CN105355987A - Preparation method for nanoscale silicon oxide composite dispersion liquid - Google Patents
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Abstract
The invention discloses a preparation method for nanoscale silicon oxide composite dispersion liquid, belongs to the technical field of nanomaterial preparation, and solves the problems of low stability, high probability of demulsification, non-ideal gel forming state, and high usage amount of gel in the existing nanoscale silicon oxide sol. The preparation method comprises a step of adding a dispersing agent, a step of adding the nanoscale silicon oxide, a step of adjusting the PH value and a step of adding compatibilizer in sequence; and the prepared nanoscale silicon oxide composite dispersion liquid is colorless transparent liquid, the PH value of the composite dispersion liquid is 9-12, the specific gravity at the temperature of 25 DEG C is 1.07-1.13 g/cm3, and the viscosity at the temperature of 25 DEG C is 1.71-1.78 mPa.S. The preparation method for the nanoscale silicon oxide composite dispersion liquid effectively solves the problems of difficulty in adding gel and the non-ideal gel forming state in using domestic and overseas gel electrolyte products, so that the quality of the conventional storage battery product is improved.
Description
Technical field
The invention belongs to technical field of nanometer material preparation, be specifically related to a kind of preparation method of nano silicon oxide composite dispersion liquid.
Background technology
When China's lead acid accumulator production capacity is 2.8 hundred million kilovolt-amperes, exceed 2/3rds of global total amount, in recent years whole industry output with 20% speed increase, at present, lead acid accumulator also there is energy density and power density is low, the problems such as suitable environment is temperature limited, 12 plan the nuclear energy of new generation explicitly pointed out, solar thermal utilization and photovoltaic and photothermal generating, wind power technology is equipped, intelligent grid and plug-in hybrid-power automobile, the development of pure electric automobile industry, propose higher to its matching used lead accumulator product quality and service condition, harsher requirement.
Gelled lead acid battery is as the one of valve-regulated lead-acid battery, be the novel product adopting colloidal electrolyte to replace electrolyte sulfuric acid on the basis of traditional lead acid batteries, be widely used in the applications such as electric power, telecommunications, the power supply system for communications, the military communication station, electric automobile.Gelled lead acid battery have convenient transportation, acid nonleakage, slow without acid mist, water consumption, have extended cycle life, suppress pole plate to corrode and distortion, prevent active material from coming off, the advantage such as maintenance period is long.
The performance quality of gelled lead acid battery depends on its gel that uses, and gel conventional in the market mainly contains two types: one is adopt fumed nano silica to be gel, and two is adopt colloidal silica as gel.
With fumed nano silica powder for gel, after the colloidal electrolyte perfusion battery of preparation, although the performance of lead acid accumulator can be improved, extend service life cycle, prevent acid liquor leakage, but still there is shortcomings, such as: prepared in the process of colloid by gaseous oxidation silicon, dust pollution operational environment; Silicon oxide particle is assembled serious, is difficult to dispersion, perfusion difficulty in the battery, poor to the permeability of accumulator plate and dividing plate; Reach the performance promoting colloid battery, need larger silica consumption, the used in amounts of usual silica powder will reach 6 ~ 10%.
Using colloidal silica as gel, can electrolyte leakage be prevented, improve operational environment, but the colloid generated is unstable, and under the mode of operation of deep discharge, colloid easily occurs aquation, lamination, loses original colloid property, shortens the useful life of battery.Due to adding of Ludox, the capacity of lead acid accumulator is reduced.
The particle diameter of nano oxidized silicon grain and specific area are the key factors affecting its performance, and particle diameter is less and specific area is larger, then its activity is higher, affinity and reinforcing property better, the adhesion of product is stronger.
Colloidal silica preparation is easy, overcomes aerosil dust, but poor stability, easily produce demulsifying phenomenon; Storage battery keeps electrolytical ability inadequate, and under different mechanics and environmental condition, easily occur hydration phenomena after gel, plastic state is undesirable, and the use amount of colloid is high; The gel time of colloid and gel strength are not easy to control, and also there is the problem of poor permeability during filling.As the colloidal silica of Akzo Nobel N.V. of Sweden, be made up of nano silicon oxide and deionized water etc., it is creamy paste pasty state, and the proportion at 25 DEG C is 1.2 ~ 1.4g/cm
3, the viscosity at 25 DEG C is 7.5mPaS; When being mixed to form electrolyte with sulfuric acid, for translucent muddiness, there is clustering phenomena; Addition under the electrolyte equal strength formed is comparatively large, and only partial penetration in storage battery, forms starchiness and pile up; The major reason of these problems is caused to be that nano silicon oxide particle diameter is wherein little not and specific area is large not.
Summary of the invention
The invention provides a kind of nano silicon oxide composite diffusion liquid and preparation method thereof, solve existing colloidal silica poor stability, easily produce demulsifying phenomenon, plastic state is undesirable, colloid use amount is high problem.
The preparation method of a kind of nano silicon oxide composite dispersion liquid provided by the present invention, order comprises and adds dispersant step, plus nano silica step, adjustment pH value step and add bulking agent step, it is characterized in that:
(1) add dispersant step: add deionized water in a kettle., then add the dispersant of mass percent 0.5% ~ 6%, the stabilizer of 0.1% ~ 5% that account for nano silicon oxide powder, at 20 DEG C ~ 50 DEG C temperature, stir 10 minutes ~ 15 minutes;
(2) plus nano silica step: in the liquid that step (1) obtains, add nano silicon oxide powder, nano silicon oxide powder accounts for the mass percent 5% ~ 11% of nano silicon oxide composite dispersion liquid, at 20 DEG C ~ 50 DEG C temperature, stirs 5 minutes ~ 10 minutes; Described nano silicon oxide powder particle size is 5 ~ 10nm, its specific area >=1100 ㎡/g;
(3) pH value step is adjusted: in the liquid that step (2) obtains, add alkali lye, at 20 DEG C ~ 50 DEG C temperature, stir 30 minutes ~ 120 minutes, pH value is adjusted to 9 ~ 12;
(4) bulking agent step is added: in the liquid that step (3) obtains, add the bulking agent of the mass percent 0.1% ~ 5% accounting for nano silicon oxide powder, at 20 DEG C ~ 50 DEG C temperature, stir 15 minutes ~ 30 minutes, obtain nano silicon oxide composite dispersion liquid, described nano silicon oxide composite dispersion liquid is colourless transparent liquid, and pH value is the proportion at 9 ~ 12,25 DEG C is 1.07 ~ 1.13g/cm
3, the viscosity at 25 DEG C is 1.71 ~ 1.78mPaS.
In described step (1), described dispersant is polycarboxylate sodium, alkyl polyoxyethylene ether (paregal O), AEO, polyethylene glycol or glycerine; Described stabilizer is dextrin, CMC, hydroxyethylcellulose or polyvinyl alcohol;
In described step (3), described alkali lye is NaOH, potassium hydroxide, lithium hydroxide or ammoniacal liquor;
In described step (4), described bulking agent is one or more in ammoniacal liquor, phosphoric acid, lithium hydroxide, molybdenum oxide, stannous sulfate, nano-sized carbon.
Nano silicon oxide composite dispersion liquid provided by the present invention, is colourless transparent liquid, is mixed to form the colloidal electrolyte needed for storage battery with electrolyte sulfuric acid, after perfusion, prepare solid accumulator.
Employing particle diameter is 1.5 ~ 10nm, the nano silicon oxide powder of its specific area >=1100 ㎡/g, has not only ensured its easily disperse but also has had containing amount and the surface activity of its superelevation specific surface; By adding dispersant, slurry viscosity obviously reduces, and between particle, agglomeration obviously improves;
For the stability making dispersion liquid keep higher, the isoelectric point of nano silicon oxide is positioned near pH=2, and near pH=10, the Zeta potential of particle has maximum value, higher as guidance to control its Zeta potential absolute value, controls pH value 9 ~ 12; Disperse a difficult problem when solving nano silicon oxide application, fully retain the nano-meter characteristic of its high activity, high-ratio surface simultaneously;
Get the present invention and import Japan soup shallow glue, Sweden Aksu. Asia dragon 1000 glue of Nobel company, sub-imperial 2000 glue, mix with the sulfuric acid of 1.36g/ml simultaneously, test its gelling performance, as shown in table 1:
Table 1 colloidal property and the contrast of gel outward appearance
As shown in Table 1:
(1) colloid that under the condition of identical glue consumption, the present invention and sulfuric acid are mixed to form is for block, and the colloid starchiness that other colloids and sulfuric acid are mixed to form, although its silica content is 2 ~ 3 times of the present invention, its intensity but only has of the present invention 1/2 ~ 1/3, rear the present invention's substantially anhydrousization phenomenon placed by gel, and other products all occur stratification state.
(2) for reaching the gel state of same colloid, consumption of the present invention is only 1/2 ~ 1/3 of other colloids, and silica content is only 1/3 ~ 1/5 of other import glue.
The present invention is as shown in table 2 in tank formation and the characteristic being internalized into gel time and sour temperature under sour proportion condition, measure with glue (nano silicon oxide composite dispersion liquid):
Table 2
As shown in Table 2:
(1) nano silicon oxide composite dispersion liquid consumption is at 4% (silica content 0.4%), time can form all solid state colloid storage battery;
(2) when sour proportion is higher, gel time is faster;
(3) the lower gel time of acid adding temperature is longer, and as adopted cold sour temperature often to decline 10 DEG C, gel time can extend about one times;
(4) under same sour proportion condition, nano silicon oxide composite dispersion liquid consumption is larger, and gel time is faster;
The rear different colloidal electrolyte proportion of glue temperature, different nano silicon oxide composite dispersion liquid consumption and mixing is added according to difference, gel strength time diagram can be obtained, the control of gel time can according to acid adding temperature, acid adding amount and acid adding mode, add glue (nano silicon oxide composite dispersion liquid) amount and control.
Due to the present invention mix with sulfuric acid after before non-gel, viscosity still like water, strictly should control to operate the gel-filling technology time, before colloidal gel, be filled in storage battery, be allowed to condition at storage battery inner gel.
When embody rule is of the present invention, should according to each producer different battery separator, different chemical synthesis technology, that difference adds glue mode is different with to the requirement of colloid battery, with reference to gel strength time diagram of the present invention (gel strength contrasts with dioxide-containing silica), determine nano silicon oxide composite dispersion liquid usage percentage.
The setting of gel-filling technology can refer to gel strength time diagram of the present invention, determines to add glue mode according to gel time.For the colloid formula of gel time below 40 minutes, must namely mix namely with adding glue online; For the colloid formula of gel time more than 40 minutes, the scheme of the acid metering of transformation large metering glue and hybrid system on original equipment can be adopted, by the good colloidal electrolyte of design glue acid proportions on improved glue injection equipment; Note gel time before test or production, single preparation colloid mixture total amount answers conservative control, must ensure that before formation gel, add glue completes.
Silicon oxide particle in the present invention is evenly dispersed the size to primary particle, and the viscosity of dispersion liquid, close to the viscosity of water, because the small particle diameter of its uniqueness, single dispersing are conducive to the uniformity of the network configuration of gel, makes the colloid of formation have the transparency; The specific area of its superelevation, make colloid lock acid, carry sour ability by force, be conducive to the stability of gel colloidal network configuration, gel hydration phenomena reduces, and few consumption, can reach stronger gel strength; Completely solve the stability of inlet gas phase oxidation silicon, a dispersed difficult problem technically; When overcoming the perfusion of traditional colloid, by the forced filtration of pole plate, dividing plate, colloid is separated with electrolyte seriously, and colloid is mainly collected at cluster top and side, only has trace to enter the problem of cluster internal.
Compared with similar products at home and abroad, the nano silicon oxide that nano silicon oxide composite dispersion liquid of the present invention uses has that particle diameter is little, even particle size distribution (being less than 10 nanometers), specific surface large (being up to 1100 ㎡/g), surface activity are strong, purity high (more than 99.8%), stably dispersing;
The invention solves existing use domestic and international colloidal electrolyte product and add the problem that glue is difficult and plastic state is undesirable, effectively promote and improve traditional storage battery product quality, develop the premium quality product that can substitute import completely.The nano-colloid electrolyte of preparation has the advantages such as activity is high, year sour ability is strong, colloid-stabilised, gel time is long, viscosity is low, thixotropy is excellent, adds glue easy to operate, is easily formed with the stable tridimensional network of many porous nanos silica.The new forms of energy storage battery utilizing it filling comparatively common lead acid accumulator has use safety, and capacity is large, and the life-span is long, fluid loss and self discharge speed less; Anacidity mist gas evolution, without electrolyte spilling, lamination; The floating current that discharge and recharge receiving ability is strong and less, less heat; The particular advantages such as suitable environment is wide.It is completely coated that its addition is only that 1/3 ~ 1/5 of aerosil can realize fluid sulphuric acid electrolyte, no liquid seepage and splashing.
Accompanying drawing explanation
Fig. 1 is the process flow diagram of the embodiment of the present invention;
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in more detail.
Nano silicon oxide powder in following each embodiment, derive from Jiangxi and receive space nanometer new material Co., Ltd, particle diameter is 5 ~ 10nm, its specific area 1128 ㎡/g;
Embodiment 1, nano silicon oxide composite diffusion liquid and preparation method thereof, as shown in Figure 1, order comprises and adds dispersant step, plus nano silica step, adjustment pH value step and add bulking agent step:
(1) add dispersant step: add deionized water in a kettle., then add the dispersant of mass percent 6%, the stabilizer of 0.1% that account for nano silicon oxide powder, at 20 DEG C of temperature, stir 15 minutes; Described dispersant is polycarboxylate sodium; Described stabilizer is CMC;
(2) plus nano silica step: in the liquid that step (1) obtains, add nano silicon oxide powder, nano silicon oxide powder accounts for the mass percent 5% of nano silicon oxide composite dispersion liquid, at 20 DEG C, stirs 10 minutes; Described nano silicon oxide powder particle size is 5 ~ 10nm, its specific area 1128 ㎡/g;
(3) pH value step is adjusted: in the liquid that step (2) obtains, add alkali lye, at 20 DEG C of temperature, stir 120 minutes, pH value is adjusted to 9; Described alkali lye is NaOH;
(4) bulking agent step is added: in the liquid that step (3) obtains, add mass percent 0.05% lithium hydroxide and 0.05% stannous sulfate, two kinds of bulking agents that account for nano silicon oxide powder, at 20 DEG C of temperature, stir 30 minutes, obtain nano silicon oxide composite dispersion liquid, described bulking agent is lithium hydroxide, stannous sulfate.
The nano silicon oxide composite dispersion liquid obtained is colourless transparent liquid, and pH value is the proportion at 9,25 DEG C is 1.075g/cm
3, the viscosity at 25 DEG C is 1.71mPaS.
Embodiment 2, nano silicon oxide composite diffusion liquid and preparation method thereof, order comprises and adds dispersant step, plus nano silica step, adjustment pH value step and add bulking agent step:
(1) add dispersant step: add deionized water in a kettle., then add the dispersant of mass percent 0.5%, the stabilizer of 5% that account for nano silicon oxide powder, at 35 DEG C, stir 15 minutes; Described dispersant is alkyl polyoxyethylene ether (paregal O); Described stabilizer is polyvinyl alcohol;
(2) plus nano silica step: in the liquid that step (1) obtains, add nano silicon oxide powder, nano silicon oxide powder accounts for the mass percent 8% of nano silicon oxide composite dispersion liquid, at 50 DEG C of temperature, stirs 5 minutes; Described nano silicon oxide powder particle size is 5 ~ 10nm, its specific area 1100 ㎡/g;
(3) pH value step is adjusted: in the liquid that step (2) obtains, add alkali lye, at 40 DEG C of temperature, stir 90 minutes, pH value is adjusted to 10.5; Described alkali lye is potassium hydroxide;
(4) bulking agent step is added: in the liquid that step (3) obtains, add the bulking agent of the mass percent 5% accounting for nano silicon oxide powder, at 45 DEG C of temperature, stir 25 minutes, obtain nano silicon oxide composite dispersion liquid, described bulking agent is lithium hydroxide.
What obtained is colourless transparent liquid, and pH value is the proportion at 10.5,25 DEG C is 1.122g/cm
3, the viscosity at 25 DEG C is 1.76mPaS.
Embodiment 3, nano silicon oxide composite diffusion liquid and preparation method thereof, order comprises and adds dispersant step, plus nano silica step, adjustment pH value step and add bulking agent step:
(1) add dispersant step: add deionized water in a kettle., then add the dispersant of mass percent 3%, the stabilizer of 2% that account for nano silicon oxide powder, at 50 DEG C of temperature, stir 10 minutes; Described dispersant is glycerine; Described stabilizer is hydroxyethylcellulose;
(2) plus nano silica step: in the liquid that step (1) obtains, add nano silicon oxide powder, nano silicon oxide powder accounts for the mass percent 11% of nano silicon oxide composite dispersion liquid, at 40 DEG C of temperature, stirs 8 minutes; In described nano silicon oxide powder, nano silicon oxide particle diameter is 5 ~ 10nm, its specific area 1160 ㎡/g;
(3) pH value step is adjusted: in the liquid that step (2) obtains, add alkali lye, at 50 DEG C of temperature, stir 30 minutes, pH value is adjusted to 12; Described alkali lye is lithium hydroxide;
(4) bulking agent step is added: in the liquid that step (3) obtains, add the phosphoric acid of the mass percent 3% accounting for nano silicon oxide powder and Nano carbon two kinds of bulking agents of mass percent 0.1%, at 50 DEG C of temperature, stir 15 minutes, obtain nano silicon oxide composite dispersion liquid, described bulking agent is phosphoric acid and Nano carbon.
Claims (2)
1. a preparation method for nano silicon oxide composite dispersion liquid, order comprises and adds dispersant step, plus nano silica step, adjustment pH value step and add bulking agent step, it is characterized in that:
(1) add dispersant step: add deionized water in a kettle., then add the dispersant of mass percent 0.5% ~ 6%, the stabilizer of 0.1% ~ 5% that account for nano silicon oxide powder, at 20 DEG C ~ 50 DEG C temperature, stir 10 minutes ~ 15 minutes;
(2) plus nano silica step: in the liquid that step (1) obtains, add nano silicon oxide powder, nano silicon oxide powder accounts for the mass percent 5% ~ 11% of nano silicon oxide composite dispersion liquid, at 20 DEG C ~ 50 DEG C temperature, stirs 5 minutes ~ 10 minutes; Described nano silicon oxide powder particle size is 5 ~ 10nm, its specific area >=1100 ㎡/g;
(3) pH value step is adjusted: in the liquid that step (2) obtains, add alkali lye, at 20 DEG C ~ 50 DEG C temperature, stir 30 minutes ~ 120 minutes, pH value is adjusted to 9 ~ 12;
(4) bulking agent step is added: in the liquid that step (3) obtains, add the bulking agent of the mass percent 0.1% ~ 5% accounting for nano silicon oxide powder, at 20 DEG C ~ 50 DEG C temperature, stir 15 minutes ~ 30 minutes, obtain nano silicon oxide composite dispersion liquid, described nano silicon oxide composite dispersion liquid is colourless transparent liquid, and pH value is the proportion at 9 ~ 12,25 DEG C is 1.07 ~ 1.13g/cm
3, the viscosity at 25 DEG C is 1.71 ~ 1.78mPaS.
2. preparation method as claimed in claim 1, is characterized in that:
In described step (1), described dispersant is polycarboxylate sodium, alkyl polyoxyethylene ether, AEO, polyethylene glycol or glycerine; Described stabilizer is dextrin, CMC, hydroxyethylcellulose or polyvinyl alcohol;
In described step (3), described alkali lye is NaOH, potassium hydroxide, lithium hydroxide or ammoniacal liquor;
In described step (4), described bulking agent is one or more in ammoniacal liquor, phosphoric acid, lithium hydroxide, molybdenum oxide, stannous sulfate, nano-sized carbon.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101894979A (en) * | 2010-07-15 | 2010-11-24 | 山东康洋电源有限公司 | Electrolyte of nano-colloid storage battery |
| CN102903964A (en) * | 2012-10-31 | 2013-01-30 | 秦飞 | Silicon gel electrolyte |
| CN103346357A (en) * | 2013-06-09 | 2013-10-09 | 长兴亿创纳米科技有限公司 | Colloid additive and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101894979A (en) * | 2010-07-15 | 2010-11-24 | 山东康洋电源有限公司 | Electrolyte of nano-colloid storage battery |
| CN102903964A (en) * | 2012-10-31 | 2013-01-30 | 秦飞 | Silicon gel electrolyte |
| CN103346357A (en) * | 2013-06-09 | 2013-10-09 | 长兴亿创纳米科技有限公司 | Colloid additive and preparation method thereof |
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