CN1312331A - Organic high molecular composite for accumulator and its preparation method - Google Patents
Organic high molecular composite for accumulator and its preparation method Download PDFInfo
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Abstract
The present invention relates to an organic macromolecular composition for lead accumulator, its preparation method and application as electrolyte or chemical solution. said composition contains polyorganosiloxane 0.5-2 portions as component A, organic silicon oil 0.5-2 portions as component B, sulfuric acid whose density is 1.40-1.60 10-50 portions as component C and diluent water 10-300 portions. Fistly the component A and component B are fully stirrd and mixed, then diluted by adding component D, and then mixed with component C. Said invented composition can effectively raise the low-temp. discharge capacity service life and all electric indexes of accumulator and can reduce the corrosion of electrode plate by electrolyte.
Description
The present invention relates to a kind of as lead storage battery ionogen or change into the composition of liquid, particularly relate to organic polymer composition that a kind of lead storage battery uses and preparation method and as ionogen or change into the liquid purposes.
The foundation structure of store battery formed blank before 150 years, its electrochemical principle is that the electrode with two kinds of different metals is dipped in acidity or the alkaline electrolyte, produces electrochemical action between one of them electrode is with electrolytic solution, then just has current potential to exist between electrode.The current potential extent is decided on the metal of composition electrode and the character of electrolytic solution.In the lead storage battery of routine, adopt the distilled water diluting vitriol oil usually as ionogen.The tradition lead acid cell is generally on technology is made, because manufacturing process, acidic electrolyte bath is dealt with improperly can cause large-area environmental pollution after making, use and discard, becomes one of source of pollution to the living environment maximum; A series of shortcomings such as structural relation and corrosive nature owing to electrolyte sulfuric acid and pole plate exist lead storage battery large current charge thermal value big, and work-ing life is short.In use there are hard nut to cracks such as acid mist effusion, interface corrosion in tradition open type lead acid cell, also fails thoroughly to solve the interface etching problem even install the general maintenance-free battery of reduced pressure sealing valve additional, all brings great inconvenience for transportation and use.
In the technical development of nearly decades, repeatedly great reform has appearred in lead acid cell.Wherein industrial process there is great effect, it is the valve controlled type sealed lead accumulator that the shallow company of Japanese soup took the lead in realizing the seventies in 20th century, the structural reform of this shell drops to than low degree the acid mist effusion of lead acid cell, and this sealed lead storage battery has obtained widespread use in communication, illumination and part train starting, traction field at present.In present technological transformation thinking, generally can be summed up as two classes: the one, on plumbic acid principle basis, pole plate is subtracted pound, for example adopt the measure that L glass fiber, conductive plastics replacement lead base grid etc. reduce the pole plate weight of covering.Another kind of innovation thinking is to seek the sulfuric acid pendular ring to protect substitute, and back one direction more and more obtains the various countries expert and payes attention to.As document 1 " solid electrolyte " (Shi Meilun work, science tech publishing house, 1982), introduce in the book: " high-energy-density battery " is as electrolytical with the beta-alumina pottery.Also has sosoloid battery etc.
Organic polymer composite electrolyte of the present invention can increase in time in mixed viscosity, distinguishes with the normal temperature physical aspect and can classify as people's alleged colloidal electrolyte usually.In history, when existing experiment found that micelle in the colloidal sol contact with solid as far back as 1809, meeting formation electrostatic double layer on the liquid-solid two-phase interface.To the mechanism of this particle surface charge source, have multiple explanation at present in theory, as ionization, ionic adsorption, lattice replace, multiple theory such as particle is charged in the non-aqueous media.In industrial process, than adopting liquid electrolyte commonly used such as sulfuric acid, potassium hydroxide, the development of colloidal electrolyte is comparatively slow always, more influential in history practical colloid battery appears at phase early 1950s, and purpose is to solve the military vehicle starting problem of Korea battlefield under severe cold environment at that time.Nineteen sixty-five patent disclosure, this very early time is used the store battery of water glass colloidal electrolyte, is pushed to the commercial market first by German sunlight company.Through development decades, the ripe colloid storage battery of grasping with silicate ionogen main chemical compositions of existing at present many countries, this class colloidal electrolyte formula is all on the books in the patent documentation of various countries.Its advantage is to exempt to use bright sulfur acid, has tentatively adapted to electrolytical environmental protection demand; Shortcoming is that the specific energy of product is little than lead acid cell, and internal resistance is bigger, and in use dehydration sclerosis easily causes product performance and life-span all undesirable.Use the colloidal electrolyte of organic high molecular polymer, in disclosed patent or the technical literature report is being arranged seldom at present.
The objective of the invention is to: 1. the organic polymer that the corrodibility of the application of the invention is lower compound (colloidal state) thing replaces electrolyte sulfuric acid, has improved the easy corrosive degree of lead storage battery interface.2. make of the pollution of pole plate process in order to reduce lead acid cell effectively to environment.3. in order to reduce the corrodibility of ionogen, improve the work-ing life and the specific energy of lead storage battery to the internal storage battery pole plate; 4. bigger in order to overcome existing lead acid cell internal resistance, in use easy dehydration hardened shortcoming, effectively
Improve the comprehensive electric property of lead storage battery, thus the organic polymer composition that provides a kind of store battery to use
And Preparation method and use.
The object of the present invention is achieved like this: the organic polymer composition that a kind of lead storage battery provided by the invention is used, and its composition comprises:
The A component is: molecular weight less than 3000, possess hydrophilic property and chemically active polyorganoelementosiloxane, wherein addition is the 0.5-2 parts by volume;
The B component is an organic silicone oil, and wherein addition is the 0.5-2 parts by volume;
The C component is that density is the sulfuric acid of 1.40-1.60, the 10-50 parts by volume;
The D component is a pure water, the 10-300 parts by volume; When this organic polymer composition was done the ionogen use, the addition of water was the 10-50 parts by volume; Be used as change into liquid when using the addition of water be 50-300 part.The main purpose of adding water is the A+B component after the diluted mixture, and the sulfuric acid density in the compound prescription is adjusted to the density value of required purposes.
Also be included in and add sodium lauryl sulphate or water miscible polyvinyl alcohol (PVA) emulsifying agent in the mixed A+B component, the emulsifying agent addition is 0.1～0.5 parts by volume.
Wherein the A component comprises: main chain backbone has the polyorganoelementosiloxane of m Si-O-Si or C-Si-O segmented structure, and side group (side chain) contains one or more unsaturated hydrophilic active radicals R, as: R is H, OH, SO
2H, NH
2, CH
3Or the like, in existing various countries Chemicals, belonged to conventional products, as " the hydrogenous organo-siloxane of side group " supplied on the market, " organo-siloxane of side group amino-contained " or chloride, contain alkoxyl group, hydroxyl, contain vinyl, amino-contained, contain organo-siloxanes such as cyclosiloxane, its structural formula is:
The m=positive integer;
When composition of the present invention is made ionogen, need select the wetting ability and the chemically reactive of its polymkeric substance to the side group functional group of A component, its molecular weight makes it the flowability that can keep good less than 3000.
Wherein organic silicone oil B component comprises: methyl-silicone oil, ethyl silicon oil, methyl phenyl silicone oil, cyanoethyl methyl polysiloxane etc., should select the organic silicone oil of viscosity during application less than 1500 handkerchiefs.One of B vital role in compound prescription be with the A copolymerization as A molecular structure segment end-capping reagent.In water that (A+B) copolymerization forms and oil phase mixed system, when the reasonable ratio of (A+B) and C and D, can produce and form numerous elementide active centre, the ion motion activity in the raising combined electrolysis plastome there is special booster action.Research thinks that (A+B) the even existence in combined electrolysis plastome can be formed with the passage that is beneficial to the ion orientation movement, makes ion transition therein.Simultaneously, this combined electrolysis plastome helps setting up at electrode and electrolytic solution two-phase interface the absorption electrostatic double layer of dynamic stability, strengthen the activation energy of ion, electrode reaction is speeded up, thereby strengthened the large current discharging capability of acid storage battery in the electrode surface reaction.
C component and D component are used conventional sulfuric acid and the pure water of battery industry.
The preparation method of wood invention is undertaken by following technology:
1, at first be by the A component: molecular weight less than 3000, possess hydrophilic property and chemically active polyorganoelementosiloxane, wherein addition is the 0.5-2 parts by volume;
The B component is an organic silicone oil, and wherein addition is the 0.5-2 parts by volume;
The C component is that density is the sulfuric acid of 1.40-1.60, the 10-50 parts by volume;
The D component is a water, gets material ready, then A component and B component is fully mixed;
2, with the tret D component dilution again of the mixture of the step 1 behind the thorough mixing, and then compound with C, the adjustment by D component addition at last makes the density of C component in prescription be fit to use.
For making the A+B mixed system better mixed, can A component and B component mixed evenly after, add the D component of 0.5-2 part volume earlier, or add sodium lauryl sulphate or water miscible polyvinyl alcohol (PVA) emulsifying agent, the volume proportion of emulsifying agent addition is 0.1～0.5 part.
It should be noted that the concentration range of choice of C component: when C component during with (A+B) chemical combination, the chemical combination concentration of C component is a key issue.Experiment shows that low excessively as the concentration of C component, meeting can not form full and uniform dispersion system because of active deficiency makes compound prescription, produces the coarse particles polymer too early, causes the ion motion ability of composite electrolyte to reduce.If the excessive concentration of C component may make (A+B component) mixed system by strong oxidation again, cause polymkeric substance dehydration carbonization, the ionic activity and the work-ing life of reducing composite electrolyte to occur.When this compound prescription changed into the liquid use as pole plate, the D component addition that should at first use by ionogen mixed, and then continuation tret D component is diluted to the C component density that routine changes into system regulations.
The purposes of the organic polymer composition that a kind of lead storage battery that invention provides is used is ionogen that uses as lead storage battery or the liquid that changes into that is used as battery plate.
Be made as the purposes and the advantage of example explanation organic polymer composition of the present invention below with lead storage battery.
When 1, using as the ionogen of lead storage battery, organic polymer composition of the present invention is in described component ratio range, can select with the sulfuric acid density in the composite electrolyte is benchmark, by C component and the D component ratio calibration same magnitude density to the normal temperature electrolyte sulfuric acid, using method is identical with conventional bright sulfur acid electrolyte.For example the sulfuric acid density in the compound prescription is transferred to 1.26-1.32, be added into the ionogen of in cotton adsorption type lead storage battery, doing of finishing assembling and use by diluting water.During actual the use, should give one's full attention to (A+B component) and C component and add composite electrolyte that the D component mixes formation increased viscosity in time, progressively change colloidal state into, thus best mode be after mixing as early as possible (generally in tens of minutes) be filled into store battery.
When 2, changing into liquid replacement bright sulfur acid use as pole plate, in the described composition ratio range of organic polymer composition of the present invention, increase pure water D component consumption is diluted to pole plate and changes into the required sulfuric acid density of liquid, for example prescription is diluted to sulfuric acid density 1.05～1.08, chemical synthesizing method can adopt conventional pole plate to change into system.Adopting this prescription as the benefit that changes into liquid, at first is because the existence of (A+B component) mixed system in dilute sulphuric acid formed prevention sulfuric acid mist evaporable barrier at liquid-air interface layer.Reduce the acid mist escaped quantity of pole plate formation process, helped environmental protection.Help when changing into simultaneously at the surperficial activated adsorption layer that forms of plate active material, the electrostatic double layer that forms dynamic stability after polar plate solidification and the charging of assembling filling liquid is all had obvious effect.
Adopt organic polymer composition of the present invention to make ionogen and pole plate changes into liquid, produced lead storage battery possesses following superiority:
1. by using organic polymer composite electrolyte prescription, reduced effectively lead storage battery make, use and discarded process to the pollution of environment.
2. store battery effectively adapts to 0.5-2C (A) large current charge, and the normal charge time foreshortens to 1-2 hour.
3. the heavy-current discharge characteristic is good, and the general lead acid cell of high-multiplying power discharge volume ratio is big more than 30%.
4. self-discharge is little, and the capacity rate of descent of depositing of exempting to charge generally can be made to average every month＜2%.
5. cold property is good, and than the big 20-40% of general lead acid cell ,-50 ℃ of environment still can satisfy big electric current and spark-10 ℃ of environment loading capacities.
6. long service life generally can be made to the 500-2000 circulation and be filled time (75% surpassing deep discharge).
7. possess outstanding electric restorability, when battery uses to low potential, only need very short time can return to noble potential certainly, continue output than macro-energy.When intermittent discharge or the use of non-steady load, its discharge voltage profile is indentation in time, and this discharge characteristic utmost point is suitable as power cell and uses.Research is thought, this characteristic is relevant in the system effect of ionogen and polar board surface electrostatic double layer with (A+B component), even under the low voltage electric field environment, the ion transition passage that (A+B component) dispersion system forms helps the pole plate electrostatic double layer to recover original distribution rapidly, thereby has improved the utilization ratio of plate active material.
The present invention is described in more detail below in conjunction with drawings and Examples:
Fig. 1 a-d is 12V.38Ah store battery (" voltage-time " curve that weight 14.1Kg, volume 198 * 166 * 171mm) discharge with 6.6A, 10.89A, 66A and 264A respectively with electrolyte fabrication of the present invention
Fig. 2 is that the 12V.38Ah store battery of making is at-10 ℃ of low temperature environments " voltage-time " curve with the 10.89A discharge when being used as ionogen with composition of the present invention
Fig. 3 is when being used as ionogen with composition of the present invention, the 12V.38Ah store battery of making " voltage-time " curve of 30.4A (0.8C) constant current secondary intermittent discharge
Fig. 4 is when being used as ionogen with composition of the present invention, the 12V.38Ah store battery of making repeatedly " voltage-time " curve of intermittent discharge of 30.5A (0.8C) constant current
Fig. 5 is that the 12V.17Ah store battery of making is used " voltage-time " curve and " energy-time " curve of 3.4A, 17A and 25A constant-current discharge respectively when being used as ionogen with composition of the present invention
Fig. 6 is when being used as ionogen with composition of the present invention, the 12V.17Ah store battery of making " voltage-time " curve of 3.4A constant-current discharge
Fig. 3 center line is represented constant current 30.4A (0.8C) discharge curve;-----line is represented zero load;
Fig. 4 center line is represented constant current 30.5A (0.8C) discharge curve;-----line is represented zero load.
Embodiment 1
In a kind of preferred embodiment of routine, adopt prescription:
A. molecular weight 1200 contains H polysiloxane, 1 part;
B. the methyl-silicone oil of viscosity 1000,1 part;
C. density is 1.58 sulfuric acid, 30 parts;
D. pure water is 28 parts.
With A component and component B fully mixed after, more respectively with D component, C component mixings composite electrolyte, be filled into one finish that pole plate changes into and be equipped with every cotton adsorption type lead storage battery (12V38Ah).After irritating liquid, end during to battery terminal voltage 15.6～16.0V with 3A electric current supplementary charging (also claiming that secondary changes into), continue after the discharge to charge again, the discharge of its 4 kinds of different strength of current " voltage-time " curve such as Fig. 1 a-d show.
In a kind of preferred embodiment of routine, adopt prescription:
A. molecular weight 1600 side groups contain CH
3With the polysiloxane of H, 2 parts;
B. viscosity is less than 1000 methyl-silicone oil, 1.5 parts;
C. density is 1.40 sulfuric acid, 50 parts;
D. surplus is a pure water.
When above-mentioned prescription mixes, earlier the A component is mixed with the B component fully and stir, after adding 30 parts of pure water dilutions then, mix with sulfuric acid again, by the pure water addition sulfuric acid density of compound prescription is adjusted to 1.07 at last, the liquid that changes into as grid type plate uses, and the energising system is identical with the system that changes into of conventional sulfuric acid liquid.In the pole plate formation process, the acid mist escaped quantity obviously lacks an order of magnitude when becoming with the bright sulfur acidifying, thereby has improved the air environmental protection index of this technology.After pole plate changed into and finishes, technology was finished assembling routinely, was filled into embodiment 1 described composite electrolyte, and the secondary chemical synthesizing method is identical.At a 12V.38Ah store battery that adopts this processing method to make, " voltage-time " curve as shown in Figure 2 during its low temperature discharge.
In the conventional preferred embodiment of another kind, the combination matching of embodiment 1 can be adjusted, the proportioning of C component and D component is adjusted into 32 parts and 21 parts respectively, the proportioning of A component and B component is constant, and making processes is identical.Intermittent discharge " voltage-time " curve of a 12V.38Ah store battery of producing with present method as shown in Figure 3.
In another conventional embodiment, the 12V.38Ah store battery that the pole plate that adopts embodiment 2 methods to change into out is equipped with out.Electrolyte formula adds 0.5 part of sodium lauryl sulphate on the basis of embodiment 1 prescription, fully mixed in A component and B component mixed processes, all the other making methods are identical with embodiment 1.Repeatedly intermittent discharge " voltage-time " curve of this store battery as shown in Figure 4.
In a kind of preferred embodiment of routine, adopt prescription:
A. molecular weight 1600 contains NH
2Polysiloxane, 0.9 part;
B. viscosity is less than 1000 methyl-silicone oil, 1.1 parts;
C. density is 1.50 sulfuric acid, 32 parts;
D. diluting water is 24 parts.
Prescription blending means and using method are identical with embodiment 1.The lead storage battery of a 12V17Ah who produces with the can of this prescription, it sees Fig. 5 a-d with " voltage-time " curve and " energy-time " curve of 3.4A, 17A and 25A discharge respectively.
In another conventional preferred embodiment, adopt prescription:
A. molecular weight 1100 side groups contain the polysiloxane of H, 1 part;
B. viscosity is less than 1000 ethyl silicon oil, 1.1 parts;
C. density is 1.53 sulfuric acid, 28 parts;
D. diluting water is 26 parts.
Elder generation is mixed the A component during mixing with the B component, and elder generation adds 2 parts of water and 0.3 part of water miscible polyvinyl alcohol when mixed, and is mixed with D component and C component again after fully mixing, and all the other filling liquid chargingmethods are identical with embodiment 1.What battery plate was used changes into liquid based on this prescription, and further being diluted to sulfuric acid density with pure water is 1.08, adopts the conventional system that changes into.With the 12V17Ah lead storage battery that present method is produced, " voltage-time " curve of its 3.4A discharge, as shown in Figure 6.
Claims (12)
1. organic polymer composition that store battery is used comprises following component and content:
A. polyorganoelementosiloxane 0.5-2 parts by volume;
B. organic silicone oil 0.5-2 parts by volume;
C. density is the sulfuric acid 10-50 parts by volume of 1.40-1.60;
D. diluting water, the 10-300 parts by volume.
2. the organic polymer composition that a kind of store battery as claimed in claim 1 uses, it is characterized in that: also be included in and add sodium lauryl sulphate or water miscible polyvinyl alcohol emulsifying agent in the mixed A+B component, its emulsifying agent addition is 0.1～0.5 parts by volume.
3. the organic polymer composition that a kind of store battery as claimed in claim 1 uses is characterized in that: when the organic polymer composition that described store battery uses changed into the liquid use as pole plate, D component addition was 50-300 part.
4. the organic polymer composition that a kind of store battery as claimed in claim 1 uses is characterized in that: when the organic polymer composition that described store battery uses was done the ionogen use, D component addition was the 10-50 parts by volume.
5. the organic polymer composition used of the described a kind of store battery of claim 1, it is characterized in that: described A component is the polyorganoelementosiloxane with m Si-O-Si or C-Si-O segmented structure, side group contains one or more unsaturated hydrophilic active group, and its molecular weight is less than 3000.
6. the organic polymer composition used of the described a kind of store battery of claim 1, it is characterized in that: the side group of described A component contains one or more unsaturated hydrophilic active group, comprising: H, OH, SO
2H, NH
2, CH
3Or organic active group.
7. the organic polymer composition that a kind of store battery as claimed in claim 6 is used is characterized in that: the contained organic active group of described A side group is band polarity or ionic group, comprises H, OH, SO
2H, NH
2, CH
3Or other active group.
8. the organic polymer compound prescription that a kind of store battery as claimed in claim 1 uses, it is characterized in that: described B component comprises: methyl-silicone oil, ethyl silicon oil, methyl phenyl silicone oil, cyanoethyl methyl polysiloxane or contain the organic silicone oil of other active group, its viscosity are less than 1500 handkerchiefs.
9. the organic polymer composition that a kind of store battery as claimed in claim 5 is used is characterized in that: described A component is the polyorganoelementosiloxane with m Si-O-Si or C-Si-O segmented structure, wherein m=positive integer.
10. method for preparing the organic polymer composition that the described a kind of store battery of claim 1 uses is characterized in that: carry out according to the following steps: (1), at first get the raw materials ready by following composition and content;
The A component is: molecular weight less than 3000, possess hydrophilic property and chemically active polyorganoelementosiloxane, wherein addition is the 0.5-2 parts by volume;
The B component is an organic silicone oil, and wherein addition is the 0.5-2 parts by volume;
The C component is that density is the sulfuric acid of 1.40-1.60, the 10-50 parts by volume;
The D component is a pure water, and 10-300 parts by volume water is got material ready;
(2), then A component and B component are fully mixed;
(3), tret D component 10-50 part dilution again in the mixture that the step 2 behind the thorough mixing is obtained, and then the C component sneaked into, the adjustment by D component addition at last makes the density of C component in prescription reach the desired density value of use.
11. the method for the organic polymer composition that preparation store battery as claimed in claim 10 is used, it is characterized in that: also be included in A component and B component mixed evenly after, when adding the D component of 0.5-2 part volume earlier, add sodium lauryl sulphate or water miscible polyvinyl alcohol emulsifying agent, the emulsifying agent addition is 0.1～0.5 parts by volume.
12. the purposes of the organic polymer mixture that uses as the described any described a kind of store battery of claim 1-9 is characterized in that: the ionogen that described organic polymer mixture uses as lead storage battery or as the liquid that changes into of battery plate.
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| CN101552354B (en) * | 2008-04-03 | 2011-12-07 | 鞍山夺标化工机电股份有限公司 | Storage battery electrolyte prepared by organic silicon and inorganic silicon |
| CN103268966A (en) * | 2013-05-07 | 2013-08-28 | 杭州储蕴丰科技有限公司 | Electrolyte additive for substantially prolonging lead-calcium battery service life, preparation method and use method thereof |
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| CN107611491A (en) * | 2017-08-30 | 2018-01-19 | 东莞恒量新能源科技有限公司 | A kind of additive package for lead accumulator and preparation method thereof |
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- 2001-02-23 CN CNB01104182XA patent/CN1152923C/en not_active Expired - Fee Related
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| CN103268966A (en) * | 2013-05-07 | 2013-08-28 | 杭州储蕴丰科技有限公司 | Electrolyte additive for substantially prolonging lead-calcium battery service life, preparation method and use method thereof |
| CN103268966B (en) * | 2013-05-07 | 2015-09-16 | 杭州储蕴丰科技有限公司 | Significantly extend the electrolysis additive in lead calcium cell life-span and preparation, using method |
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