CN103467338A - 2-octanone condensation-compound ethylenediamine and application thereof - Google Patents
2-octanone condensation-compound ethylenediamine and application thereof Download PDFInfo
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- CN103467338A CN103467338A CN2013104491578A CN201310449157A CN103467338A CN 103467338 A CN103467338 A CN 103467338A CN 2013104491578 A CN2013104491578 A CN 2013104491578A CN 201310449157 A CN201310449157 A CN 201310449157A CN 103467338 A CN103467338 A CN 103467338A
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Abstract
The invention discloses a Schiff base surface active agent named 2-octanone condensation-compound ethylenediamine and application thereof. The structural formula of the 2-octanone condensation-compound ethylenediamine is as follows. The 2-octanone condensation-compound ethylenediamine is applied to alkaline Zn-Ni batteries as mercury substituting corrosion inhibition additives and used for preventing corrosion, dendritic growth, deformation, migration and the like of zinc electrodes. The 2-octanone condensation-compound ethylenediamine can effectively prevent alkaline electrolytes from corroding the zinc electrodes. Moreover, the cyclic voltammetry and zinc migration experiments prove that the 2-octanone condensation-compound ethylenediamine plays good roles in inhibiting the dendritic growth, the deformation and the migration of the pasted zinc electrodes.
Description
Technical field
The invention belongs to the alkali zinc nickel battery for mercury corrosion inhibition additive technical field, particularly a kind of Containing Schiff-bases tensio-active agent methyln-hexyl ketone contracting quadrol and in the alkali zinc nickel battery as for the application of mercury corrosion inhibition additive.
Background technology
Along with social development, the application of secondary alkaline zinc battery is also promoted day by day, and rapidly, the secondary alkaline zinc battery is widely used in the fields such as military affairs, aviation, business in current various portable electronics development.But zinc electrode is the problems such as the distortion of ubiquity burn into, dendrite, migration under alkaline condition, shorten its life-span.Past warp mercury commonly used turns into solving this series of problems together zinc surface, but mercury is a kind of poisonous and hazardous material, has brought huge threat to the health of human body and the protection of environment.Enhancing and scientific and technological development of advancing by leaps and bounds along with human environment protection consciousness; the harmonious development of Sustainable development and man and nature has become the theme of countries nowadays development; the requirement of the corrosion inhibition additive of using for secondary alkaline zinc electrode is also more and more higher, environmental protection and to economize on resources be the corrosion inhibition additive developing direction in future.Forefathers have had many achievements in research solving on the problems such as the distortion of zinc electrode burn into, dendrite, migration, are mainly reflected in the development research of various generation mercury corrosion inhibition additive.Secondary zinc electrode corrosion inhibition additive kind commonly used is mainly inorganic corrosion inhibition additive, organic inhibition additive, polymer class corrosion inhibition additive.Wherein inorganic corrosion inhibition additive mainly contains metal oxide, oxyhydroxide, inorganic salts; The organic inhibition additive mainly contains mercaptobenzothiazole, benzotriazole, Sodium dodecylbenzene sulfonate, Tetrabutyl amonium bromide etc.; The polymer class corrosion inhibition additive mainly comprises polyethylene kind.Methyln-hexyl ketone Containing Schiff-bases tensio-active agent is the Containing Schiff-bases tensio-active agent with coordination function, this structure had not only contained Containing Schiff-bases coordinating group, but also the amphiphilic structure that contains tensio-active agent, add a small amount of methyln-hexyl ketone Containing Schiff-bases tensio-active agent in electrolytic solution or electrode, can there is coating effect how much at electrode surface, can well be adsorbed on the metallic zinc surface, form the hydrophobic adsorption film of one deck, thereby effectively suppress the corrosion certainly of zinc electrode.Tensio-active agent also can play the sedimentation velocity of improving zinc in the absorption on zinc electrode surface simultaneously, thereby improves the electric current distribution homogeneity, reaches the purpose that suppresses distortion and dendrite, and prevents to a certain extent the generation of zinc migration.
Summary of the invention
The purpose of this invention is to provide a kind of Containing Schiff-bases tensio-active agent methyln-hexyl ketone contracting quadrol and application thereof.
The structural formula of methyln-hexyl ketone contracting quadrol is:
Described methyln-hexyl ketone contracting quadrol is applied in the alkali zinc nickel battery as for the mercury corrosion inhibition additive, for preventing the phenomenons such as zinc electrode the burn into dendritic growth occurs, deforms, migration.
Methyln-hexyl ketone contracting quadrol of the present invention can effectively prevent the corrosive nature of alkaline electrolyte to zinc electrode, and through cyclic voltammetry and zinc migration experiment, show, methyln-hexyl ketone contracting quadrol of the present invention has restraining effect preferably to paste spread type zinc electrode dendritic growth, distortion, migration.
The accompanying drawing explanation
Fig. 1 is that the embodiment of the present invention is tested the cyclic voltammetry curve figure of paste spread type zinc electrode in blank electrolysis liquid.
The cyclic voltammetry curve figure that Fig. 2 is embodiment of the present invention test paste spread type zinc electrode in adding the methyln-hexyl ketone contracting quadrol electrolytic solution that mass percent is 4%.
Embodiment
embodiment:
(1) structural formula of methyln-hexyl ketone contracting quadrol:
(2) preparation method of methyln-hexyl ketone contracting quadrol is:
Measure 3.2 milliliters of methyln-hexyl ketones (20 mmole), be dissolved in 15 milliliters of dehydrated alcohols, then add in there-necked flask, under 50 ℃ of water-baths, add 0.8 milliliter of quadrol (because quadrol is easy to volatilization loss, therefore make that it is slightly excessive), add again 1 milliliter of Glacial acetic acid to make catalyzer, start reaction, react after 3 hours, there-necked flask is taken out and to put into that refrigerator is standing is cooled to 2 ℃, now Glacial acetic acid becomes solid and separates out, then cross and filter out the catalyzer Glacial acetic acid, steam the solvent dehydrated alcohol with Rotary Evaporators under 60 ℃ of conditions again, obtain the thick material of yellowish brown, 50 ℃ of oven dry obtain the yellowish brown solid and are methyln-hexyl ketone contracting quadrol.
(3) application of methyln-hexyl ketone contracting quadrol:
1. for preventing that corrosion (slow releasing function) from appearring in zinc electrode
A. the making of zinc metal sheet
The bulk zinc metal sheet successively uses the sand papering of 400CW, 1000CW, 1200CW, 2000CW smooth smooth, then be cut into the zinc metal sheet of 3 centimetres of 1 cm x, with 2 oil removings of acetone rinsing, use again distilled water flushing 3 times, be placed in the oven for drying of 50 ℃, then encase 2 centimetres of upper end 1 cm x with tetrafluoroethylene envelope band, expose below 1 centimetre of 1 cm x, tested for soaking electrolytic solution.
B. the configuration of electrolytic solution
Add 1.5 gram zinc oxide in the KOH of 50 milliliter of 6 mol/L solution, constantly stir, make its dissolving, can obtain the saturated oxidation zinc electrolyte of 6 mol/L KOH.
C. the test of alternating-current impedance
Use CHI860D electrochemical workstation analyser to be tested, adopt three-electrode system: working electrode is Electrode, the zinc metal sheet (area is 1 square centimeter) that a step is made, Hg/HgO is as reference electrode, and supporting electrode is nickel sheet (2 1 centimetre of cm x 5 cm x); The saturated oxidation zinc electrolyte of 50 milliliter of 6 mol/L KOH that blank electrolysis liquid is the configuration of b step; Corrosion inhibition additive is the methyln-hexyl ketone contracting quadrol that the present embodiment makes, and it is added in above-mentioned electrolytic solution, add that concentration is respectively 2%, 4%, the 5%(mass percent).
During experiment, at first working electrode is dipped in the saturated oxidation zinc electrolyte of 6 mol/L KOH, the open circuit point position is surveyed in examination, until open circuit point position basicly stable rear (three invariant positions after radix point), start to test alternating-current impedance, test parameter is: the point of beginning position is set to the open circuit point position, high frequency is set to 10000 Hz, low frequency is set to 0.01 Hz, sensitivity is made as automatic adjusting sensitivity, simulate equivalent electrical circuit according to ac impedance spectroscopy, and then obtain the working electrode charge-transfer resistance, and be calculated as follows inhibition efficiency:
η?=?(R
P－R
0 P?)/R
P?×100?%
R wherein
pand R
0 prespectively to be added with in the electrolytic solution of the made corrosion inhibition additive of the present embodiment the corrosion reaction charge-transfer resistance of zinc electrode in zinc electrode and blank electrolysis liquid.
The electrochemical AC impedance parameter list of table 1 different concns methyln-hexyl ketone contracting quadrol
As can be seen from Table 1, the methyln-hexyl ketone contracting quadrol of the present embodiment can effectively prevent the corrosive nature of the saturated oxidation zinc electrolyte of 6 mol/L KOH to zinc electrode, and when the mass percent of methyln-hexyl ketone contracting quadrol in electrolytic solution is 5%, corrosion inhibition rate is up to 98.6%.
2. for preventing the zinc electrode dendritic growth, deforming
A. the making of paste spread type zinc electrode
I. the processing of copper mesh: copper mesh is first eliminated rust, then uses the acetone rinsing oil removing by strong acid, highly basic soaking flushing respectively.
II. take zinc oxide 0.6 gram, zinc powder 0.3 gram, oildag 0.05 gram in mortar, grind 5 minutes, make its even mixing, then dripping 5 dehydrated alcohols makes it dispersed, drip again the PTFE emulsion of 1 60% as tackiness agent, after grinding evenly, form the sticking paste of tool.
III. using in the step I copper mesh handled well as skeleton, evenly be applied on copper mesh by the sticking paste of the tool made in the step II and push solidly, copper mesh is covered fully uniformly, then be placed under 50 ℃ and dry, make the paste spread type zinc electrode.
B. the test of cyclic voltammetry curve
Dendrite, distortion easily occur in zinc electrode under alkaline condition, finally cause the damage of zinc electrode, greatly reduce its work-ing life, cyclic voltammetry curve can reflect the stability of zinc electrode charge and discharge process in alkaline electrolyte, usually peak current and spike potential are unstable, show that zinc electrode has dendrite and distortion to produce, also show that the charging and discharging process is affected simultaneously, therefore, can utilize cyclic voltammetry curve research corrosion inhibition additive whether can effectively suppress dendrite, the distortion of zinc electrode.
This test is carried out on CHI860D electrochemical workstation analyser, the paste spread type zinc electrode that the present embodiment of take is made is as working electrode (area is 1 centimetre of 1 cm x), using Hg/HgO as reference electrode, supporting electrode is nickel sheet (2 1 centimetre of cm x 5 cm x), the saturated burnett's solution of the 6 mol/L KOH that blank electrolysis liquid is 50 milliliters, using methyln-hexyl ketone contracting quadrol as corrosion inhibition additive, be added in blank electrolysis liquid as experiment electrolytic solution, the amount of interpolation is set as electrolytic solution containing corrosion inhibition additive 4%(mass percent).
Before test, first allow electrode be immersed in electrolytic solution 2 minutes, until open circuit potential basicly stable after (after radix point, three figure places are constant), just start the test loop volt-ampere curve; Experiment parameter is set to: initial potential is open circuit potential, and noble potential is 0.55 V, and low potential is 0.25 V, and sweep velocity is 0.01 V/s, and the scanning hop count is 200.
Analyzing accompanying drawing can reach a conclusion: when the paste spread type zinc electrode is carried out cyclic voltammetry scan in the saturated oxidation zinc electrolyte of 6 mol/L KOH (blank electrolysis liquid), it is large that peak point current can become with the increase of the circulation number of turns, illustrate that electrode is unstable in charge and discharge process, zinc dendrite and zinc distortion may occur; Added by contrast the 4%(mass percent in blank electrolysis liquid) methyln-hexyl ketone contracting quadrol after, cyclic voltammetry curve peak current and spike potential do not change substantially with the increase of the circulation number of turns, show higher stability, therefore can judge that methyln-hexyl ketone contracting quadrol can suppress the dendritic growth of zinc electrode, deform.
Claims (2)
1. a Containing Schiff-bases tensio-active agent methyln-hexyl ketone contracting quadrol is characterized in that the structural formula of methyln-hexyl ketone contracting quadrol is:
2. the application of methyln-hexyl ketone contracting quadrol according to claim 1, is characterized in that described methyln-hexyl ketone contracting quadrol is applied to conduct in the alkali zinc nickel battery and, for the mercury corrosion inhibition additive, for preventing zinc electrode, the burn into dendritic growth occurs and deform.
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Cited By (7)
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| CN104183873A (en) * | 2014-09-07 | 2014-12-03 | 桂林理工大学 | Electrolyte containing Bi-(p-(N,N,N-dodecyl dimethylamino ammonium bromide) benzaldehyde) hydrazine and preparation method of electrolyte |
| CN104201426A (en) * | 2014-09-07 | 2014-12-10 | 桂林理工大学 | Electrolyte containing 2,4-dinitrophenylhydrazine reduction 4-formylbenzoic acid polyethylene glycol 400 laurate and preparation method of electrolyte |
| CN104201427A (en) * | 2014-09-07 | 2014-12-10 | 桂林理工大学 | Electrolyte containing phenylhydrazine reduction 4-formylbenzoic acid polyethylene glycol 400 laurate surfactant and preparation method of electrolyte |
| CN104241709A (en) * | 2014-09-07 | 2014-12-24 | 桂林理工大学 | Electrolyte containing bis-(p-N,N,N-tetradecyl dimethylamino ammonium bromide) benzaldehyde) hydrazine and preparation method of electrolyte containing bis-(p-N,N,N-tetradecyl dimethylamino ammonium bromide) benzaldehyde) hydrazine |
| CN104332664A (en) * | 2014-09-07 | 2015-02-04 | 桂林理工大学 | Electrolyte containing di-(p-(N,N,N-decyldimethylamino ammonium bromide)benzaldehyde)hydrazine acetal, and its preparation method thereof |
| CN105680103A (en) * | 2014-12-04 | 2016-06-15 | 株式会社杰士汤浅国际 | Alkaline storage battery |
| CN110372537A (en) * | 2019-08-01 | 2019-10-25 | 福州大学 | A kind of Gemini surface active and preparation method thereof containing schiff base structure |
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Cited By (13)
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| CN104332664B (en) * | 2014-09-07 | 2017-01-11 | 桂林理工大学 | Electrolyte containing di-(p-(N,N,N-decyldimethylamino ammonium bromide)benzaldehyde)hydrazine acetal, and its preparation method thereof |
| CN104201426A (en) * | 2014-09-07 | 2014-12-10 | 桂林理工大学 | Electrolyte containing 2,4-dinitrophenylhydrazine reduction 4-formylbenzoic acid polyethylene glycol 400 laurate and preparation method of electrolyte |
| CN104201427A (en) * | 2014-09-07 | 2014-12-10 | 桂林理工大学 | Electrolyte containing phenylhydrazine reduction 4-formylbenzoic acid polyethylene glycol 400 laurate surfactant and preparation method of electrolyte |
| CN104241709A (en) * | 2014-09-07 | 2014-12-24 | 桂林理工大学 | Electrolyte containing bis-(p-N,N,N-tetradecyl dimethylamino ammonium bromide) benzaldehyde) hydrazine and preparation method of electrolyte containing bis-(p-N,N,N-tetradecyl dimethylamino ammonium bromide) benzaldehyde) hydrazine |
| CN104332664A (en) * | 2014-09-07 | 2015-02-04 | 桂林理工大学 | Electrolyte containing di-(p-(N,N,N-decyldimethylamino ammonium bromide)benzaldehyde)hydrazine acetal, and its preparation method thereof |
| CN104201426B (en) * | 2014-09-07 | 2016-05-18 | 桂林理工大学 | Electrolyte contracting to carboxyl benzaldehyde PEG400 laurate containing DNPH and preparation method thereof |
| CN104201427B (en) * | 2014-09-07 | 2016-08-24 | 桂林理工大学 | Electrolyte containing phenylhydrazine contracting p-carboxybenzaldehyde PEG400 laurate surfactant and preparation method thereof |
| CN104183873B (en) * | 2014-09-07 | 2017-01-11 | 桂林理工大学 | Electrolyte containing Bi-(p-(N,N,N-dodecyl dimethylamino ammonium bromide) benzaldehyde) hydrazine and preparation method of electrolyte |
| CN104183873A (en) * | 2014-09-07 | 2014-12-03 | 桂林理工大学 | Electrolyte containing Bi-(p-(N,N,N-dodecyl dimethylamino ammonium bromide) benzaldehyde) hydrazine and preparation method of electrolyte |
| CN105680103A (en) * | 2014-12-04 | 2016-06-15 | 株式会社杰士汤浅国际 | Alkaline storage battery |
| CN105680103B (en) * | 2014-12-04 | 2019-11-26 | 株式会社杰士汤浅国际 | Alkaline storage battery |
| CN110372537A (en) * | 2019-08-01 | 2019-10-25 | 福州大学 | A kind of Gemini surface active and preparation method thereof containing schiff base structure |
| CN110372537B (en) * | 2019-08-01 | 2021-04-27 | 福州大学 | Gemini surfactant containing Schiff base structure and preparation method thereof |
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Application publication date: 20131225 |