CN1167345A - Colloid electrolyte of high electric capacity and making method - Google Patents
Colloid electrolyte of high electric capacity and making method Download PDFInfo
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- CN1167345A CN1167345A CN96117578A CN96117578A CN1167345A CN 1167345 A CN1167345 A CN 1167345A CN 96117578 A CN96117578 A CN 96117578A CN 96117578 A CN96117578 A CN 96117578A CN 1167345 A CN1167345 A CN 1167345A
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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
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- Y02E60/10—Energy storage using batteries
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Abstract
The present invention relates to a colloidal electrolyte with high electric capacity and its preparation method. Said colloidal electrolyte is formed from (mass percentage) 9-18% of silicasol and 10-30% of sulfuric acid, and the mass ratio of sulfuric acid/silicon dioxide is 0.56-3.3%. Its preparation method is characterized by that the silicasol is made into gel, and its large part of sodium ions is washed off, then said gel and sulfuric acid and distilled water are passed through the process of mixing-reaction in an acid-proof reactor, and its reaction temp. is controlled below 50 deg.C, then cooled for 2-5 hr, so that the inveted colloidal electrolyte with high electric capacity can be made up. After having been cooled to room temp., said colloidal electrolyte is poured into accumulator, and processed by twice charging and discharging process so as to can obtain high-capacitance colloidal accumulator.
Description
The present invention relates in lead-sour battery not flowing electrolyte and method for making thereof, just have colloid electrolyte of high electric capacity and manufacture method thereof in the lead acid accumulator.
Lead-acid battery as one of principal item of storage battery, is widely used in industry-by-industry always.But ooze the excessive acid of acid, generation acid mist pollution environment because it exists, shortcomings such as working service inconvenience have caused a lot of troubles to the user.
Use the colloidal silica electrolyte that sulfuric acid absorption is formed solidifying phase in recent years in colloid, make colloidal electrolyte accumulator, thereby avoided the phenomenon of oozing, overflow of sulfuric acid.Many people are used at the colloidal silica electrolyte having done a large amount of work aspect the research of storage battery, have produced numerous patents and non-patent literature.
Chinese patent CN2045148 document discloses a kind of double colloidal layers colloid storage battery, battery designs is become double-layer structure up and down, and the bottom gel is by 8～10% sodium metasilicate, 6～8.5% silicon dioxide, 1～2% phosphoric acid, 0.05～0.15% polyvinyl sulfuric acid sodium and dilute sulfuric acid are formed.The top layer gel is by 15～22% sodium metasilicate, 3～6% silicon dioxide, and 1～2% phosphoric acid and dilute sulfuric acid are formed.
Provided a kind of method for making of high power capacity colloid storage battery, it is characterized in that for Chinese patent literature CN2072278 number: buffer unit is equipped with at the top at storage battery, and the acid mist processing unit is housed on hand-hole.
Provided a kind of prescription of colloidal electrolyte of high-capacitance Chinese patent literature CN1056019 number, contained silicon dioxide 3～9.9% in the colloid, sulfuric acid 48.1～75%, aluminium hydroxide 0.1～0.5%; Wherein the weight ratio of sulfuric acid and silicon dioxide is 4.5～10.5%.The purpose of this invention is colloidal electrolyte and the method for making thereof that provides a kind of novel, high-capacitance.
In above-mentioned document, the sodium metasilicate in the colloidal electrolyte that has and the ratio of sulfuric acid are improper, still exist the seepage phenomenon of acid, and what have will change electrode structure, use special material to make, and make storage battery manufacturing work complicated more, and cost improves, and is unfavorable for promoting; Simultaneously, because the proportioning of each composition of colloidal electrolyte is unreasonable, and be added with additive, it is bigger that the capacitance that makes colloid storage battery and the capacitance of existing lead acid accumulator are compared gap, capacitance only reaches about 80% of similar lead acid accumulator generally speaking, be exactly the best result that Chinese patent literature CN1056019 provides, its peak capacity just reaches 91.6%.Be still current urgency technical problem to be solved so how to improve the capacitance of colloid storage battery.
The objective of the invention is to, can produce the higher colloid storage battery of capacitance after making the colloidal electrolyte of generation be used to pour into storage battery.And the colloidal electrolyte that generates is difficult for aquation, is difficult for be full of cracks, has good thixotropy, is convenient to disposable perfusion, and is easy to operate.With the storage battery of this electrolyte perfusion, long service life, discharge performance is stable, and starting performance is good, and the self discharge coefficient is little, is suitable for high-power power supply, and working service is convenient.
The present invention also aims to provide a kind of method for preparing above-mentioned colloid electrolyte of high electric capacity, method is simple for this, is easy to behaviour and uses.
The present invention also aims to be convenient to the large-scale production of colloid storage battery, production cost reduces.
Purpose of the present invention is again, makes the process of preparation colloidal electrolyte be convenient to operator's safety in production, in the production process, does not produce acid mist, and the colloid storage battery acid non-permeability of generation, the acid of not overflowing can not cause environmental pollution.
Purpose of the present invention is achieved by following means.
In a kind of colloidal electrolyte of high-capacitance, the colloidal electrolyte of per 100 gram masses contains Ludox (in silicon dioxide) 9～18%, sulfuric acid 10～30%.Its mass ratio is 0.56～3.3%.
Colloidal electrolyte of a kind of high-capacitance and preparation method thereof makes the silicon gel with commercially available Ludox or the Ludox and the distilled water that utilize sodium silicate solid to be mixed with; Again the silicon gel is used the most of sodium ion in the distilled water flush away silicon gel colloid; Again the silicon gel washed and sulfuric acid, distilled water are joined and carry out hybrid reaction in the acid tolerance response container, constantly stir in the course of reaction, and with coolings such as salt solution or frozen water, the order that the three adds is: earlier sulfuric acid is slowly splashed in (under agitation) distilled water, make dilute sulfuric acid, be chilled to room temperature; Add the colloidal solution that silicon gel and distilled water form again, and the control temperature is no more than 50 degree, the pH value is 4～7.If＜4, then continue to drip colloidal silica solution, the pH value of rising solution; If＞7 o'clock, continue to drip dilute sulfuric acid, reduce the pH value of solution; To control the scope that the pH value is requiring.Make at last in the colloidal electrolyte of generation to contain silicon dioxide 9～18%, sulfuric acid 10～30% dropwises, and continues to stir, reaction, cooling 2～4 hours, up to room temperature; So just made the colloidal electrolyte of high-capacitance.
The colloid electrolyte of high electric capacity that generates is poured in the lead acid accumulator vessel shell of getting ready, carry out twice 48～72 hours chargings and discharge process, promptly made the colloid storage battery of high-capacitance with voltage 380V, electric current 5～15A.
In above-mentioned preparation process, the most of sodium ion in the flush away Ludox is the electrolytical key of preparation high-capacitance, and experiment shows: sodium ions content is low more, and the capacitance of colloidal electrolyte is high more.
The operation of most of sodium ion is performed such in the flush away Ludox: the Ludox that will contain distilled water with cloth encases, and puts into drier or centrifuge, dehydration; Again the silicon gel is immersed in the distilled water after the dehydration, and then encase spin-dry; So repeat six to eight times.
The consumption of sulfuric acid also is the requisite key factor of preparation colloid electrolyte of high electric capacity, and when the content of sulfuric acid in colloid was lower than 10%, the capacitance of silica-gel accumulator obviously reduced, when being higher than 30%, easily form gel faster, and be difficult for pouring into storage battery, produce acid mist simultaneously.So sulfuric acid content is that the better performances and the capacitance of the colloidal electrolyte that made in 10～30% o'clock is higher, is preferable span with 11～26% wherein.
Generating the reacting liquid pH value size of colloidal electrolyte, is to influence the colloid-stabilised key factor of solution.When the pH value was 4～7, colloidal sol was more stable.If pH value＜4.5 o'clock, the time of formation gel is longer; When the pH value surpasses 7, easily form gel quickly, be difficult for can.
The consumption of silica gel when less than 9% the time, forms the chronic of gel, often surpasses 7 hours, and the gel strength of formation is low, can be destroyed in charging process, produce hydration phenomena; When greater than 18% the time, easily very fast formation gel, viscosity is big, and intensity is big, is difficult for can, easily produces crack performance after the charging again.So dioxide-containing silica is that the performance and the capacitance of the colloidal electrolyte that made in 9～18% o'clock is better, is preferable span with 10-16% wherein.
Experiment shows: in the colloidal electrolyte reaction that forms, contain silicon dioxide 9-18% at Ludox, in the scope of sulfuric acid 10-30%, when the mass ratio of sulfuric acid and silicon dioxide was 0.56-3.3%, the colloidal electrolyte capacitance superior performance that makes was better.The raw material of preparation colloidal electrolyte: commercially available Ludox, wherein the content of silicon dioxide is 10～30%, proportion 1.06～1.22, pH value is 8～9.5, iron-holder less than 100,000/, also can use sodium silicate solid prepare silicon colloidal sol as raw material.
Sulfuric acid gets final product with diluting concentrated sulfuric acid with commercially available laboratory.High-quality pure, analyze various credit ratings such as pure, chemical pure, technical pure all can be used as raw material.
The present invention is described in further detail below in conjunction with embodiment.
At first a certain amount of sodium silicate solid is dissolved in distilled water, is made into saturated solution, make with distilled water again and solidify the attitude colloid; Or with commercially available Ludox and distilled water mixed gel; Prepared gel is used the most of sodium ion in the distilled water flush away colloid, most of sodium is performed such from the operation of giving in the flush away Ludox: the Ludox that will contain distilled water with cloth encases, and puts into drier or centrifuge, dehydration again; Again the silicon gel is immersed in the distilled water after the dehydration, and then encase spin-dry; So repeat six to eight times; Again the colloid of cleaning is mixed, stirred with sulfuric acid, distilled water, make it reaction, be cooled to room temperature,, when pH equals 4.5～7, mixed liquor is poured in the lead accumulator, cooling, reaction precipitated silicic acid gel with the check of pH test paper.
Then charged 48～72 hours to storage battery with the voltage and current of 380V, 10～15A (1); (2) discharging after substituting the bad for the good, is that 2.2 (± 0.1) V stops discharge up to monomer voltage; (3) recharged (under 380V, 10～15A voltage, electric current) 48～72 hours, till single battery voltage is 2.8 (± 0.1) V.
Compare with the colloid storage battery of prior art with the colloid storage battery of this electrolyte fabrication and to have following characteristics:
(1) long service life.Between 250～300 times, and conventional accumulators has only 108 times according to experiment life-span cycle-index.
(2) the few maintenance.Every 6 months, only the distilled water that need add about 10ml got final product, and does not need to add acid in addition or adds water acid adjustment degree.
(3) this storage battery be not afraid of self discharge, overcharge, reverse charge.
(4) this capacity of the accumulator reaches more than 95%, is up to 99%.Be applicable to the high power discharge starting.
(5) pollution-free.This storage battery because sulfuric acid content is 10～30% to have descended 1.6 times to 3 times even 6～7 times than original 48.1～75% in the colloid, does not produce acid mist in the charge and discharge process, outwards do not spatter, leak sour, and fail safe is better.
(6) colloidal electrolyte of the present invention does not need doping, has simplified production routine, has reduced cost, more helps the production of storage battery.
(7) this colloid storage battery can be+45 ℃ to-45 ℃ following operate as normal.
(8) this colloid storage battery directly utilizes the housing of original dress lead acid accumulator and electrode structure as the container filling of the high-capacitance colloid of preparation, makes storage battery, helps scale, batch process, has saved the trouble that designs new housing.
Further specify the present invention with indefiniteness embodiment below.
Embodiment 1:
With commercially available Ludox (contain silicon dioxide 30%, density 1.22, pH9.5) distilled water carried out mixed silicon gel in 9: 8 by volume: again with distillation washing 6 times, the most of sodium ion of flush away, recording silicon gel voltage through voltmeter is 0.2 volt; Again with 92% sulfuric acid distilled water diluting; With silicon gel distilled water diluting, sulfuric acid after will diluting then and silicon gel are under stirring and the condition with cold salt ice water for cooling, be added drop-wise in the container of acid tolerance response and react, the control rate of addition, make reaction temperature be no more than 50 ℃, contain silica 1 6% in the colloidal electrolyte of Sheng Chenging at last, sulfur acid 26%, the mass ratio of sulfuric acid/silicon dioxide is 1.62, reaction, stirring were cooled off 5 hours down, reach room temperature, the milky colloidal electrolyte that generates is poured in the storage battery, form gel after about 2.5 hours.
Under the state of voltage 380V, electric current 10A, carry out the charge and discharge process 60 hours twice.Obtain the colloid storage battery of capacitance 95%.
This battery not aquation, do not chap, can store 2～3 years.
Embodiment 2:
This implementation method is substantially with embodiment 1, and its difference is that raw silicon colloidal sol contains silicon dioxide 20%, and the pH value is 8.5, and density is 1.1g/cm
3Raw material sulphuric acid content is 98.3%: making that sulfur acid is 30% in the colloidal electrolyte of generation, contain silicon dioxide is 12%, sulfuric acid/silicon dioxide quality ratio is 2.5: control reaction temperature is lower than 50 ℃, adding the raw material reaction time is 3 hours, and cooling and stirring 4 hours is chilled to room temperature, poured into the storage battery gelling time 2.5 hours, discharge and recharge and finish, capacitance is 94%, stores 2.5 years and does not chap, aquation not.
Embodiment 3:
Operation is substantially with embodiment 1, and its difference is that it is 18% that raw silicon colloidal sol contains silicon dioxide, and pH value 9, density are 1.1g/cm
3: raw materials used sulfuric acid is 88%, and the colloidal electrolyte of generation contains silica 1 0%, sulfur acid 23%, and the mass ratio 2.3 of sulfuric acid/silicon dioxide, the capacity of the accumulator of generation are 90.8%.This battery storage did not chap and aquation in 3 years.
Embodiment 4:
Operation is substantially with embodiment 1, and its difference is that it is 25% that raw silicon colloidal sol contains silicon dioxide, and pH value 9.2, density are 1.16g/cm
3: raw materials used sulfuric acid is 95.2%, and the colloidal electrolyte of generation contains silica 1 3.2%, sulfur acid 29.2%, and the mass ratio 2.22 of sulfuric acid/silicon dioxide, continues to stir 3.5 hours cool to room temperature time at 2.8 hours charging reaction time; Pour into and generate gel time 2.5 hours behind the storage battery, capacitance 99%, stores 3 years aquation not chaps.
Embodiment 5:
Operation is substantially with embodiment 1, and its difference is that it is 29% that raw silicon colloidal sol contains silicon dioxide, and pH value 8, density are 1.18g/cm
3: raw materials used sulfuric acid is 90%, and the colloidal electrolyte of generation contains silica 1 7.5%, sulfur acid 25%, and the mass ratio 1.43 of sulfuric acid/silicon dioxide, the capacity of the accumulator of generation are 97.2%, store not aquation and be full of cracks in 2,3 years.
Embodiment 6:
Operation is substantially with embodiment 1, and its difference is that it is 27% that raw silicon colloidal sol contains silicon dioxide, and pH value 8.8, density are 1.12g/cm
3: raw materials used sulfuric acid is 93%, and the colloidal electrolyte of generation contains silicon dioxide 9%, sulfur acid 28.7%, the mass ratio 3.20 of sulfuric acid/silicon dioxide, capacitance 91.5%, store 2.8 years aquation not.
Embodiment 7:
Operation is substantially with embodiment 1, and its difference is that it is 12% that raw silicon colloidal sol contains silicon dioxide, and pH value 8.0, density are 1.06g/cm
3: raw materials used sulfuric acid is 95.2%, and the colloidal electrolyte of generation contains silica 1 0%, sulfur acid 14.%, and the mass ratio 1.40 of sulfuric acid/silicon dioxide, the capacitance 92% of the colloidal electrolyte that obtains stores not aquation, be full of cracks in 2 years.
Embodiment 8:
Operation is substantially with embodiment 1, and its difference is that it is 16% that raw silicon colloidal sol contains silicon dioxide, and pH value 8.1, density are 1.09g/cm
3: raw materials used sulfuric acid is 68%, and the colloidal electrolyte of generation contains silicon dioxide 9%, sulfur acid 10.%, and the mass ratio 1.1 of sulfuric acid/silicon dioxide, the capacitance 91.8% of the colloidal electrolyte that obtains stores not aquation, be full of cracks in 2 years.
Embodiment 9:
Operation is substantially with embodiment 1, and its difference is that it is 25% that raw silicon colloidal sol contains silicon dioxide, and pH value 8.2, density are 1.1g/cm
3: raw materials used sulfuric acid is 95.6%, and the colloidal electrolyte of generation contains silica 1 5.8%, sulfur acid 10.5%, and the mass ratio 0.66 of sulfuric acid/silicon dioxide, the capacitance 94.6% of the colloidal electrolyte that obtains stores not aquation, be full of cracks in 2 years.
Embodiment 10:
Operation is substantially with embodiment 1, and its difference is that it is 26.7% that raw silicon colloidal sol contains silicon dioxide, and pH value 8.3, density are 1.13g/cm
3: raw materials used sulfuric acid is 82.%, and the colloidal electrolyte of generation contains silica 1 7%, sulfur acid 11.3%, and the mass ratio of sulfuric acid/silicon dioxide is 0.66, the capacitance 93.4% of the colloidal electrolyte that obtains stores not aquation, be full of cracks in 2 years.
Embodiment 11
At first a certain amount of sodium silicate solid is dissolved in distilled water, being made into sodium metasilicate content is 18% saturated solution, makes with distilled water and solidifies the attitude colloid; Again prepared gel is washed 6～8 times with distillation, most of sodium ion in the flush away colloid, at last, the colloid that to wash is operated routinely to be stirred down with dilute sulfuric acid, distilled water that Dilution of sulphuric acid with raw material 96% forms and is mixed again, makes it reaction, is cooled to room temperature, with the check of pH test paper, when pH equals 4.5～7, mixed liquor is poured in the lead accumulator housing, and cooling, reaction precipitated silicic acid gel have so just made the colloid storage battery of high-capacitance.
Then charged 68 hours to storage battery with the voltage and current of 380V, 13A (1); (2) discharge after substituting the bad for the good, when voltage is 2.2～2.4V, stop discharge; (3) recharged (under 380V, 13A voltage, electric current) 60 hours, single battery voltage is 2.6～2.8V.
The colloid storage battery capacitance made from the method is 93.8%, stores not aquation and be full of cracks in 2.5 years.
Claims (7)
1, a kind of colloidal electrolyte of high-capacitance is mainly made by Ludox that contains sodium metasilicate and sulfuric acid reaction, it is characterized in that: contain Ludox (in silicon dioxide) 9-18%, sulfuric acid 10～30% in per 100 gram colloidal electrolytes.
2, the colloidal electrolyte of high-capacitance according to claim 1 is characterized in that, the mass ratio of sulfuric acid and silicon dioxide is about 0.56～3.3% in above-mentioned concentration range.
3. the colloidal electrolyte of high-capacitance according to claim 1, wherein adding Ludox, to make the amount that contains Ludox (in silicon dioxide) in the colloidal electrolyte be preferable span with 10～16%.
4. the colloidal electrolyte of high-capacitance according to claim 1, wherein to make in the colloidal electrolyte vitriolated amount be 11～26% to be preferable span to the sulfuric acid of Jia Ruing.
5, a kind of process for preparing colloid electrolyte of high electric capacity as claimed in claim 1, it is characterized in that, with commercially available Ludox or utilize the Ludox and the distilled water of sodium silicate solid preparation to make the silicon gel, again the silicon gel is washed six to eight times the most of sodium ion in the flush away colloid with distillation; Silicon gel and sulfuric acid, the distilled water of the most of sodium ion of flush away are carried out hybrid reaction, constantly stir in the course of reaction, with coolings such as salt, frozen water, below temperature control 50 degree, reinforced finishing continues to stir, cooled off 2-4 hour, when reducing to room temperature, promptly obtain colloid electrolyte of high electric capacity.
6, preparation technology's method of high-capacitance colloid according to claim 5 is characterized in that: the operation of most of sodium ion is performed such in the flush away Ludox: the Ludox that will contain distilled water with cloth encases, and puts into drier or centrifuge, dehydration; Again the silicon gel is immersed in the distilled water after the dehydration, and then encase spin-dry; So repeat six to eight times.
7, preparation technology's method of high-capacitance colloid according to claim 5, it is characterized in that: the Ludox of adding and sulfuric acid make and contain silicon dioxide Ludox 9～18% (quality) in the colloidal electrolyte, sulfuric acid is 10～30% (quality), and the better scope of its mass ratio is 0.56～3.3%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN96117578A CN1167345A (en) | 1996-06-05 | 1996-06-05 | Colloid electrolyte of high electric capacity and making method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN96117578A CN1167345A (en) | 1996-06-05 | 1996-06-05 | Colloid electrolyte of high electric capacity and making method |
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| CN1167345A true CN1167345A (en) | 1997-12-10 |
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| CN96117578A Pending CN1167345A (en) | 1996-06-05 | 1996-06-05 | Colloid electrolyte of high electric capacity and making method |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2002101866A1 (en) * | 2001-06-12 | 2002-12-19 | Yuesheng Feng | A liquid low-sodium silicate electrolyte used for a storage battery and manufactured by magnetization process, and the usage thereof |
| WO2002101867A1 (en) * | 2001-06-12 | 2002-12-19 | Yuesheng Feng | A liquid low-sodium silicate forming-solution used for a storage battery, and a container formation method |
| WO2008077391A1 (en) * | 2006-12-22 | 2008-07-03 | White Fox Technologies Ltd | Fuel cell |
| CN102723530A (en) * | 2012-06-29 | 2012-10-10 | 无锡华燕新电源有限公司 | Colloidal electrolyte of storage battery of electric vehicle and configuration method thereof |
| CN104064818A (en) * | 2014-05-12 | 2014-09-24 | 超威电源有限公司 | Internal formation colloidal electrolyte of storage battery and preparation method of internal formation colloidal electrolyte |
| CN111952589A (en) * | 2020-06-30 | 2020-11-17 | 黄俊雄 | Nano activating agent of lead-acid storage battery and preparation method thereof |
-
1996
- 1996-06-05 CN CN96117578A patent/CN1167345A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2002101866A1 (en) * | 2001-06-12 | 2002-12-19 | Yuesheng Feng | A liquid low-sodium silicate electrolyte used for a storage battery and manufactured by magnetization process, and the usage thereof |
| WO2002101867A1 (en) * | 2001-06-12 | 2002-12-19 | Yuesheng Feng | A liquid low-sodium silicate forming-solution used for a storage battery, and a container formation method |
| WO2008077391A1 (en) * | 2006-12-22 | 2008-07-03 | White Fox Technologies Ltd | Fuel cell |
| CN102723530A (en) * | 2012-06-29 | 2012-10-10 | 无锡华燕新电源有限公司 | Colloidal electrolyte of storage battery of electric vehicle and configuration method thereof |
| CN104064818A (en) * | 2014-05-12 | 2014-09-24 | 超威电源有限公司 | Internal formation colloidal electrolyte of storage battery and preparation method of internal formation colloidal electrolyte |
| CN111952589A (en) * | 2020-06-30 | 2020-11-17 | 黄俊雄 | Nano activating agent of lead-acid storage battery and preparation method thereof |
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