CN104201426B - Electrolyte contracting to carboxyl benzaldehyde PEG400 laurate containing DNPH and preparation method thereof - Google Patents
Electrolyte contracting to carboxyl benzaldehyde PEG400 laurate containing DNPH and preparation method thereof Download PDFInfo
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- CN104201426B CN104201426B CN201410451417.XA CN201410451417A CN104201426B CN 104201426 B CN104201426 B CN 104201426B CN 201410451417 A CN201410451417 A CN 201410451417A CN 104201426 B CN104201426 B CN 104201426B
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- carboxyl benzaldehyde
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/24—Alkaline accumulators
- H01M10/26—Selection of materials as electrolytes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/24—Alkaline accumulators
- H01M10/28—Construction or manufacture
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M2300/00—Electrolytes
- H01M2300/0002—Aqueous electrolytes
- H01M2300/0014—Alkaline electrolytes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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Abstract
The invention discloses a kind of electrolyte contracting to carboxyl benzaldehyde PEG400 laurate containing DNPH and preparation method thereof. Should be containing 2, the DNPH contracting that the contracting of 4-dinitrophenylhydrazine is 0.7mmol/L to the electrolyte of carboxyl benzaldehyde PEG400 laurate by concentration is the KOH solution composition that 6mol/L contains saturated ZnO to carboxyl benzaldehyde PEG400 laurate surfactant and concentration; Described DNPH contracting to the structural formula of carboxyl benzaldehyde PEG400 laurate surfactant is:. Take above-mentioned 2,4-dinitrophenylhydrazine contracts to carboxyl benzaldehyde PEG400 laurate surfactant, is dissolved in containing in the KOH solution of saturated ZnO, fully mixes, make the electrolyte contracting to carboxyl benzaldehyde PEG400 laurate containing DNPH.
Description
Technical field
The invention belongs to electrolyte technical field, particularly one contains DNPH and contracts to carboxyl benzaldehydeAlkaline zinc cell electrolyte of PEG400 laurate surfactant and preparation method thereof.
Background technology
Zinc due to the advantages such as source is abundant, low price, toxicity is low, specific energy is high, electrode potential is low become alkaline zinc margunese,The negative material of the batteries such as zinc air, zinc-nickel, zinc silver oxide. Rapidly, high performance mini is close in current various portable electronics developmentEnvelope battery is widely used in the fields such as military affairs, aviation, business. But in secondary alkaline zinc battery, zinc electrode is general in charge and discharge processAll over there is zinc distortion, zinc dendrite, from problems such as burn into passivation, reduce battery capacity, reduce circulating battery access times,Its application is restricted. Past utilizes mercury in zinc surface amalgamation technology conventionally, addresses the above problem, but because mercury is acutePoisonous substance matter, therefore the development of mercury-free battery becomes extremely urgent problem, is the important of head it off for mercury corrosion inhibition additiveApproach. That studies at present is mainly divided into two types of electrode corrosion inhibition additive, electrolyte corrosion inhibition additives for mercury corrosion inhibition additive.But the battery under current researched and developed charging and discharging capabilities, the especially high magnification that tends to reduce battery for mercury corrosion inhibition additive fillsDischarge capability, not yet finds the material of the complete replacement for mercury of a kind of energy. Surfactant has amphiphilic structure, and its hydrophilic group is easily inhaledBe attached on metal surface, and the long alkyl carbon chain of lipophilic group-----points to corrosive medium, form one deck protection in metal surfaceFilm, can effectively stop corrosion of metal process. The corrosion mitigating effect of schiff bases corrosion inhibiter is obvious to all, if by schiff basesGroup is introduced in surfactant, should be able to prepare and be applicable to the corrosion inhibition additive that alkaline zinc cell is used. In the present invention, contain 2,The alkaline zinc cell electrolyte that 4-dinitrophenylhydrazine contracts to carboxyl benzaldehyde polyethylene glycol (400) laurate surfactantPreparation method, this achievement in research is to providing and comply with for mercury corrosion inhibition additive as alkaline zinc cell containing schiff bases surfactantAccording to, have no bibliographical information.
Summary of the invention
The object of this invention is to provide a kind of DNPH that contains contracts to carboxyl benzaldehyde PEG400 laurateElectrolyte of ester and preparation method thereof.
The DNPH that contains of the present invention contracts to the electrolyte of carboxyl benzaldehyde PEG400 laurate by denseDegree is that the DNPH of 0.7mmol/L contracts to carboxyl benzaldehyde PEG400 laurate surfactant and denseDegree is for 6mol/L is containing the KOH solution composition of saturated ZnO.
The described DNPH structural formula to carboxyl benzaldehyde PEG400 laurate surfactant that contractsFor:
Prepare above-mentioned containing the contract tool of the electrolyte to carboxyl benzaldehyde PEG400 laurate of DNPHBody step is:
(1) be that 2:0.125:1.25 takes respectively 3 grams to carboxyl benzaldehyde, 0.153 gram of 4-dimethylamino according to mol ratioPyridine DMAP and 2.58 grams of dicyclohexylcarbodiimide DCC are placed in there-necked flask, and there-necked flask is placed in water-bath, take2.58 grams of PEG400 lauric acid monoesters are dissolved in 10mL carrene, put into constant pressure funnel, slowly splash into above-mentioned three mouthfulsIn flask, start reaction under normal temperature, add magneton at the uniform velocity to stir, reaction is carried out 24 hours under nitrogen protection, after having reacted,Reactant liquor is put into refrigerator and cooled and freeze 15 minutes, separate out dicyclohexylurea (DCU) precipitation, suction filtration, is rotated evaporation by gained filtrate,Obtain white thickness oily solid, be carboxyl benzaldehyde PEG400 lauric acid monoester.
(2) what take that 2 grams of steps (1) make is dissolved in 20mL ethanol to carboxyl benzaldehyde PEG400 lauric acid monoesterIn, make carboxyl benzaldehyde PEG400 lauric acid monoester ethanolic solution; Weighing 0.54 gram of DNPH addsIn there-necked flask, with the dissolving of 30mL ethanol, after having dissolved, there-necked flask is placed in to glycerine bath and heats, Temperature Setting is 70DEG C, add magneton at the uniform velocity to stir, in the time that temperature rises to 70 DEG C, with constant pressure funnel by above-mentioned make to the poly-second two of carboxyl benzaldehydeAlcohol 400 lauric acid monoester ethanolic solutions slowly splash in flask and react 6 hours, after reaction finishes, reactant liquor are rotated to steamingBeam back receipts alcohol solvent, obtain brown color thickness oily solid, be DNPH and contract to carboxyl benzaldehyde polyethylene glycol400 laurate surfactants.
(3) taking the DNPH that step (2) makes contracts to carboxyl benzaldehyde PEG400 laurate tableSurface-active agent, is dissolved in 6mol/L containing in the KOH solution of saturated ZnO, makes DNPH contracting to the poly-second of carboxyl benzaldehydeThe concentration of glycol 400 laurate surfactants in solution is 0.7mmol/L, fully mixes, and makes and contains 2,4-bis-The nitrophenyl hydrazine alkaline zinc cell electrolyte to carboxyl benzaldehyde PEG400 laurate surfactant that contracts.
Electrolyte of the present invention is assembled into simulation alkali zinc nickel battery, and with blank assay contrast, result shows, adds contractingDNPH yl benzoic acid PEG400 laurate surfactant can significantly improve the performance of battery, at headInferior and repeatedly in charge and discharge cycles process, the decay of battery capacity is obviously slack-off; And surfactant of the present invention has amphiphilicStructure, its hydrophilic group is easily adsorbed on metal surface, and the long alkyl carbon chain of lipophilic group-----points to corrosive medium, at goldMetal surface forms layer protecting film, can effectively stop corrosion of metal process.
Brief description of the drawings
Fig. 1 is that the present invention prepares the electricity contracting to carboxyl benzaldehyde PEG400 laurate containing DNPHSeparate the process chart of liquid.
Fig. 2 contracts to carboxyl benzaldehyde PEG400 laurate containing DNPH in the embodiment of the present inventionThe alkali zinc nickel battery of the electrolyte assembling of surfactant (M3) and the curve of impulse electricity first of blank battery. From figureVisible, the alkaline battery charging platform of paste spread type zinc electrode and nickel electrode composition is at 1.7V～1.85V, discharge platform 1.7V～1.85V, between discharging and recharging, current potential difference is less, and visible battery has better reversibility. Under equal conditions, added thisPrepared by bright embodiment contracts to carboxyl benzaldehyde PEG400 laurate surfactant (M3) containing DNPHWith un-added blank group contrast, add after M3, alkali zinc nickel battery has longer discharge time, shows the embodiment of the present inventionThe M3 of the preparation burn into dendrite under alkali condition, distortion to zinc electrode, zinc migration, have good inhibitory action, and with sky, this paste spread type zinc electrode has higher discharge capacity to white appliances solution liquor ratio.
Fig. 3 contracts to carboxyl benzaldehyde PEG400 laurate containing DNPH in the embodiment of the present inventionAlkali zinc nickel battery and the repeatedly charging and discharging curve figure of blank battery of the electrolyte assembling of surfactant (M3). From figureVisible, in 30 charge and discharge process of simulation alkali zinc nickel battery, battery capacity is relatively stable. Add embodiment of the present invention systemStandby containing DNPH contracting to the electrolyte of carboxyl benzaldehyde PEG400 laurate surfactant (M3) withDo not add blank group contrast, add after M3, battery capacity increases, the increased frequency of circulation, cycle performance of battery is better, this be because ofFor the corrosion of M3 to zinc electrode, dendrite, passivation etc. have good inhibitory action, can extend largely the service life of batteryAnd cycle-index.
Detailed description of the invention
Further illustrate the present invention below in conjunction with specific embodiment, but embodiment does not limit the scope of the invention.
Embodiment:
(1) be that 2:0.125:1.25 takes respectively 3 grams to carboxyl benzaldehyde, 0.153 gram of 4-dimethylamino according to mol ratioPyridine DMAP and 2.58 grams of dicyclohexylcarbodiimide DCC are placed in there-necked flask, and there-necked flask is placed in water-bath, take2.58 grams of PEG400 lauric acid monoesters are dissolved in 10mL carrene, put into constant pressure funnel, slowly splash into above-mentioned three mouthfulsIn flask, start reaction under normal temperature, add magneton at the uniform velocity to stir, reaction is carried out 24 hours under nitrogen protection, after having reacted,Reactant liquor is put into refrigerator and cooled and freeze 15 minutes, separate out dicyclohexylurea (DCU) precipitation, suction filtration, is rotated evaporation by gained filtrate,Obtain white thickness oily solid, be carboxyl benzaldehyde PEG400 lauric acid monoester.
(2) what take that 2 grams of steps (1) make is dissolved in 20mL ethanol to carboxyl benzaldehyde PEG400 lauric acid monoesterIn, make carboxyl benzaldehyde PEG400 lauric acid monoester ethanolic solution; Weighing 0.54 gram of DNPH addsIn there-necked flask, with the dissolving of 30mL ethanol, after having dissolved, there-necked flask is placed in to glycerine bath and heats, Temperature Setting is 70DEG C, add magneton at the uniform velocity to stir, in the time that temperature rises to 70 DEG C, with constant pressure funnel by above-mentioned make to the poly-second two of carboxyl benzaldehydeAlcohol 400 lauric acid monoester ethanolic solutions slowly splash in flask and react 6 hours, after reaction finishes, reactant liquor are rotated to steamingBeam back receipts alcohol solvent, obtain brown color thickness oily solid, be DNPH and contract to carboxyl benzaldehyde polyethylene glycol400 laurate surfactants.
(3) taking the DNPH that step (2) makes contracts to carboxyl benzaldehyde PEG400 laurate tableSurface-active agent, is dissolved in 6mol/L containing in the KOH solution of saturated ZnO, makes DNPH contracting to the poly-second of carboxyl benzaldehydeThe concentration of glycol 400 laurate surfactants in solution is 0.7mmol/L, fully mixes, and makes and contains 2,4-bis-The nitrophenyl hydrazine alkaline zinc cell electrolysis to carboxyl benzaldehyde PEG400 laurate surfactant (being designated as M3) of contractingLiquid.
The above-mentioned DNPH structural formula to carboxyl benzaldehyde PEG400 laurate surfactant that contractsFor:
Alkaline zinc cell electrolyte prepared by the present embodiment carries out performance measuring and evaluating, with blank assay contrast, specific as follows:
First be assembled into simulation alkali zinc nickel battery, by measuring battery charging and discharging curve and repeatedly charge/discharge capacity variationCurve, to evaluate the combination property of above-mentioned electrolyte. When experiment, paste spread type zinc electrode is as negative pole (area is 1 × 3cm), nickelFor positive pole, the Area Ratio of positive and negative electrode is 1:3, and separates with hydrocellulose membrane, avoids both positive and negative polarity contact in experimentation. FillThe electricity time is 2 hours, and charging current is set as 60mA, and discharge current is 30mA, and final discharging voltage is 1V, carries out 1 time and charges and dischargeElectricity circulation, to mapping discharge time, obtains battery charging and discharging curve, as shown in Figure 2 with discharge voltage. Charging interval is 2 hours, fillsElectricity current settings is 60mA, and discharge current is 30mA, and final discharging voltage is 1V, carries out charge and discharge cycles 30 times, by electric discharge appearanceAmount, to the mapping of charge and discharge cycles number of times, obtains repeatedly charge/discharge capacity change curve, as shown in Figure 3.
Claims (2)
1. the electrolyte contracting to carboxyl benzaldehyde PEG400 laurate containing DNPH, its feature existsBe 0.7mmol/ to the electrolyte of carboxyl benzaldehyde PEG400 laurate by concentration containing DNPH contracting in thisThe DNPH contracting of L is that 6mol/L contains to carboxyl benzaldehyde PEG400 laurate surfactant and concentrationThe KOH solution composition of saturated ZnO;
Described DNPH contracting to the structural formula of carboxyl benzaldehyde PEG400 laurate surfactant is:
。
According to claim 1 containing DNPH contracting to carboxyl benzaldehyde PEG400 laurateThe preparation method of electrolyte, is characterized in that concrete steps are:
(1) be that 2:0.125:1.25 takes respectively 3 grams to carboxyl benzaldehyde, 0.153 gram of DMAP according to mol ratioDMAP and 2.58 grams of dicyclohexylcarbodiimide DCC are placed in there-necked flask, and there-necked flask is placed in water-bath, take 2.58Gram PEG400 lauric acid monoester is dissolved in 10mL carrene, puts into constant pressure funnel, slowly splashes into above-mentioned there-necked flaskIn, under normal temperature, start reaction, add magneton at the uniform velocity to stir, reaction is carried out 24 hours under nitrogen protection, after having reacted, will be anti-Answer liquid to put into refrigerator and cooled and freeze 15 minutes, separate out dicyclohexylurea (DCU) precipitation, suction filtration, is rotated evaporation by gained filtrate, obtains whiteLook thickness oily solid, is carboxyl benzaldehyde PEG400 lauric acid monoester;
(2) take 2 grams of steps (1) make carboxyl benzaldehyde PEG400 lauric acid monoester is dissolved in 20mL ethanol, systemMust be to carboxyl benzaldehyde PEG400 lauric acid monoester ethanolic solution; Weigh 0.54 gram of DNPH and add three mouthfulsIn flask, with the dissolving of 30mL ethanol, after having dissolved, there-necked flask is placed in to glycerine bath and heats, Temperature Setting is 70 DEG C,Add magneton at the uniform velocity to stir, in the time that temperature rises to 70 DEG C, with constant pressure funnel by above-mentioned make to carboxyl benzaldehyde polyethylene glycol400 lauric acid monoester ethanolic solutions slowly splash in flask and react 6 hours, after reaction finishes, reactant liquor are rotated to evaporationReclaim alcohol solvent, obtain brown color thickness oily solid, be DNPH and contract to carboxyl benzaldehyde PEG400Laurate surfactant;
(3) taking the DNPH contracting that step (2) makes lives to carboxyl benzaldehyde PEG400 laurate surfaceProperty agent, be dissolved in 6mol/L containing in the KOH solution of saturated ZnO, DNPH is contracted to carboxyl benzaldehyde polyethylene glycolThe concentration of 400 laurate surfactants in solution is 0.7mmol/L, fully mixes, and makes and contains 2,4-dinitroThe phenylhydrazine alkaline zinc cell electrolyte to carboxyl benzaldehyde PEG400 laurate surfactant that contracts.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410451417.XA CN104201426B (en) | 2014-09-07 | 2014-09-07 | Electrolyte contracting to carboxyl benzaldehyde PEG400 laurate containing DNPH and preparation method thereof |
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| CN201410451417.XA CN104201426B (en) | 2014-09-07 | 2014-09-07 | Electrolyte contracting to carboxyl benzaldehyde PEG400 laurate containing DNPH and preparation method thereof |
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| CN104201426B true CN104201426B (en) | 2016-05-18 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102088115A (en) * | 2011-01-11 | 2011-06-08 | 中南大学 | Compound corrosion inhibitor of alkaline electrolyte of alkaline aluminium battery, electrolyte and preparation method of compound corrosion inhibitor |
| CN103467338A (en) * | 2013-09-27 | 2013-12-25 | 桂林理工大学 | 2-octanone condensation-compound ethylenediamine and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102088115A (en) * | 2011-01-11 | 2011-06-08 | 中南大学 | Compound corrosion inhibitor of alkaline electrolyte of alkaline aluminium battery, electrolyte and preparation method of compound corrosion inhibitor |
| CN103467338A (en) * | 2013-09-27 | 2013-12-25 | 桂林理工大学 | 2-octanone condensation-compound ethylenediamine and application thereof |
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