Separation of materials from processed electrochemical cells and batteries

FIELD: process engineering.

SUBSTANCE: invention relates to processing of electrochemical cells and storage batteries. Proposed method comprises mincing of storage battery, removal of case materials, suspending of produced battery suspension in water in foam flotation tank. Foam flotation agent is added to said suspension to bubble said tank by air to produce foam. This allows hydrophobic materials to be trapped by air bubbles and trapped materials to afloat with said trapped materials. Compounds Pb (IV) are separated from compounds Pb (II) in battery suspension in foam flotation tank. Method of separation of materials in wastes of lead-acid batteries comprises extraction of pasted from used battery, suspending of extracted paste in water, addition of foam flotation agent to said suspension including paste and water, bubbling of said tank by gas to get the foam, separation of (PbO2) from other lead-bearing compounds of suspension is said tank.

EFFECT: higher efficiency of separation.

14 cl, 6 tbl, 10 ex

 

The LEVEL of TECHNOLOGY

Processing of electrochemical cells and batteries are important from the point of view of economy and environmental protection. Currently more than 98% of lead-acid batteries are recycled. Recycling of rechargeable and non-rechargeable consumer items, such as button batteries and batteries size D, C, AA and AAA, which have the advantage of Li-ion, Zn-carbon and zinc-alkali chemical nature, is also desirable.

Currently, the processing is performed mainly by using pyrometallurgical processing. Pyrometallurgical methods are not optimal from the point of view of the environment, as they cause emissions of carbon dioxide and generate waste, such as slag and cinders. These methods of waste processing are also expensive due to the high energy intensity of pyrometallurgy.

In modern practice, recycling of used batteries and cells are first directed to the operation of crushing or grinding, where they are subjected to mechanical fragmentation. The polymeric materials used in the body of the cell is removed from the crushed batteries using the sink/float, in which plastics low density emerge from other materials due to differences in density. In the case of lead-acid batteries this paste is then� processed in pyrometallurgical operations, where the material is heated to >1000°C in a chemically reducing atmosphere. In this activity, connection lead-based (i.e. PbSO4, PbO2, PbO) chemically restored to metallic lead, which is removed for further metallurgical processing. This is a very energy-intensive processes, especially in light of the fact that most of the lead produced in this operation, re-converted into lead oxides for use in the manufacture of new lead-acid batteries.

Carbon is found in many batteries as electrochemically active material, for example, as the anode in Li-ion cell or as a modifier to improve the conductivity of the electrochemically active material or to add a capacitive element in the battery to improve the charge/discharge. When used pyrometallurgical processing technology, this carbon can cause additional emissions of carbon dioxide and difficulty in maintaining appropriate relations WITH2/CO for efficient melting. Conventional methods of pyro - and hydrometallurgical processing of these cells also often make this inactive carbon, making it unfit for reuse in making new batteries.

During the recycling process the presence of carbon may also Ogre�acivate the efficiency of the separation process, driven through leaching, electrostatics and density. It was discovered during processing and lead-acid and lead-acid batteries, e.g. Li-Yonah, Nickel-metal hydride batteries and zinc. In particular, in the case of leaching, when chemically active solutions used for extraction and separation of metal particles, carbon can form colloidal suspensions, which remove the leaching agent from the process. The carbon may be contaminated by reagents used in hydrometallurgical operations, complicating its elimination from the point of view of the environment. Therefore, the removal of carbon to recycling batteries is favorable.

Although froth flotation has been used in other fields, its application in the field of recycling of batteries and electrochemical cells is absent. Now discovered that by using the technology of froth flotation for the separation of certain compounds during processing and the batteries can be avoided phase thermochemical recovery used in modern refining methods. When apply the methods of froth flotation, the cost of the resulting recycled material suitable for reuse in the creation of new electrochemical cells based on lead, can be reduced with respect pirone�allergiesa ways. Using the technology of froth flotation in the processing also causes a reduced impact on the environment compared to pyrometallurgical technologies of the prior art, because unwanted emissions are reduced or eliminated. When the carbon is removed by froth flotation, it is possible to avoid disadvantages associated with carbon. In particular, carbon, separated using froth flotation, can be directly used in the manufacture of batteries. Similarly, other materials batteries, separated using froth flotation, also are of a quality suitable for direct use in the manufacture of batteries.

Summary of the INVENTION

Froth flotation is used during the recycling of batteries for the separation of materials. Lead compounds present in lead-acid batteries, can be retrieved using froth flotation. Carbon materials in batteries can also be separated from materials of batteries by froth flotation.

In the practical execution of this invention, the battery may be subjected to the usual operations of fragmentation or grinding. The materials remaining after the operation, and then subjected to froth flotation process. The process of froth flotation involves the management of hydrophilic and hydrophobic parameters of shared materials. To�Yes processed materials purged, hydrophobic materials adhere to air bubbles and float to the surface where they can be removed. Hydrophilic materials remain in solution or fall off.

In particular, the present invention provides an improved method for the separation of materials during the recycling of batteries containing (a) crushing of batteries, (b) the deletion of materials used, (C) suspending the resulting suspension battery in water in a tank, (d) adding a froth flotation agent to the suspension, (e) purging the tank of air with the formation of the foam, resulting in hydrophobic materials are trapped air bubbles, and (f) enabling data captured content to float up in the tank and the captured floating materials from the tank.

DETAILED DESCRIPTION

According to the present invention froth flotation is used to separate certain materials used in batteries and electrochemical cells. It should be understood that as used in this application references to batteries include all types of batteries and electrochemical cells. Technologies included in the methods of the present invention, can be used instead of pyrometallurgical technologies of the prior art, which are less desirable from the point of view of the environment for hundred�bridges, energy consumption and emissions.

As mentioned above, in modern practice, recycling of used batteries and cells are first sent to the operation fragmentation, where they are subjected to mechanical grinding. The polymeric materials used in the buildings of the elements is removed from the crushed batteries using the sink/float, in which plastics low density emerge from other materials due to the difference density. In the practice of the present invention, this process of pre-grinding and removal can be used. The remaining material is then subjected to separation froth flotation.

Separation froth flotation perform by controlling the hydrophilic/hydrophobic properties of surfaces share materials. Hydrophilic surface will tend to unite with water, whereas the hydrophobic surface will connect with non-aqueous phase, for example, air or oil. To control the hydrophilicity/hydrophobicity of the surface by applying chemical agents that preferentially binds to the surface of a material. This is usually achieved by creating an aqueous suspension, to which is added the appropriate agents for controlling hydrophilic and hydrophobic properties of the partial products, typically when mixing or paramashiva�AI. For purposes of this application it should be understood that the froth flotation agent is a material that is suitable to control the hydrophobic and/or hydrophilic nature of detachable material. After treatment with these agents, the suspension passes into the tank, barbotirovany air. In that tank, hydrophobic materials mainly stick to air bubbles and float to the surface for removal of relatively hydrophilic materials, which are deposited or remain in the water. Thus, the materials can be separated from each other.

The methods of the present invention is applicable for the separation of any components of the battery, hydrophilic and hydrophobic nature which can be controlled relative to each other. Among the materials present in the recycled materials batteries, suitable for separation by froth flotation, are compounds of lead and carbon. Although froth flotation is not used when the cations in the partial materials are the same, in the practice of the present invention, it was found that froth flotation is particularly suitable for separating compounds of Pb(IV) from compounds of Pb(II). Similarly, it is possible to separate Nickel compounds present in the battery, from each other.

Commercially available cell froth flotation can be used for practical IP�Anenii of this invention. One suitable cell is a cell of Denver D-12. The material is subjected to froth flotation, is placed in this cell, preferably with a foaming agent. Suitable blowing agents include alcohols, pine oil, polyglycols, polyoxypropylene and Xylenol. These reagents stabilize education exciting air bubbles, which cause the separation is based on the modified hydrophobic and hydrophilic nature of shared materials. Reagents known as collectors, can also be added to the cell. Collectors help hydrophobic materials float and/or adhere to air bubbles. Depressants can also be added to the cell. Depressants help hydrophilic materials to settle and/or be captured by the foam.

Reagents that affect the hydrophobic and hydrophilic nature of shared materials include fatty acids (e.g., stearates, oleate), xanthates, dithiophosphates, lignosulfonates, oximes, urea and aminosulfonic. These reagents act by modifying the properties of the partial particles. These reagents are added to the froth flotation cell according to the conventional technology.

Reagents that modify the behavior of the absorption of the above reagents, it is desirable to use to improve the separation of lead compounds. These modifiers vklyuchyeniye (for example, CaO, NaOH, NaCO3), acid (H2SO4, HCl, HNO3), organic compounds (e.g., dextrin, starch, glue), cations (Pb2+, Ba2+Ca2+Cu+, Pb2+, Zn2+, Ag+) and/or anions (SiO32-, RO43-CN-WITH32-, S2-).

Lead-acid batteries are the dominant technology for energy conservation in automotive starter motors, batteries, lighting and ignition, sources of continuous power, electric vehicles, telecommunications and energy from alternative sources. The method of the present invention is particularly applicable to lead-acid batteries. When conventional design cell battery consists of electrically active lead compounds and lead electrical conductors along with the body material, usually a polymer. Table 1 below represents a typical composition used lead-acid batteries.

Table 1
ComponentProportion, %
PbSO450-60
PbO215-35
PbO 5-10
Pb2-5
Other2-4
The entire active material70-90
Pb lattice, pole, top metal5-25
Polymeric housing material5
Total100

These shares may be part of the change in practice because of custom design batteries and profiles of the charge/discharge observed during use in the application.

When using the present invention, the active materials of lead-acid batteries can be recycled for reuse in the manufacture of new lead-acid batteries, avoiding the use of pyrometallurgical operations. In particular, in the manufacturing method of the present invention the technology of froth flotation (rather than pyrometallurgical operation) can be used for separation of Pb(IV) materials such as lead dioxide, Pb(II) materials, such as lead oxide or lead sulfate.

To carry out the separation of lead products according to the method of froth flotation, used lead-acid batteries, or ale�options subjected to the usual operations of crushing, to mechanically grind the battery or power feature. Used conventional techniques for the removal of polymeric materials from fragmented battery or element. This can be performed using normal operation of the sink/float, in which plastics with relatively low density emerge from the materials lead-based higher density.

The resulting paste of lead-containing batteries are subjected to a froth flotation process. Preferably, prior to subjecting the lead paste to the froth flotation process, the paste is sieved to remove unwanted particles that may contaminate the return of lead compounds and/or contain particles with compounds and Pb(IV), and Pb(II). The process of screening, preferentially removes material that has a size greater than 200 microns.

To carry out the separation froth flotation, lead-containing paste is suspended in water, preferably with mixing or stirring. The froth flotation agents are added and mixed, forming what in the art is called "suspension", subjected to froth flotation. You can use any agent that causes partial particles to become hydrophobic and hydrophilic relative to each other so that the hydrophobic detachable material will be captured with aerial�and bubbles through this solution, whereas the hydrophilic material remains in solution and is deposited. In the case of lead particles in an aqueous suspension of hydrophobic materials will attach themselves to air bubbles produced by the froth flotation apparatus, and thereby be separated from the hydrophilic particles during stage froth flotation. Can be used in the froth flotation device type Denver. However, other configurations are also suitable for this purpose. For example, the froth flotation tank can have a cascading organization in the Denver cell, in which detachable material passes with the foam through a series of cascading reservoirs, or may be the only tank that has a height that is effective to cause the flotation through the top only hydrophobic materials. Separation occurs when air bubbles float to the surface of the bath, carrying hydrophobic particles in contrast to hydrophilic particles that remain suspended in a water bath.

Separation may be achieved by modifying the hydrophobic and hydrophilic nature PbO2and PbSO4with the use of froth flotation agents, known as collectors. Suitable collectors include fatty acids (e.g., stearates, oleate), xanthates, dithiophosphates, lignosulfonates, oximes, urea, aminosulfonic. These collectors pieces�Ute as a surface active particles, making possible the separation of the compounds Pb(IV) and Pb(II) in the aquatic environment. This separation can occur with blowing agents, such as alcohols, pine oil, polyglycols, polyoxypropylene and Xylenol, or without them. Additionally, modifiers can cause the absorption of flotation reagents on each of the inorganic phase. Among the modifiers applicable to froth flotation, there are pH modifiers, such as bases (e.g., Cao, NaOH, NaCO3), acid (H2SO4, HCl, HNO3), neutral organic compounds (for example, dextrin, starch, glue), cations (Pb+2, Ba2+Ca2+Cu+, Pb2+, Zn2+, Ag+) and/or anions (SiO32-, RO43-CN-WITH32-, S-). These foaming agents can modify the behavior of the absorption above flotation agents.

Froth flotation can also be used to remove carbon from different materials, as it is hydrophobic in nature. However, when carbon is used in batteries, changing the chemistry of its surface, preferably the use of surface-active chemical agents to improve the floatability of carbon and to produce a product suitable for reuse when creating panels. This method of separating the carbon by froth flotation can be improved by the removal of the organic binder, associated with the manufacture of the electrode.

The method of this invention is also applicable for recycling of lithium batteries. The Sloop patent for "System and method for removing an electrolyte from an energy storage and/or conversion device using a supercritical fluid," US 7198865 describes the use of supercritical CO2to remove the electrolyte from used Li-ion and other elements. The Association of this method with vacuum degassing and/or by extraction with suitable solvents to remove sticky organic compounds, thereby improving the separation of froth flotation by increasing the degree of difference between hydrophilic and hydrophobic compounds, the components of the electrochemical element.

The following General procedure can be used to implement a split foam flotation material in the batteries.

First, the battery is cut to expose the contents for removal. In the second stage, the battery is subjected to mechanical grinding, such as rotation, shaking, shaking to release the active materials from the buildings, separators and cathode and/or anode conductive grids. At this point, the third operation is to sort material by size, removing floating material, which usually has a <200 microns, with larger residues, consisting again of the buildings, separators and cathode �/or anode grids. This size sorting can be done by wet or dry sieving, the slurry or air sorting. The preferred methodology of the authors is wet screening or elutriation, which prevents fine particles from the air entrainment, which is a problem for the health of personnel and the environment.

The fourth stage is a key technology, which is a froth flotation. Add reagents that are preferentially absorbed by the surface Pb of the compounds present in the paste used lead-acid batteries. More specifically, PbO2, PbO and PbSO4that are present in the active material used lead-acid batteries. It was shown that three of modifying the surface of the reagent, i.e. the collector, are effective. This mercaptobenzotriazole office (ILO), its sodium salt (Na-MBT) and dialkyldithiophosphate (sold under the brand Aerophine from Cytec). Preferably, they are added to the mass percentage of 10-3up to 10-1. These compounds enhance the flotation PbO2while PbSO4settles. It was found that the addition of methylisobutylcarbinol (MIBC) increases the stability of the foam, improving the separation. It was also found that in the case of ILO, the use of the depressant of lignosulfonate (648 product derived from Borregard-Lignotech) �silive flotation PbO 2while PbSO4POPs up in his absence. Preferred concentrations shown in table 2 together with the distribution coefficient PbSO4/PbO2.

It is known that carbon has a hydrophobic nature, i.e. it repels water. At the same time, other active materials in the battery are hydrophilic, i.e. attract water, for example, oxides and phosphates of lithium, inorganic compounds of lead, zinc and manganese. When the carbon is separated according to the present invention, the air was bubbled into the tank, which contains 10-40% by volume of solids in the aquatic environment. According to the preference of the authors, 15-20 percent by volume to maintain the fine particles, i.e., <75 microns. To improve separation, the organic phase is added to 0.1 to 5.0 percent by volume. In a preferred practice of 1.0 volume percent of methylisobutylcarbinol (MIBC) or kerosene. It enhances the flotation of carbon by increasing the adhesion of the carbon particles to the rising air bubbles, forming the carbon-enriched phase on the surface of the tank. MILK is preferred, as it is easily removed from the carbon after froth flotation by vacuum degassing at <1 Torr or when heated to 100°C in flowing gas because of its higher vapor pressure than that of kerosene. Carbon returned by e�th way suitable for reuse in making new batteries. To remove residual impurities from carbon, may be used in the washing step in which impurities are removed by dissolution in acidic/basic solutions. This process is preferably followed by drying of the material to a moisture content of <10 percent by weight, and packaging for shipment.

The material that surfaced, which is now cleaned of carbon, can be further processed with the aid of technology, hydrometallurgical, pyrometallurgical or physical cleaning. For example, you can corroding acid Zn and Mn from material that settles in Zn-Mn elements. Etched material is then subjected to solvent extraction and electrolysis of metallic Zn and MnO2. In the case of Li-ion batteries is also possible to remove the oxide Li. When the excavated material hydrothermal treated with LiOH and thermally treated at 800°C in flowing air, remove the material suitable for use in the manufacture of Li-ion rechargeable battery.

This technology is particularly suitable in the processing of modern lead-acid batteries, which contain large amounts of carbon to increase the battery capacity. Although carbon is the key to improve the performance of charge/discharge of these elements, for pererabotav�setup portion of the industry that is the problem, since this excess carbon is in direct conflict with the desire to reduce carbon dioxide emissions from commonly used pyrometallurgical processing operations. In addition, the removal of carbon froth flotation is considered to be an important preliminary step to the use of froth flotation to separate PbO2and PbSO4because the carbon absorbs the reagents used for the separation of these phases, and pollutes the phase that POPs up.

In the case of the chemical nature of all these batteries carbon is expensive, constituting, thus, a significant cost in the manufacture of batteries. The return of this material will allow you to reduce costs in the manufacture of batteries since the return process less expensive than obtaining new material.

EXAMPLES

Example 1 - Separation of Pb(IV) and Pb(II):

Experimental tests of this method and reagents was carried out using a flotation cell type Denver D-12 received from Metso Minerals. 300 grams of sifted material was placed inside the cell Denver and suspended in 3 liters of water with stirring for 5 minutes. The air was barbotirovany into the tank containing 10-40% by volume of solids in the aqueous stream, preferably 15-20% by volume to maintain flotation of fine particles, i.e., <75 μm, and maximum performance. The flotation agents DOB�Lyali and mixed for 5 minutes, ensuring that the art is called the slurry is subjected to froth flotation. All processing was performed at a pH in the range of 4-10, preferably pH=7,0-8,5. Other configurations/designs of flotation cell is also applicable for this purpose, but the type of Denver is normal for the laboratory process.

A paste of lead-acid batteries were obtained from the destructive operations of the battery Quemetco Metals in Indianapolis, Indiana. This paste is a mixed raw material of automotive, industrial, telecommunication and power supply panels and elements.

This material was sieved to a size of <200 microns, using conventional methods. This sifting operation can provide benefits beyond simple sorting by size. For example, to optimize the separation of PbO2from particles on the basis of PbSO4preferably the reduction or elimination of multiphase particles. Screening or fractionation by size makes it. Also for the purpose of hardening in the active material paste as additives are usually present polymeric and/or glass fibers. These additional materials in the paste consume contaminate reagents and products, which must be entered the returned lead. Therefore, the removal of these additives during the refining process strengthens the dignity of the whole method.

Approximately 30 grams of the screened material was placed in a cell type Denver D-12, received from Metso Minerals, and suspended in 3 liters of water under stirring for approximately 5 minutes. At this point, the added reagents and stirred for 5 minutes. The details of the procedure are outlined below.

Experimental procedure

1. Sifting pasta to 200 μm in preparation for flotation:

and. weighed five hundred grams of Pb paste as received,

b. took five hundred milliliters of DI water,

C. paste and water were combined in a standard mixer,

d. the contents were mixed for five minutes to obtain a homogeneous suspension,

E. suspension was poured onto a 200 µm sieve inside a 5-gallon (18.9 l) bucket,

f. the suspension was slowly stirred, allowing the minerals to pass through the sieve, whereas the remaining polymer fiber was late,

g. a small amount of wash water (DI) was periodically added to ensure complete screening,

h. a bucket of sifted paste was left to settle for some period of time (at least overnight)

i. most of the water was decanted.

2. Screening of paste to 100 μm in preparation for flotation:

and. weighed five hundred grams of sieved paste (200 μm),

b. took five hundred milliliters of DI water,

C. paste and water were combined in a standard mixer,

d. the contents were mixed for five minutes, getting odnorodno�th suspension,

E. suspension was poured onto a 100 μm sieve inside a 5-gallon (18.9 l) bucket,

f. the suspension was slowly stirred, allowing smaller minerals to pass through the sieve, while the remaining, larger minerals delayed,

g. a small amount of wash water (DI) was periodically added to ensure complete screening,

h. a bucket of sifted paste was left to settle for some period of time (at least overnight)

i. most of the water was decanted.

3. Sifting pasta to 50 μm in preparation for flotation:

and. weighed five hundred grams of sieved paste (100 μm),

b. took five hundred milliliters of DI water,

C. paste and water were combined in a standard mixer,

d. the contents were mixed for five minutes to obtain a homogeneous suspension,

E. suspension was poured onto a 50 micron filter held over a small plastic bucket,

f. the suspension was slowly stirred with the hand, allowing for fine minerals pass through the filter, whereas the remaining, larger minerals delayed,

g. a small amount of wash water (DI) was periodically added to ensure complete screening,

h. a bucket of sifted paste was left to settle for some period of time (at least overnight)

i. most of the water was decanted.

4 Grinding/grinding paste in the preparation of flotation:

pasta grated and crushed according to normal procedures.

5. The flotation process:

and. installed the flotation cell Denver,

b. weighed three hundred grams of sieved Pb paste (procedure 1),

S. took three liters of DI water and added to the cell Denver,

d. cell Denver included with the valve closed air supply,

E. regulated speed,

f. added lead paste,

g. selected reagents and added to the suspension,

h. the suspension was stirred without air for five minutes,

i. valve, the air supply is opened and allowed the slurry to mix with air within five minutes,

j. the foam is continuously removed from the top of the cell to Denver and placed in the reserve tank for ten minutes,

k. the foam samples were taken after one minute, after five minutes and after ten minutes,

l. the Denver cell was switched off, allowing the main Baku to settle, while the tank was cleaned,

m. the main tank was decanted slowly and took away the sediment sample,

n. all samples collected during this procedure were left to dry in the air.

6. Procedure three-stage flotation:

and. installed the flotation cell Denver,

b. weighed three hundred grams of sieved Pb paste (procedure 1),

S. took three liters of DI water and added to the cell Denver,

d. cell Denver included with the valve closed air supply,

E. regul�grown speed,

f. added lead paste,

g. selected reagents and added to the suspension,

h. the suspension was stirred without air for five minutes,

i. valve, the air supply is opened and allowed the slurry to mix with air within five minutes,

j. the foam is continuously removed within ten minutes and were placed in a small plastic bucket marked "foam 1",

k. the Denver cell was switched off,

l. the main tank was emptied and pour into another small plastic bucket labeled "sample 1",

m. both buckets were left to settle down for the night,

n. the water was decanted slowly in each bucket,

O. small samples were taken from each for consideration,

R. the rest of the contents of two buckets were passed through the procedure 4 again, replacing the place of the expression "three hundred grams of the sieved paste and replacing mark the buckets on "foam 2" and "sample 2", respectively,

q. when stage 4 is completed for "foam 2" and "draft 2", the contents of these buckets were passed through the procedure 4 third time, marking them as "foam 3" and "sample 3",

r. all samples were left to dry in the air.

The effectiveness of a particular combination of reagents was calculated in the form of K, which represents the ratio of interest materials in flotirovanija (hydrophobic) phase to a certain content in the settled (hydrophilic) phase. The value of K is equal to 1, indicates from�OUTSTA separation. The larger the value of K deviates from 1, the more desirable it becomes, as the increase in size To reflect the increased separation for materials. In this experiment, the desired goal was the separation of PbO2from PbSO4. Therefore, To reflect this separation. If K<1, PbO2POPs up. If K>1, POPs up PbSO4. What is the connection of lead POPs up, depends on the chemistry of the reagents used. The value K was determined using the Leco analysis of sulfur and x-ray diffraction analysis.

Table 2 provides the results of several test combinations of collectors, depressants and frothers.

Table 2
Summary of studies on the separation of PbO2and PbSO4
The collectorThe concentration of the collectorA depressantThe concentration of depressantFoamerThe concentration of foaming agentTo
N1.00 E-02MIBK1.00 E-02 0,66
AR1.00 E-02MIBK1.00 E-020,53
MBT1.00 E-026481.00 E-02MIBK1.00 E-020,76
MBT1.00 E-02MIBK1.00 E-021,32

Example 2 - Application of the office:

Performed an experiment with flotation by introducing the office (mercaptobenzothiazole). Also simultaneously used MINT, providing a more stable foam. This experiment was performed using sifted pasta, requiring implementation of procedure 1, and focused on trying to raise the pH of the suspension to determine its significance. More specifically, between steps 5f and 5g flakes NaOH was added to the suspension, adjusting the pH level. Although this attempt to raise the pH to 10 was completely unsuccessful due to the reaction between NaOH and PbSO4the remaining procedure 5 was completed, and the samples were dried and examined. Analysis of the values of "K" showed �this combination is very effective in the opposite direction, flotation PbSO4instead PbO2.

The second experiment with flotation with the introduction of the office were performed using the sifted pasta, requiring implementation of procedure 1. Flotation started by following the procedure 5 with some minor changes. During stage 5j foam was shot in a small plastic bucket instead of a backup tank. The 5k stage was absent during the execution of flotation. Instead, samples were taken from a plastic bucket after a sufficient time for the occurrence of subsidence, approximately during the night. Sample "beveled foam" was a remaining organic layer after sedimentation, whereas the sample "pop-up material" collected from material that donkey from the solution in the bucket with foam. Sample "beveled foam had K=0,66 and sample "pop-up material" had K=0,95.

Example 3 - Use of Aerophine:

Pasta processed as received, bypassing all the procedures 1, 2, 3 and 4 from example 1. For procedure 5 was followed to obtain samples, which are dried and sent for analysis of carbon and sulfur. Division of sulfur in each sample pop-up of material on the relevant contents in the sediment sample gave a value of "K", representing the effectiveness of this particular combination of reagents. The value "K" is less than one meant flotation PbO2. The samples taken on this day, gave K=1,04, 1,1, 0,94.

p> Sifted paste used according to the procedure 1, using a foaming agent MIBK. Reached values of "K" is 0.8 and 0.53. It is believed that the removal of polymer fibers (greater than 200 microns) makes more reagents available for the target materials.

In an additional experiment with aerophine sifted pasta again subjected to the procedure 1 and used the foam MILK. Similar to the above experiment, the NaOH was used between steps 5f and 5g to raise the pH and raise the pH to 8.3. The obtained value of "K" was 0,89.

Example 4 - Using N:

The experiment with the introduction of flotation N performed using a foaming agent MIBK for sustainability. Treatments 1 and 5 were performed with a slight modification. As in the previous experiments, during stage 5j foam was shot in a small plastic bucket instead of a backup tank. The 5k stage was absent during the execution of flotation. Instead, taking samples from a plastic bucket after a sufficient time for the occurrence of subsidence, approximately during the night. The results were the value of "K" to 0.76 for "beveled foam" and 0.79 for "pop-up material".

The second experiment was performed by following the procedures 1 and 5. The combination of reagents was a N with MIBK depressant and 648. This experiment was performed with the same changes to the stages 5j and 5k. Costigliole "K" Of 0.90.

Third flotation experiment was performed in the same day (12/11/08), following the procedures 1 and 5 with the same changes to the stages 5j and 5k. This time used a combination of N and depressant 648, yielding K=0,95.

Example 5 - Use of Aerophine:

Again tested Aerophine, this time in combination with the foaming agent MIBK depressant and 648. Follow procedures 1 and 5 with a small change. As in the previous experiments, during stage 5j foam was shot in a small plastic bucket instead of a backup tank. The 5k stage was absent during the execution of flotation. Instead, taking samples from a plastic bucket after a sufficient time for the occurrence of subsidence, approximately during the night. Although the resulting separation of lead compounds was poor (K=1,25 and 1.04), and the precipitate had a very low content of carbon.

The second flotation experiment with the use of Aerophine with MIBK performed, following the procedures 1 and 5. This experiment was conducted with the same changes to the stages 5j and 5k. The results showed the value of "K" to 0.94.

Third flotation experiment using a combination of Aerophine and depressant 648 performed, following the procedures 1 and 5 with the same changes to the stages 5j and 5k. Received K=0,85.

Example 6 - Use of the office:

Another flotation experiment was performed, using the office on �Roseanne pasta (procedure 1). This time the addition of foaming agent MIBG combined with a depressant 648, lignosulfate. Flotation was performed in the cell Denver, following the procedure 5, and taking samples. The results showed the value of "K" of 0.76, 0.86 and 0.79 in.

In a similar flotation experiment sifted paste (procedure 1) was combined with the office and MIBK. Follow procedure 5, receiving the samples. Data of sulfur analysis gave a value "K" of 1.3, 1.0 and 0,97.

Example 7 - three-stage flotation with N:

Three-stage flotation experiment was performed using a combination N and MIBK. Used sifted pasta according to the procedure 1. Procedure 6 was followed in its entirety, yielding three samples of foam and three samples of sediment. Although it was also given a sample of the foam sediment 1, sediment sample foam 1, foam sample 2 sediment and the sediment sample foam 2, these four samples were considered as intermediate stage and was discarded as unnecessary. The results of the third stage showed a steady, almost linear separation with almost identical values of "K" for all three pop-up content (K=0.787 in first foam, 0,774 second pins, 0.787 in third pins). This means that the separation occurred at approximately the same speed in all three stages.

Example 8 - three-stage flotation with Aerophine:

Three-stage flotation experiment was performed using a combination of Aerophine and M�BC. Used sifted pasta according to the procedure 1. Again followed the procedure of 6, receiving three samples of foam and three samples of sediment. Similarly to the above case has also selected four intermediate sample. The value of "K" for "pen" 1, 2, and 3 were 0,86, 1.03 and 0.98 m, respectively.

Example 9 - Removal of carbon:

The procedure for removal of carbon can be effective when using procedure 1 for sifting and procedures 5 and 6 for flotation.

More specifically, procedures 1 and 2 performed, using a black mass LiMOx, floated with water only (no additives) and with reagents MIBC, kerosene and dodecylphenol. These reagents were chosen because of their known wettability with the carbon. After the completion of the flotation samples were dried and sent for analysis of carbon using a LECO. The measured carbon content of each sample pop-up material was divided by the amount of carbon contained in the sediment, getting the value of "K" that is used to determine separation efficiency. This value was calculated for all results of flotation.

According to the data obtained (table 3) reagent MIBC gives the best separation, although simple flotation in the water close in effectiveness. It was suggested that this efficiency is mainly due to the natural hydrophobicity of carbon. The reagent MIBC only provides a stub�optimum foam which pull carbon.

Table 3
Comparison of flotation reagents black mass LiMOx
SampleCarbon (% wt.)Value To
World Cup, no additives, 10 min60,82,79
World Cup, no additives, sludgeOf 21.8
World Cup, kerosene, 10 min56,02,60
World Cup, kerosene, residueA 21.5
World Cup, MIBK, 10 min70,12,85
World Cup, MILK, precipitate24,6
World Cup, dodecylphenol, 10 min35,51,45
World Cup, dodecylphenol, precipitate24,4

Example 10 - three-stage flotation of carbon:

Performed a three-stage flotation experiment, in which black LiMOx used in conjunction with a foaming agent MIBK. Follow procedures 1 and 3 and samples were prepared, dried and sent for analysis of carbon. The results of this experiment are shown in table 4 and reflect great separation.

Table 4
Testudinea flotation LiMOx + MIBK
SampleWith (% wt.)Cu (% wt.)Fe (% wt.)Carbon (% wt.)Carbon (K-value)
FM + MILK foam29,300,270,0741,041,96
FM + MILK foam CH225,300,270,0753,843,12
FM + MILK foam CH320,700,290,0668,552,97
FM + MILK foam draught35,500,280,0932,06
FM + MILK foam draught draught27,200,300,0847,80
FM + MIBK sediment39,700,360,0720,96
FM + MIBK precipitate B242,000,380,07To 17.23
FM + MIBK residue CH341,100,370,07At 23.08
FM + MIBK sludge foams39,200,260,0628,95
FM + MIBK residue foam foam30,400,250,0546,25

The samples listed above are re-directed to x-ray analysis, and again at the definition�their carbon using a LECO. The data set re-direction (table 5) is very similar to the original except for the sludge of the second stage.

Table 5
SampleCarbon (%wt.)Sulfur (%wt.)Value To
FM + MILK foam41,10no data2,069486
FM + MILK foam CH252,95no data2,355427
FM + MILK foam CH366,39no data2,774342
FM + MIBK sediment19,89no data
FM + MIBK precipitate B222,48no data
FM + MIBK residue CH323,93no data

Eight hundred grams of Zn black mass was sieved according to the procedures�e 1. Flotation of the black mass (smaller than 200 μm) was performed according to procedure 2. Four samples were left to dry in the air for two weeks before making and consideration.

From the results it is clear (table 6) that the separation of carbon between the foam and the precipitate is effective similar to the previous results with the black mass LiMOx.

Table 6
SampleCarbon (% wt.)The value To
Sifted Zn-FMOf 6.022,03
Sifted Zn-FM + MILK foam 1 min8,672,92
Sifted Zn-FM + MILK foam 5 minA 7.872,65
Sifted Zn-FM + MILK foam 10 min7,262,44
Sifted Zn-FM + MIBK sediment2,97

1. The method of separation of materials in scrap batteries, in which:
(a) ground battery,
(b) remove the materials of the shell,
(c) suspend the resulting suspension b�tarei in water in a froth flotation tank;
(d) adding a froth flotation agent to the suspension,
(e) the reservoir was bubbled with air with the formation of the foam, resulting in hydrophobic materials are captured by air bubbles and
f) allow the captured content to float up in the tank and remove the captured material from the reservoir,
at the same compound Pb (IV) is separated from the compounds Pb (II) in suspension battery in the froth flotation tank.

2. A method according to claim 1, wherein the foaming agent is added to the vessel in step d.

3. A method according to claim 1, wherein the collector is added to the vessel in step d.

4. A method according to claim 1, wherein the depressant is added to the vessel in step d.

5. A method according to claim 1, where the froth flotation agent selected from the group consisting of mercaptobenzothiazole, mercaptobenzothiazole sodium and dialkyldithiophosphate.

6. A method according to claim 1 where the slurry of the battery contains carbon.

7. A method according to claim 7, where the agent froth flotation is methylisobutylcarbinol or kerosene.

8. A method according to claim 1, where the tank froth flotation is a Denver cell.

9. A method according to claim 1, wherein lead dioxide (PbO2) is separated from the other compounds of lead in the froth flotation tank.

10. A method according to claim 1, further comprising manufacturing a new battery containing the separated lead dioxide (PbO2).

11. A method according to claim 1, wherein dioxo� of lead (PbO 2) is separated from the lead oxide (PbO) and/or lead sulfate (PbSO4in the froth flotation tank.

12. The method of separation of materials in the scrap lead-acid batteries, comprising stages on which:
remove the paste of lead-acid batteries waste lead-acid batteries,
suspend a paste of lead-acid batteries in water,
adding a froth flotation agent to the suspension containing the paste of lead-acid batteries and water;
was bubbled a froth flotation tank containing the slurry, the gas with the formation of foam;
separate lead dioxide (PbO2) from other lead-containing compounds in the slurry in a froth flotation tank.

13. A method according to claim 12, in which lead dioxide (PbO2) is separated from the lead oxide (PbO) and/or lead sulfate (PbSO4in the froth flotation tank.

14. A method according to claim 12, further comprising sorting lead-acid paste to a particle size of less than 200 μm before suspendirovanie acid-lead paste in water.



 

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FIELD: electrical engineering.

SUBSTANCE: invention relates to electrical engineering and can be used for recovery of storage battery capacity under negative ambient temperatures. invention aims at accelerating the capacity recovery and increasing the service life. For this, storage battery is pre-discharged to 0-0.5 V and charged to maximum magnitude. Prior to charging, battery voltage is measured and compared with preset value to control residual capacity to be discharged at load element. Note here that battery charging is carried out only at positive temperatures. For this, storage battery is placed into heat-insulated container. If temperature in container is negative or under required positive temperature electric heater built in said container is used to up the temperature to required level. The latter is controlled by temperature detector. Thereafter, battery is charged with charge current amplitude kept at 0.5-1.0 of rated capacity magnitude.

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FIELD: electricity.

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1 ex, 1 tbl

FIELD: electrical engineering.

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FIELD: chemistry; electrochemistry.

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3 cl, 1 dwg, 8 tbl

FIELD: medicine.

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EFFECT: higher safety of medical waste transportation to the residential solid waste ground.

4 cl, 1 dwg

FIELD: chemistry.

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EFFECT: inventions provide the complete recycling of fine fractions of processing products, enable producing high-calorie gas and increasing yield and quality of the finished products.

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EFFECT: minimising energy consumption during treatment of low-value natural and human-made refuse.

9 cl, 6 dwg, 1 tbl, 2 ex

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EFFECT: improved hydrophobic property of the disposed product and reduced concentration of harmful substances in aqueous extract of the disposed product.

2 cl, 1 tbl, 7 ex

FIELD: mining.

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EFFECT: improving development efficiency of an underground coal formation through process wells due to complex use of a heat resource of a coal combustion process, a mineral part of coal ash, and a degassed volume of an underground gas generator.

7 cl, 8 dwg

FIELD: chemistry.

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EFFECT: increased degree of samarium extraction due to the formation of strong complexes of samarium cations with sodium dodecylsulphate, transferred into the organic phase.

1 dwg, 1 ex

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