CN107059064A - The electricity growth powder method processed of lead-acid accumulator special-purpose nanometer lead powder - Google Patents
The electricity growth powder method processed of lead-acid accumulator special-purpose nanometer lead powder Download PDFInfo
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- CN107059064A CN107059064A CN201611119242.8A CN201611119242A CN107059064A CN 107059064 A CN107059064 A CN 107059064A CN 201611119242 A CN201611119242 A CN 201611119242A CN 107059064 A CN107059064 A CN 107059064A
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- lead
- powder
- lead powder
- plate
- negative plate
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C5/00—Electrolytic production, recovery or refining of metal powders or porous metal masses
- C25C5/02—Electrolytic production, recovery or refining of metal powders or porous metal masses from solutions
Abstract
The invention discloses the electricity growth powder method processed of lead-acid accumulator special-purpose nanometer lead powder.The core material of lead-acid accumulator most critical is lead powder, at present, and its main milling method has two kinds：One kind is manufactured with lead powder ball mill, is oxidized while lead button is ground in machine, and another is vapour phase oxidation process, is oxidized while being and the lead liquid of melting is dispelled and nebulized with Jet Stream big Strong.Manufacture lead powder with two methods of the above, equipment is grand and expensive, and power consumption is big, and the particle of especially product is big and uneven, and specific surface area is little, limits the capacity of lead-acid accumulator.The present invention is using pure lead as raw material, cast thicker stereotype and serve as positive plate, negative plate is worked as with Ni8 Cr18 etc stainless sheet steel, it is immersed in simultaneously after being powered in the solution based on sodium hydroxide, fast-growth gone out on negative plate to particle is superfine and uniform lead particulate, thus lead particulate constitutes the lead powder cavernous body of foam state, and the surface of negative plate can be departed from easily, give after collection takes, through the simple powder new technology processed of dealkalize, dehydration, drying for finished product.
Description
Technical field
The present invention relates to the preparation of lead-acid accumulator core material, the powder-making technique of its active material lead powder, with most simple
Electricity growth powder method processed, the new technology of manufacture nanometer lead powder.
Background technology
Lead-acid accumulator is initially invented by French scientist Pulan spy, is inserted in by two panels stereotype in dilute sulfuric acid and is passed to direct current
Electricity, makes positive plate end be oxidized to brown lead oxide for active material, negative plate end is still that the open-circuit voltage between metallic lead, two ends is
2.2V, because the specific surface area of positive and negative pole plate is little, so capacity is little.Descendant is in order that capacity increases, using prior art
Lead grid, and lead powder and water are tuned into paste, the sub- Inner in the space that this lead plaster is coated in into lead grid by drying, drenches acid, chemical conversion (charging)
After a series of formality, positive plate is set to be oxidized to the great brown lead oxide cavernous body of specific surface area, negative plate is reduced to compare table
The great lead matter cavernous body of area, making could be practical after the specific surface area increase of two kinds of plate active materials.
Lead powder is the core material of modern lead-acid accumulator, at present, and the main preparation method of the special lead powder of lead-acid accumulator has two
Kind, one kind is manufactured with lead powder ball mill, is oxidized while lead button is ground in machine, and another is vapour phase oxidation process, is
Aoxidized while the lead liquid dissolved is dispelled and nebulized with Jet Stream big Strong, the lead manufactured with two methods of the above
Powder, wherein all containing 60% to 80% lead monoxide, particle is uneven, particle diameter is from 1 micron to 16 microns.
In addition, also chemical synthesis, be with pure magnesium or fine aluminium as reducing agent, it is molten in the HCl containing lead (II) ion
Reacted in liquid, prepare lead monoxide, the temperature for controlling reaction is 90 degree Celsius or so, can obtain spongiform lead powder.
The hydrolysis PbO2 of Pb (CH3.COO) 4 are also used, its particle diameter only has 5 rans, and fractions distribution is also equal
Uniform, unfortunate cost is too high.
On network inquire about, in 2012, have " preparation method of lead-acid battery PbO nano-powder, patent information,
Its author Yang Chunxiao, publishes source CN2012, it is as follows that the present takes passages its summary：
The invention discloses a kind of preparation method of lead-acid battery PbO nano-powder, its step for summary；
(1) raw material containing lead is reacted with reactant A, generates water miscible primary product 1；
(2) primary product 1 is reacted with reactant B, and generation primary product 2 is precipitated；
(3) primary product 2 is decomposed, obtains PbO nano-powder；
Applicants contemplate that, three Ma step powder of foregoing invention belong to chemical legal system powder, if according to said method implementing,
The actual production cycle is long, and cost is quite high, and technique is also complicated, and Jia Ge Ang are expensive, it is difficult to be used by lead-acid accumulator manufactory.
The similar patents of invention of Ling mono- Ma are taken passages on network again, its is entitled：A kind of " system of nano spherical lead powder
Preparation Method ", now takes passages its main contents under：
January 8 2014 patent No. CN201410008034.5 applying date
Open open (bulletin) number CN103752844A on April 30 2014 (bulletin) day
Applicant (patentee)：Luoyang Institute Of Science And Technology intelligent Qu Yang of invention (design) people Wang Xuemeng Jia Xiao
Page with sovereign right；A kind of preparation method of nano spherical lead powder, it is characterised in that comprise the following steps；
(1) take the plumbi nitras aqueous solution to add polyvinylpyrrolidone, obtain middle interstitial fluid A, it is standby；
(2) hydration callosity solution is instilled into step (1) intermediate solution A, after being added dropwise to complete, through filtering and washing, is obtained
Spherical lead powder particle.
The lead powder preparation method of the present invention, technique is simple, and lead powder purity height is made, and particle mean size is in 10nm, maximum
Granularity is no more than 100nm, and the lead powder both can be applied to traditional lead acid batteries industry, to prepare the work on polar plate of lead acid storage battery
The industrial chemicals that property material can be made, applied to Powder Metallurgy Industry, or as metallurgical addition agent, to fire wear part.
A variety of lead powder preparation methods in summary, for lead-acid accumulator industry, " only hearing thunder, lose rainy ", most
Main reasons is that the problems such as batch production and the too high expense of cost, so major producers still use ball-milling method at present, also having
Lead powder, its price per kilogram only more than ten yuan of RMB are produced with vapour phase oxidation process.
Inner is invented to hold
Electricity consumption of the present invention grows powder legal system processed and makes a nanometer lead powder, it is characterized in that；Only need at normal temperatures, to set with simplest
Standby, most easy technique, cheapest raw material, the power consumption most saved, the most short production cycle, production when noiseless, to ring
Border and pollution-free, the cheap nanometer lead powder with regard to that can produce, the pole plate to manufacture lead-acid accumulator.
The especially particle diameter of this lead powder is below 0.02 microns, 0.1 micron, and it is with lead powder ball mill (Shimadzu
Method) and the lead powder (about 1 micron to 16 microns of its particle diameter) produced of vapour phase oxidation process (Ba Dunfa) compare, its particle is straight
There was only their 1/tens in footpath.Namely under equal weight, its specific surface area is more several ten times larger than their increasings, if using this
Lead powder manufactures the pole plate of lead-acid accumulator, and its capacity increase several times are affirmatives, so the prospect with popularization.
Based on described above, though the technology of the present invention content it is low and produce effects it is high, every household can small-scale production it is this
Lead powder, especially lead powder particle diameter are less than 0.1 micron, and uniformly, specific surface area greatly, can improve the appearance of lead-acid accumulator
Amount.
The present invention is that, from achievement derived from electroplating technology, in lead plating technology, there is fluorborate solution lead plating, tartaric acid
The multiple technologies such as salting liquid lead plating, silicate fluoride solution casting lead.Related to the present invention is tartrate solution lead plating technology, its
The formula of " tartrate solution " is；180 grams to 200 grams of sodium potassium tartrate tetrahydrate (KNaC4H4O6.4H2O) is dissolved in 1 liters of water,
90 grams of 60 grams to 80 grams of sodium hydroxide (NaOH), lead monoxide (PbO) or lead hydroxide (Pb (OH) 2) is to 120 grams, with this winestone
Acid salt solution is " seed ", and the consumption of " seed " seldom, only accounts for the 0.05% to 0.15% of electrolyte cumulative volume, hereinafter referred to as wine
Stone acid solution lead plating liquid is " seed ".
The present invention is different with technologies such as fluorborate solution lead plating, tartrate solution lead plating and fluorine silicon salting liquid casting lead,
Three of the above, the lead plating technology of first two, positive plate must be pure lead, and the third casting lead technology is the refining of lead, its positive pole
Plate is to use lead bullion, and just pure lead is gone out in its cathode deposition after electrolysis, and the first two is planted lead plating technology and casts lead technology with latter, is all just
The overall lead of pole is transferred to negative pole after electrolysis, is still overall lead, is to be combined unseparated entirety with negative plate, without
It is loose pulvis.
The present invention is by the overall lead of positive plate, after being immersed in the solution based on sodium hydroxide by electric current, in negative plate
Superficial growth go out about 20 nanometers of particle diameter (conservative numeral), not more than 100 nanometers of loose pulvis, thus pulvis
The lead powder cavernous body of composition, Cheng Pao Droplets states, the surface of negative plate can be departed from easily, and " when a melon is ripe it falls off its stem " gives collection and taken.
The present invention it is different from tartaric acid solution lead plating technology, tartrate solution lead plating be plated in negative plate it is overall
Lead, and the present invention is the growth nanometer lead powder on negative plate, and the present invention is participated in three kinds of main matters of electrochemical reaction below
It is described below：
(1) pure lead is the raw material of positive plate of the present invention, and it is corroded after being powered in the solution based on sodium hydroxide, and
The metallic lead that powder state is grown on negative plate is stopped on negative plate, and therefore, positive plate is corroded and constantly reduced weight.
(2) it with the Ni8 Cr18 of thick about 0.5 millimeter etc stainless steel plate is conductor that, negative plate, which is, as assembly
" hotel " of nanometer lead powder is the permanent utensil for using, never going bad.When nanometer lead powder arrives " when a melon is ripe it falls off its stem " after growing herein, into
The lead powder cavernous body of Wei Pao Droplets states, some surface for departing from negative plate is fallen and part is floated in liquid, why can
Float on above the liquid than weighing about less than 1.05 or soBecause Zhe Ma lead powder cavernous bodies have been saturated with the hydrogen of association.
(3), the solution based on sodium hydroxide, is that 50 kilograms or so of water is dissolved in industrial 2 kilograms of sodium hydroxide
In, using the solution of this ratio as mother liquor, 0.05% to 0.15% or so " seed " of mother liquor volume is added, after stirring
Into.
More than (one), (two), (three) be all to turn into a unit in the container for be present in plastics, the size of container, with many
Shao Ma units, can be determined, the size of polar plate area by production-scale size, with the size of comprehensive container used.
In process of production, over time, because the carbon dioxide transitions in sodium hydroxide absorption air are sodium carbonate, make
The Han Liang Minus of sodium hydroxide are few in solution, and positive plate occurs as soon as the titanium dioxide for being changed into light/dark balance after the lead monoxide of yellow again
Lead, can add a little calcium hydroxides, sodium carbonate therein is changed into sodium hydroxide, such as equation Na2CO3+Ca (OH) 2 ---
Shown in 2NaOH+CaCO3, produced water insoluble CaCO3 will precipitate, and can still keep the original of sodium hydroxide in solution
Concentration.
The lead powder grown on the surface of negative plate, is not to be tightened together as welding with negative plate, uses hairbrush
One brush, that is, depart from negative plate and float on liquid level, and has part to avale, and the lead matter cavernous body fast growth grown in negative pole leads to
The lead matter cavernous body collection of generation can be taken within normal 3 hours or so, not so , Zhe Ma lead matter cavernous body continues to creep to positive plate direction,
Contacted with positive plate and short-circuit, so to give foot Enough space, have the lead matter cavernous body for growing Pao Droplets states and stay in it
Ground, the vertically opposite distance of positive and negative pole plate is 150 millimeters to 300 millimeters, can be adjusted by the scale of production.
Positive plate is worked as with pure stereotype, Ni8 Cr18 stainless sheet steels work as negative plate, vertically opposite while being inserted in sodium hydroxide
Based on solution in, pass to direct current, then positive plate is corroded, the superfine lead powder cavernous body of particle grown on negative plate,
3 hours or so the rear conceited polar board surfaces of a , Zhe Ma lead powder cavernous body part that are powered depart from, and are suspended in above electrolyte, and have one
Part sinks, and various method collection can be taken to take, then rinsed with water, removes the sodium hydroxide that includes, after dehydration, drying into
For linen nanometer lead powder.Contain a small amount of lead hydroxide in lead powder, it can also serve as active material, this is with an oxidation
Lead, lead orthoplumbate and metal lead powder are the same, can be still oxidized to after chemical conversion (charging) from positive plate spongy
The brown lead oxide of state, is reduced to the metallic lead of spongy state from negative plate.
Electricity growth can be carried out at normal temperatures, and required current density presses the areal calculation of negative plate, and every 1 square decimeter is
0.7A to 1A, the byproduct of electricity growth nanometer lead powder also has hydrogen, in electric growth course, in negative plate except folding a nanometer lead
Powder sponge is external, also has the hydrogen not absorbed by lead powder cavernous body to escape, if production lead powder is large-scale, this hydrogen is just
There is collection to take the economic value utilized, can adopt various measures, hydrogen is given into collection takes manufacture hydrogen, is used as the fuel of cleaning.
Embodiment
Embodiment (1), the scale that electricity consumption growth method prepares nanometer lead powder is changeable, and the present embodiment is applicant to test
Micro- shape dress that the mode of room produces a small amount of nanometer lead powder is put, and the daily output only has several kilograms of wet-millings, can be entered according to Yi Xia a few Ma steps
OK.
(a) Yong Liu Ma rectangular plastics containers are used as Unit six, 350 millimeters of container Inner walls length, wealthy 250 millimeters, high 200 milli
Rice, the area of positive and negative pole plate multiplies 120 millimeters for 300 millimeters, (i.e. 3.6 square decimeters), and positive plate is 2 millimeters to 3 millimeters thicks
Pure stereotype, negative plate is the Ni8 Cr18 stainless steel plates of 0.5 millimeters thick, and two-plate is vertically opposite to be immersed in based on sodium hydroxide
In solution.
(2) it is dissolved in 20 ratios risen in 25 liters of water with 1 kilogram of sodium hydroxide and is made into sodium hydroxide solution, adds and " plant
Son " (tartrate lead plating liquid), the volume of seed is the 0.05% to 0.15% of Qing Yangization Na liquor capacities, it is agitated after just
Can.
The formula of " seed " (tartrate lead plating liquid) is：0.5 liter of water, plus 50 grams of lead monoxide or lead hydroxide, hydrogen-oxygen
Change 50 grams of sodium, 100 grams of sodium potassium tartrate tetrahydrate.Preparation method is；First the lead monoxide or lead hydroxide fine powder that weigh up quantity are added water in right amount,
It is degree that pulpous state is tuned into after stirring, then the sodium hydroxide and sodium potassium tartrate tetrahydrate that weigh up quantity are mixed, in the water for pouring into 0.5 liter, and
Stirring solution is generated heat, after generating heat, pour into the lead monoxide or lead hydroxide of pulpous state and stir while hot, make lead monoxide or
Lead hydroxide is dissolved, and transparent " tartrate lead plating liquid " is turned into after filtering.
(3) 6 Ma units are connected, the dc source for connecting 12V is powered, and electric current is 3A, and 3 Ma are after many hours, in negative plate
Surface on, grow the block cavernous body that Pao Droplets states are made up of nanometer lead powder of black, collection is rinsed after taking with water circulation, is removed
Remnants sodium hydroxide is removed, as caking shape lead powder cavernous body, after being dried under sunshine, as linen nanometer lead powder.
(4) the present embodiment is laboratory work powder, when powder output current processed is 3A, and power consumption 80W was made with 8 hours daily
Powder, can produce 3 kilograms of wet-millings, and power consumption only 0.64KWh, the not electricity consumption including drying, electricity consumption is saved.
(5) points for attention；Pao Droplets states are constituted by nanometer lead powder by (three) Suo Shu, grow black on negative plate
Cavernous body quantity increase to it is quite big after, the Bluish white threadiness of lead metal gloss can be grown, this is to send that " melon is
Ripe, the base of a fruit will fall " yellow signal that can harvest, it should cut off the electricity supply, nanometer lead powder cavernous body is given into collection takes.
One continuous line production of embodiment (2) factory daily output in terms of ton.It is real powder method Jing Zhong processed can be grown by electricity of the invention
Apply.
Figure of description 1, is a kind of circuit diagram of compact simplified just Zhi formulas 3A constant current rectifier power sources, can export 3V to 250V
DC voltage, can automatic lifting, can directly be connected on Unit 6 (DC12V), Unit 12, Unit 24 or Unit 48 and use,
Output current is all 3A, specializes in preparation small amount nanometer lead powder and is used, the electrotechnics personnel for having more than 4 grades can use.
Description of reference numerals：Q is regular tap, and C1 is 150 microfarads/AC500V capacitors, and C2 is 100 microfarads/DC450V electric capacity
Device, U is 20A bridge-type silicon rectifier stacks, and R is 5K resistance, and DCPA is 50A DC ammeters, and DCPV is 0 to 300V DC voltmeter.
Claims (3)
1. the present invention is the electricity growth powder method processed of lead-acid accumulator special-purpose nanometer lead powder, make positive plate using pure lead as raw material, in hydrogen
It is powered in solution based on sodium oxide molybdena, the new technology of lead powder of the particle diameter less than 1 micron is grown on negative plate, is referred to as received
The electricity growth powder method processed of rice lead powder.
2. the electricity growth powder method processed of the nanometer lead powder as described in claim 1, it is characterized in that：Put into by raw material of pure stereotype, casting
Work as positive plate into tabular, its thickness is from 5 millimeters to 10 millimeters or thicker, its area is true according to the scale of plant produced
The size of fixed plate area.
Negative plate is a nanometer lead powder " hotel ", and nanometer lead powder collects after growing herein to be taken, and is with thick about 0.5 millimeter
Ni8Cr18 stainless sheet steels are optimal, can also use copper coin, iron plate or nickel plating, the iron plate of chromium plating, but poor-performing, its area
It is identical or smaller with positive plate.
3. the electricity growth powder method processed of the nanometer lead powder as described in claim 1, it is characterized in that：Described positive plate is with negative plate
It is vertically opposite to be powered while being immersed in the aqueous solution based on sodium hydroxide, the lead powder sponge of Pao Droplets states is grown on negative plate
0.05% to 0.15% " the tartrate lead plating liquid " containing its cumulative volume in body, sodium hydroxide solution.
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