-UHFFFAOYSA-N 3-nitrobenzoic acid Chemical compound OC(=O)C1=CC=CC([N+]([O-])=O)=C1 AFPHTEQTJZKQAQ-UHFFFAOYSA-N 0.000 claims description 3
- JKTYGPATCNUWKN-UHFFFAOYSA-N 4-nitrobenzyl alcohol Chemical compound OCC1=CC=C([N+]([O-])=O)C=C1 JKTYGPATCNUWKN-UHFFFAOYSA-N 0.000 claims description 3
- BTJIUGUIPKRLHP-UHFFFAOYSA-N 4-nitrophenol Chemical compound OC1=CC=C([N+]([O-])=O)C=C1 BTJIUGUIPKRLHP-UHFFFAOYSA-N 0.000 claims description 3
- DIBUFQMCUZYQKN-UHFFFAOYSA-N butyl diphenyl phosphate Chemical compound C=1C=CC=CC=1OP(=O)(OCCCC)OC1=CC=CC=C1 DIBUFQMCUZYQKN-UHFFFAOYSA-N 0.000 claims description 3
- YICSVBJRVMLQNS-UHFFFAOYSA-N dibutyl phenyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OC1=CC=CC=C1 YICSVBJRVMLQNS-UHFFFAOYSA-N 0.000 claims description 3
- DQWPFSLDHJDLRL-UHFFFAOYSA-N triethyl phosphate Chemical compound CCOP(=O)(OCC)OCC DQWPFSLDHJDLRL-UHFFFAOYSA-N 0.000 claims description 3
- 239000004411 aluminium Substances 0.000 claims description 2
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 2
- 239000004327 boric acid Substances 0.000 claims description 2
- XZZNDPSIHUTMOC-UHFFFAOYSA-N triphenyl phosphate Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)(=O)OC1=CC=CC=C1 XZZNDPSIHUTMOC-UHFFFAOYSA-N 0.000 claims description 2
- 230000009286 beneficial effect Effects 0.000 abstract description 4
- 238000009776 industrial production Methods 0.000 abstract description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 20
- 230000000052 comparative effect Effects 0.000 description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 15
- 238000006243 chemical reaction Methods 0.000 description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 11
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 10
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 10
- HTZCNXWZYVXIMZ-UHFFFAOYSA-M benzyl(triethyl)azanium;chloride Chemical compound [Cl-].CC[N+](CC)(CC)CC1=CC=CC=C1 HTZCNXWZYVXIMZ-UHFFFAOYSA-M 0.000 description 10
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 description 10
- 238000010992 reflux Methods 0.000 description 10
- 238000007127 saponification reaction Methods 0.000 description 10
- JKNCOURZONDCGV-UHFFFAOYSA-N 2-(dimethylamino)ethyl 2-methylprop-2-enoate Chemical compound CN(C)CCOC(=O)C(C)=C JKNCOURZONDCGV-UHFFFAOYSA-N 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 5
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 229960002089 ferrous chloride Drugs 0.000 description 5
- ZUVVLBGWTRIOFH-UHFFFAOYSA-N methyl 4-methyl-2-[(4-methylphenyl)sulfonylamino]pentanoate Chemical compound COC(=O)C(CC(C)C)NS(=O)(=O)C1=CC=C(C)C=C1 ZUVVLBGWTRIOFH-UHFFFAOYSA-N 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 239000011888 foil Substances 0.000 description 4
- 238000011156 evaluation Methods 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- OWCLRJQYKBAMOL-UHFFFAOYSA-N 2-butyloctanedioic acid Chemical compound CCCCC(C(O)=O)CCCCCC(O)=O OWCLRJQYKBAMOL-UHFFFAOYSA-N 0.000 description 1
- 206010000369 Accident Diseases 0.000 description 1
- SPAUYKHQVLTCOL-UHFFFAOYSA-N C1(=CC=CC=C1)OP(OC1=CC=CC=C1)(O)=O.C1(=CC=CC=C1)C Chemical compound C1(=CC=CC=C1)OP(OC1=CC=CC=C1)(O)=O.C1(=CC=CC=C1)C SPAUYKHQVLTCOL-UHFFFAOYSA-N 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- 239000004820 Pressure-sensitive adhesive Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000002788 crimping Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000011244 liquid electrolyte Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/004—Details
- H01G9/022—Electrolytes; Absorbents
- H01G9/035—Liquid electrolytes, e.g. impregnating materials
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/145—Liquid electrolytic capacitors
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
Abstract
The invention relates to the technical field of capacitors, in particular to an electrolyte for a flame-retardant aluminum electrolytic capacitor and a preparation method thereof. The working electrolyte for the flame-retardant high-voltage aluminum electrolytic capacitor comprises the following raw materials in parts by weight: 2.5-15 parts of inorganic acid, 5-10 parts of organic acid, 0.1-5 parts of flame-retardant auxiliary agent, 0.1-2 parts of auxiliary additive and 70-90 parts of solvent. According to the invention, the inorganic acid is adopted to replace part of the organic acid, the flame-retardant auxiliary agent and the auxiliary additive are added, the consumption of the raw materials is adjusted, and the raw materials are matched with each other, so that the electrolyte has good flame retardance and thermal stability, can be used as a flame-retardant high-voltage working electrolyte, is suitable for a flame-retardant high-voltage aluminum electrolytic capacitor, has good working performance, obviously improves the use safety of the capacitor, has a simple and efficient preparation method, is convenient to control, and is beneficial to industrial production.
Description
Technical Field
The invention relates to the technical field of capacitors, in particular to an electrolyte for a flame-retardant aluminum electrolytic capacitor.
Background
An aluminum electrolytic capacitor is a capacitor made by using an aluminum cylinder as a negative electrode, filling liquid electrolyte in the aluminum cylinder and inserting a bent aluminum strip as a positive electrode, and is called as an aluminum electrolytic capacitor. It is a general electrolytic capacitor made of aluminium material with good electric property, wide application range and high reliability. However, most of the existing aluminum electrolytic capacitors have flammability problems due to the adoption of flammable organic acid electrolyte, wherein, the high-voltage large aluminum electrolytic capacitors have very high accumulated energy during working, have more electrolyte content and have strict limitation on water content, so that the high-voltage large aluminum electrolytic capacitors have greater safety problems of flammability, explosiveness and the like. With the market quality feedback, the fire accidents of the whole machine caused by the aluminum electrolytic capacitor have occupied a non-negligible proportion. Therefore, the problem of flame retardance of the aluminum electrolytic capacitor needs to be solved, the flame retardance of the aluminum electrolytic capacitor is improved, and the comprehensive use performance of the aluminum electrolytic capacitor is not influenced.
Disclosure of Invention
In order to overcome the defects and shortcomings in the prior art, the invention provides a working electrolyte for a flame-retardant high-voltage aluminum electrolytic capacitor, which has good flame retardancy and thermal stability.
The invention also aims to provide a preparation method of the working electrolyte for the flame-retardant high-voltage aluminum electrolytic capacitor, which is simple to operate, convenient to control, high in production efficiency and beneficial to industrial production.
One of the purposes of the invention is realized by the following technical scheme: the working electrolyte for the flame-retardant high-voltage aluminum electrolytic capacitor comprises the following raw materials in parts by weight:
2.5-15 parts of inorganic acid
5-10 parts of organic acid
0.1-5 parts of flame-retardant auxiliary agent
0.1-2 parts of auxiliary additive
70-90 parts of a solvent.
According to the invention, inorganic acid is adopted to replace part of organic acid, the flame-retardant auxiliary agent and the auxiliary additive are added, the consumption of the raw materials is adjusted, and the raw materials are matched with each other, so that the electrolyte has good flame retardance and thermal stability, is used as a flame-retardant high-voltage working electrolyte, and is suitable for a flame-retardant high-voltage aluminum electrolytic capacitor.
Further, each part of the solvent comprises the following raw materials in parts by weight: 50-60 parts of main solvent and 20-30 parts of auxiliary solvent. Further, the main solvent is ethylene glycol, and the auxiliary solvent is diethylene glycol.
The invention adopts the ethylene glycol as the main solvent and the diethylene glycol as the auxiliary solvent, has good solubility and compatibility to inorganic acid, organic acid, auxiliary additive and flame retardant additive, low viscosity and large dielectric constant, and the two raw materials are matched with each other, thereby improving the viscosity of the electrolyte and the oxidation efficiency of the electrolyte, and improving the flash voltage of the electrolyte, the ethylene glycol and the diethylene glycol. The mixed solvent can improve the electrical property and stability of the electrolyte, and is safe and environment-friendly to use.
Further, the organic acid is long carbon chain carboxylic acid ammonium salt with a branched chain.
Further, the preparation method of the branched long-carbon-chain carboxylic acid ammonium salt comprises the following steps:
(1) according to molar parts, taking 1-1.2 parts of cyclohexanone, 1-1.5 parts of hydrogen peroxide, 2-3 parts of ethanol, 0.2-0.6 part of phosphoric acid and 0.15-0.25 part of benzyltriethylammonium chloride to react for 20-30min at the temperature of 6-12 ℃ to obtain a mixture A;
(2) adding 0.5-0.9 part of dimethylaminoethyl methacrylate, 0.4-0.8 part of methyl methacrylate, 1-1.8 parts of ferrous chloride and 0.3-0.6 part of phosphoric acid into the mixture A obtained in the step (1) to react at the temperature of-5 to-0 ℃ for 5-7 hours to obtain a mixture B;
(3) adding the mixture B obtained in the step (2) into a sodium hydroxide solution for saponification reaction to obtain a mixture C;
(4) acidizing the mixture C obtained in the step (3) by using inorganic acid to obtain a mixture D;
(5) and (4) introducing ammonia gas into the mixture D obtained in the step (4) to carry out ammoniation reaction, wherein the pH value at the end of the reaction is 7.2-7.6. Obtaining the long carbon chain carboxylic acid ammonium salt with the branched chain.
Further, in the step (3), the reflux temperature of the saponification reaction is 95-105 ℃, and the reflux time is 4-5 h.
Further, in the step (4), the inorganic acid is sulfuric acid with a mass percentage of 30-50%, and the reaction end point is a pH value of 2-3.
By adopting the long-carbon-chain ammonium carboxylate, the invention has good solubility and thermal stability in the solvent, and has the characteristics of high flash voltage, high conductivity, high pressure resistance, high heat-resistant stability and the like, so that the prepared capacitor has the advantages of high pressure resistance, high heat resistance, low effective resistance and the like, and the service life is long.
Further, the inorganic acid is at least one of boric acid and ammonium pentaborate. According to the invention, inorganic acid is adopted to replace part of organic acid, the flame-retardant auxiliary agent and the auxiliary additive are added, the dosage of each raw material is adjusted, and the raw materials are matched with each other, so that the electrolyte has good flame retardance and thermal stability.
Further, the auxiliary additive is at least one of p-nitrobenzoic acid, p-nitrobenzyl alcohol, m-nitrobenzoic acid and p-nitrophenol. By adopting the auxiliary additive, the effects of hydrogen elimination and water prevention can be achieved, the influence on the conductivity of the electrolyte is small, and the electrolyte can keep higher conductivity under the condition of high flash power voltage, so that the flame retardance, the thermal stability and the comprehensive use performance of the working electrolyte for the flame-retardant high-voltage aluminum electrolytic capacitor are improved.
Further, the flame retardant auxiliary agent comprises at least one of triethyl phosphate, tributyl phosphate, toluene-diphenyl phosphate, triphenyl phosphate, dibutyl-phenyl phosphate and butyl-diphenyl phosphate. By adopting the flame-retardant auxiliary agent, the electrolyte has good flame-retardant effect and higher conductivity and sparking voltage.
Further, the working electrolyte for the flame-retardant high-voltage aluminum electrolytic capacitor also comprises 1-3 parts by weight of functional auxiliary agent, wherein the functional auxiliary agent is at least one of nano silicon dioxide and polyhydroxy high molecular polymer.
Further, the working electrolyte for the flame-retardant high-voltage aluminum electrolytic capacitor also comprises 1-3 parts by weight of functional additives. Further, the functional assistant is at least one of nano silicon dioxide and polyhydroxy high molecular polymer. According to the invention, by adding the nano silicon dioxide and/or the polyhydroxy high molecular polymer, the generation of discharge phenomenon of oxygen anions on the surface of the aluminum oxide film can be inhibited, the sparking voltage of the electrolyte can be improved, and the stability and the use safety of the electrolyte are improved.
The other purpose of the invention is realized by the following technical scheme: the preparation method of the working electrolyte for the flame-retardant high-voltage aluminum electrolytic capacitor comprises the following steps:
s1, adding the raw materials except the flame-retardant auxiliary agent and the auxiliary agent into a solvent according to parts by weight, heating to 50-75 ℃, uniformly stirring, heating to 115-125 ℃, and keeping the temperature for 60-90min to obtain a mixture A;
s2, cooling the mixture A to 95-100 ℃, adding the flame-retardant auxiliary agent and the auxiliary agent into the mixture A, uniformly mixing, and cooling to room temperature to obtain the working electrolyte for the flame-retardant high-voltage aluminum electrolytic capacitor.
The invention has the beneficial effects that: according to the invention, the inorganic acid is adopted to replace part of the organic acid, the flame-retardant auxiliary agent and the auxiliary additive are added, the consumption of the raw materials is adjusted, and the raw materials are matched with each other, so that the electrolyte has good flame retardance and thermal stability, can be used as a flame-retardant high-voltage working electrolyte, is suitable for a flame-retardant high-voltage aluminum electrolytic capacitor, has good working performance, and obviously improves the use safety of the capacitor. The flame-retardant high-voltage working electrolyte and the prepared aluminum electrolytic capacitor are suitable for various household appliances, industrial power supplies, communication base stations and the like with high safety requirements. The preparation method of the working electrolyte for the flame-retardant high-voltage aluminum electrolytic capacitor is simple and efficient, is convenient to control, and is beneficial to industrial production.
Detailed Description
The present invention will be further described with reference to the following examples for facilitating understanding of those skilled in the art, and the description of the embodiments is not intended to limit the present invention.
Example 1
In this embodiment, the working electrolyte for the flame-retardant high-voltage aluminum electrolytic capacitor includes the following raw materials in parts by weight:
2.5 parts of inorganic acid
Organic acid 7.5 parts
8 portions of flame retardant additive
Auxiliary additive 1 part
And 80 parts of a solvent.
Further, each part of the solvent comprises the following raw materials in parts by weight: 55 parts of a main solvent and 25 parts of an auxiliary solvent. Further, the main solvent is ethylene glycol, and the auxiliary solvent is diethylene glycol.
Further, the organic acid is long carbon chain carboxylic acid ammonium salt with a branched chain. The auxiliary additive is p-nitrobenzoic acid. The flame-retardant auxiliary agent is tributyl phosphate.
Further, the preparation method of the branched long-carbon-chain carboxylic acid ammonium salt comprises the following steps:
(1) according to molar parts, 1.1 parts of cyclohexanone, 1.2 parts of hydrogen peroxide, 2.5 parts of ethanol, 0.4 part of phosphoric acid and 0.2 part of benzyltriethylammonium chloride are reacted for 25min at the temperature of 8 ℃ to obtain a mixture A;
(2) adding 0.6 part of dimethylaminoethyl methacrylate, 0.6 part of methyl methacrylate, 1.2 parts of ferrous chloride and 0.4 part of phosphoric acid into the mixture A obtained in the step (1) to react for 6 hours at the temperature of minus 2 ℃ to obtain a mixture B;
(3) adding the mixture B obtained in the step (2) into a sodium hydroxide solution for saponification reaction to obtain a mixture C;
(4) acidizing the mixture C obtained in the step (3) by using inorganic acid to obtain a mixture D;
(5) and (4) introducing ammonia gas into the mixture D obtained in the step (4) to carry out ammoniation reaction, wherein the pH value at the end of the reaction is 7.5, so as to obtain the long carbon chain carboxylic acid ammonium salt with the branched chain.
Further, in the step (3), the reflux temperature of the saponification reaction is 100 ℃, and the reflux time is 4.5 h.
Further, in the step (4), the inorganic acid is sulfuric acid with a mass percentage of 40%, and the reaction end point is a pH value of 2.5.
Further, the working electrolyte for the flame-retardant high-voltage aluminum electrolytic capacitor further comprises 2 parts by weight of functional additives, and the functional additives are nano silicon dioxide.
The preparation method of the working electrolyte for the flame-retardant high-voltage aluminum electrolytic capacitor comprises the following steps:
s1, adding the raw materials except the flame-retardant auxiliary agent and the auxiliary agent into a solvent in parts by weight, heating to 60 ℃, uniformly stirring, heating to 120 ℃, and keeping the temperature for 75min to obtain a mixture A;
s2, cooling the mixture A to 95 ℃, adding the flame-retardant auxiliary agent and the auxiliary agent into the mixture A, uniformly mixing, and cooling to room temperature to obtain the working electrolyte for the flame-retardant high-voltage aluminum electrolytic capacitor.
The aluminum electrolytic capacitor of the embodiment is formed by nailing an anode foil and a cathode foil with certain width with a guide pin, then winding the anode foil and the cathode foil with certain width with a liner with certain width into a cylinder, fixing the capacitor core with an insulating pressure sensitive adhesive tape, then soaking the capacitor core in the working electrolyte for the flame-retardant high-voltage aluminum electrolytic capacitor of the embodiment, then filling the capacitor core into an aluminum shell, and finally crimping and rolling the capacitor core with a rubber plug to obtain the capacitor.
The electrolytic solution can be used for manufacturing an aluminum electrolytic capacitor with rated voltage of 450V and electrostatic capacity of 4.7 UF.
Example 2
In this embodiment, the working electrolyte for the flame-retardant high-voltage aluminum electrolytic capacitor includes the following raw materials in parts by weight:
inorganic acid 15 parts
10 portions of organic acid
5 parts of flame-retardant auxiliary agent
Auxiliary additive 2 parts
And 90 parts of a solvent.
Further, each part of the solvent comprises the following raw materials in parts by weight: 60 parts of main solvent and 30 parts of auxiliary solvent. The main solvent is ethylene glycol, and the auxiliary solvent is diethylene glycol.
Further, the organic acid is long carbon chain carboxylic acid ammonium salt with a branched chain. The auxiliary additive is composed of p-nitrobenzyl alcohol and m-nitrobenzoic acid according to the mass ratio of 1: 1.
Further, the preparation method of the branched long-carbon-chain carboxylic acid ammonium salt comprises the following steps:
(1) according to molar parts, 1 part of cyclohexanone, 1 part of hydrogen peroxide, 2 parts of ethanol, 0.2 part of phosphoric acid and 0.15 part of benzyltriethylammonium chloride are reacted for 20min at the temperature of 6 ℃ to obtain a mixture A;
(2) adding 0.5 part of dimethylaminoethyl methacrylate, 0.4 part of methyl methacrylate, 1 part of ferrous chloride and 0.3 part of phosphoric acid into the mixture A obtained in the step (1) to react for 5 hours at the temperature of minus 5 ℃ to obtain a mixture B;
(3) adding the mixture B obtained in the step (2) into a sodium hydroxide solution for saponification reaction to obtain a mixture C;
(4) acidizing the mixture C obtained in the step (3) by using inorganic acid to obtain a mixture D;
(5) and (4) introducing ammonia gas into the mixture D obtained in the step (4) to carry out ammoniation reaction, wherein the pH value at the end of the reaction is 7.2, so as to obtain the long carbon chain carboxylic acid ammonium salt with the branched chain.
Further, in the step (3), the reflux temperature of the saponification reaction is 95 ℃, and the reflux time is 5 hours.
Further, in the step (4), the inorganic acid is sulfuric acid with a mass percentage of 30%, and the reaction end point is a pH value of 2.
Further, the flame retardant auxiliary agent comprises triethyl phosphate and butyl-diphenyl phosphate according to a mass ratio of 2: 1.
Further, the working electrolyte for the flame-retardant high-voltage aluminum electrolytic capacitor also comprises 1 part by weight of functional additive, wherein the functional additive is polyvinyl alcohol.
Further, the working electrolyte for the flame-retardant high-voltage aluminum electrolytic capacitor further comprises 3 parts by weight of functional additives, wherein the functional additives are at least one of nano silicon dioxide and polyhydroxy high polymer.
The preparation method of the working electrolyte for the flame-retardant high-voltage aluminum electrolytic capacitor comprises the following steps:
s1, adding the raw materials except the flame-retardant auxiliary agent and the auxiliary agent into a solvent in parts by weight, heating to 50 ℃, uniformly stirring, heating to 115 ℃, and keeping the temperature for 90min to obtain a mixture A;
and S2, cooling the mixture A to 100 ℃, adding the flame-retardant auxiliary agent and the auxiliary agent into the mixture A, uniformly mixing, and cooling to room temperature to obtain the working electrolyte for the flame-retardant high-voltage aluminum electrolytic capacitor.
The rest of this embodiment is the same as embodiment 1, and is not described herein again.
Example 3
In this embodiment, the working electrolyte for the flame-retardant high-voltage aluminum electrolytic capacitor includes the following raw materials in parts by weight:
inorganic acid 8 parts
5 parts of organic acid
0.1 part of flame-retardant auxiliary agent
0.1 part of auxiliary additive
70 parts of a solvent.
Further, each part of the solvent comprises the following raw materials in parts by weight: 50 parts of main solvent and 20 parts of auxiliary solvent.
Further, the organic acid is long carbon chain carboxylic acid ammonium salt with a branched chain.
Further, the preparation method of the branched long-carbon-chain carboxylic acid ammonium salt comprises the following steps:
(1) according to molar parts, 1.2 parts of cyclohexanone, 1.5 parts of hydrogen peroxide, 3 parts of ethanol, 0.6 part of phosphoric acid and 0.25 part of benzyltriethylammonium chloride are reacted for 30min at the temperature of 12 ℃ to obtain a mixture A;
(2) adding 0.9 part of dimethylaminoethyl methacrylate, 0.8 part of methyl methacrylate, 1.8 parts of ferrous chloride and 0.6 part of phosphoric acid into the mixture A obtained in the step (1) to react for 7 hours at the temperature of 0 ℃ to obtain a mixture B;
(3) adding the mixture B obtained in the step (2) into a sodium hydroxide solution for saponification reaction to obtain a mixture C;
(4) acidizing the mixture C obtained in the step (3) by using inorganic acid to obtain a mixture D;
(5) and (4) introducing ammonia gas into the mixture D obtained in the step (4) to carry out ammoniation reaction, wherein the pH value at the end of the reaction is 7.2-7.6. Obtaining the long carbon chain carboxylic acid ammonium salt with the branched chain.
Further, in the step (3), the reflux temperature of the saponification reaction is 105 ℃, and the reflux time is 4 hours.
Further, in the step (4), the inorganic acid is 50% by mass of sulfuric acid, and the reaction end point is a pH value of 3.
Furthermore, the auxiliary additive is composed of p-nitrobenzoic acid and p-nitrophenol according to the mass ratio of 1: 2.
Further, the flame retardant auxiliary agent comprises toluene diphenyl phosphate and dibutyl phenyl phosphate according to the mass ratio of 1: 1.
Further, the working electrolyte for the flame-retardant high-voltage aluminum electrolytic capacitor also comprises 1 part by weight of functional additive, wherein the functional additive is nano silicon dioxide.
The preparation method of the working electrolyte for the flame-retardant high-voltage aluminum electrolytic capacitor comprises the following steps:
s1, adding the raw materials except the flame-retardant auxiliary agent and the auxiliary agent into a solvent in parts by weight, heating to 75 ℃, uniformly stirring, heating to 125 ℃, and keeping the temperature for 60min to obtain a mixture A;
s2, cooling the mixture A to 95 ℃, adding the flame-retardant auxiliary agent and the auxiliary agent into the mixture A, uniformly mixing, and cooling to room temperature to obtain the working electrolyte for the flame-retardant high-voltage aluminum electrolytic capacitor.
The rest of this embodiment is the same as embodiment 1, and is not described herein again.
Example 4
In this embodiment, the working electrolyte for the flame-retardant high-voltage aluminum electrolytic capacitor includes the following raw materials in parts by weight:
5 portions of inorganic acid
6 portions of organic acid
0.5 part of flame-retardant auxiliary agent
Auxiliary additive 4 parts
And 75 parts of a solvent.
Further, each part of the solvent comprises the following raw materials in parts by weight: 53 parts of main solvent and 22 parts of auxiliary solvent.
Further, the organic acid is long carbon chain carboxylic acid ammonium salt with a branched chain.
Further, the preparation method of the branched long-carbon-chain carboxylic acid ammonium salt comprises the following steps:
(1) according to molar parts, taking 1-1.2 parts of cyclohexanone, 1-1.5 parts of hydrogen peroxide, 2-3 parts of ethanol, 0.2-0.6 part of phosphoric acid and 0.15-0.25 part of benzyltriethylammonium chloride to react for 20-30min at the temperature of 6-12 ℃ to obtain a mixture A;
(2) adding 0.5-0.9 part of dimethylaminoethyl methacrylate, 0.4-0.8 part of methyl methacrylate, 1-1.8 parts of ferrous chloride and 0.3-0.6 part of phosphoric acid into the mixture A obtained in the step (1) to react at the temperature of-5 to-0 ℃ for 5-7 hours to obtain a mixture B;
(3) adding the mixture B obtained in the step (2) into a sodium hydroxide solution for saponification reaction to obtain a mixture C;
(4) acidizing the mixture C obtained in the step (3) by using inorganic acid to obtain a mixture D;
(5) and (4) introducing ammonia gas into the mixture D obtained in the step (4) to carry out ammoniation reaction, wherein the pH value at the end of the reaction is 7.2-7.6. Obtaining the long carbon chain carboxylic acid ammonium salt with the branched chain.
Further, in the step (3), the reflux temperature of the saponification reaction is 95-105 ℃, and the reflux time is 4-5 h.
Further, in the step (4), the inorganic acid is sulfuric acid with a mass percentage of 30-50%, and the reaction end point is a pH value of 2-3.
Further, the working electrolyte for the flame-retardant high-voltage aluminum electrolytic capacitor also comprises 1.5 parts by weight of functional auxiliary agent, and the functional auxiliary agent is nano silicon dioxide.
The preparation method of the working electrolyte for the flame-retardant high-voltage aluminum electrolytic capacitor comprises the following steps:
s1, adding the raw materials except the flame-retardant auxiliary agent and the auxiliary agent into a solvent in parts by weight, heating to 65 ℃, uniformly stirring, heating to 115 ℃, and keeping the temperature for 70min to obtain a mixture A;
s2, cooling the mixture A to 98 ℃, adding the flame-retardant auxiliary agent and the auxiliary agent into the mixture A, uniformly mixing, and cooling to room temperature to obtain the working electrolyte for the flame-retardant high-voltage aluminum electrolytic capacitor.
The rest of this embodiment is the same as embodiment 1, and is not described herein again.
Comparative example 1
In the comparative example, the working electrolyte for the aluminum electrolytic capacitor comprises the following raw materials in parts by weight:
55 parts of ethylene glycol, 25 parts of diethylene glycol, 7.5 parts of branched long-carbon-chain carboxylic acid ammonium salt, 1 part of p-nitrobenzoic acid and 2 parts of nano silicon dioxide.
The remainder of this comparative example is the same as example 1 and will not be described again here.
Comparative example 2
In the comparative example, the working electrolyte for the aluminum electrolytic capacitor comprises the following raw materials in parts by weight:
55 parts of ethylene glycol, 25 parts of diethylene glycol, 8 parts of ammonium pentaborate, 7.5 parts of branched long-carbon-chain carboxylic acid ammonium salt, 1 part of p-nitrobenzoic acid and 2 parts of nano silicon dioxide. The remainder of this comparative example is the same as example 1 and will not be described again here.
Comparative example 3
In the comparative example, the working electrolyte for the aluminum electrolytic capacitor comprises the following raw materials in parts by weight:
55 parts of ethylene glycol, 25 parts of diethylene glycol, 3 parts of tributyl phosphate, 7.5 parts of branched long-carbon-chain carboxylic acid ammonium salt, 1 part of p-nitrobenzoic acid and 2 parts of nano silicon dioxide. The remainder of this comparative example is the same as example 1 and will not be described again here.
Comparative example 4
In the comparative example, the working electrolyte for the aluminum electrolytic capacitor comprises the following raw materials in parts by weight:
55 parts of ethylene glycol, 25 parts of diethylene glycol, 2.5 parts of ammonium pentaborate, 8 parts of tributyl phosphate, 7.5 parts of 2-butyl suberic acid, 1 part of p-nitrobenzoic acid and 2 parts of nano silicon dioxide. The remainder of this comparative example is the same as example 1 and will not be described again here.
The working electrolytes for flame-retardant high-voltage aluminum electrolytic capacitors of examples 1 to 4 and comparative examples 1 to 4 were subjected to performance tests:
initial characteristic evaluation: testing the performance parameters of the working electrolyte: conductivity, pH, sparking voltage;
evaluation of Combustion test: after the capacitor core is impregnated with the electrolyte, absorbing the redundant electrolyte on the surface, fixing the capacitor core on a fixing clamp of a support frame, placing the flame of an alcohol lamp at the edge position of the core, keeping for 10 seconds, removing the flame, and simultaneously beginning to record the afterflame time t 1; after the fire is stopped, the flame is removed after the flame is burned again for 10 seconds, and meanwhile, the time t2 of the fire is recorded; and confirm whether the capacitor core has burning particles which drop and ignite the cotton during the burning process.
As can be seen from the above table, comparative example 1 does not contain a flame retardant aid and an inorganic acid, and cannot achieve a flame retardant effect; the comparison document 2 does not contain a flame-retardant auxiliary agent, and cannot realize a flame-retardant effect; the comparison document 2 only contains the flame-retardant auxiliary agent, does not contain inorganic acid, and has an unobvious flame-retardant effect; compared with comparative examples 1-3, the capacitor of example 1 of the invention has better flame retardancy, the capacitor element can be rapidly self-extinguished after the flame leaves, and the initial characteristics of the capacitor and the characteristic deterioration in the life process are small; example 1 of the present invention has higher conductivity and higher sparking voltage than comparative example 4.
The above-described embodiments are preferred implementations of the present invention, and the present invention may be implemented in other ways without departing from the spirit of the present invention.
Claims (9)
1. The utility model provides a fire-retardant type high pressure aluminium is work electrolyte for electrolytic capacitor which characterized in that: the feed comprises the following raw materials in parts by weight:
2.5-15 parts of inorganic acid
5-10 parts of organic acid
0.1-5 parts of flame-retardant auxiliary agent
0.1-2 parts of auxiliary additive
70-90 parts of a solvent.
2. The working electrolyte for the flame-retardant high-voltage aluminum electrolytic capacitor according to claim 1, characterized in that: each part of the solvent comprises the following raw materials in parts by weight: 50-60 parts of main solvent and 20-30 parts of auxiliary solvent.
3. The working electrolyte for the flame-retardant high-voltage aluminum electrolytic capacitor according to claim 2, characterized in that: the main solvent is ethylene glycol, and the auxiliary solvent is diethylene glycol.
4. The working electrolyte for the flame-retardant high-voltage aluminum electrolytic capacitor according to claim 1, characterized in that: the organic acid is long carbon chain carboxylic acid ammonium salt with a branched chain.
5. The working electrolyte for the flame-retardant high-voltage aluminum electrolytic capacitor according to claim 1, characterized in that: the inorganic acid is at least one of boric acid and ammonium pentaborate.
6. The working electrolyte for the flame-retardant high-voltage aluminum electrolytic capacitor according to claim 1, characterized in that: the auxiliary additive is at least one of p-nitrobenzoic acid, p-nitrobenzyl alcohol, m-nitrobenzoic acid and p-nitrophenol.
7. The working electrolyte for the flame-retardant high-voltage aluminum electrolytic capacitor according to claim 1, characterized in that: the flame retardant auxiliary agent is at least one of triethyl phosphate, tributyl phosphate, toluene-diphenyl phosphate, triphenyl phosphate, dibutyl-phenyl phosphate and butyl-diphenyl phosphate.
8. The working electrolyte for the flame-retardant high-voltage aluminum electrolytic capacitor according to claim 1, characterized in that: the working electrolyte for the flame-retardant high-voltage aluminum electrolytic capacitor further comprises 1-3 parts by weight of functional additives, wherein the functional additives are at least one of nano silicon dioxide and polyhydroxy high polymer.
9. A method for preparing the working electrolyte for the flame-retardant high-voltage aluminum electrolytic capacitor according to any one of claims 1 to 7, characterized in that: the method comprises the following steps:
s1, adding the raw materials except the flame-retardant auxiliary agent and the auxiliary agent into a solvent according to parts by weight, heating to 50-75 ℃, uniformly stirring, heating to 115-125 ℃, and keeping the temperature for 60-90min to obtain a mixture A;
s2, cooling the mixture A to 95-100 ℃, adding the flame-retardant auxiliary agent and the auxiliary agent into the mixture A, uniformly mixing, and cooling to room temperature to obtain the working electrolyte for the flame-retardant high-voltage aluminum electrolytic capacitor.
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