CN111455183B - Method for purifying and recovering lead and zinc by waste tire cracking carbon black - Google Patents

Method for purifying and recovering lead and zinc by waste tire cracking carbon black Download PDF

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CN111455183B
CN111455183B CN202010405877.4A CN202010405877A CN111455183B CN 111455183 B CN111455183 B CN 111455183B CN 202010405877 A CN202010405877 A CN 202010405877A CN 111455183 B CN111455183 B CN 111455183B
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zinc
lead
carbon black
leaching
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CN111455183A (en
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张正洁
佟永顺
孙莹
姜媛媛
朱合威
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Shenyang Xindi Environmental Technology Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/006—Wet processes
    • C22B7/008—Wet processes by an alkaline or ammoniacal leaching
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B07—SEPARATING SOLIDS FROM SOLIDS; SORTING
    • B07B—SEPARATING SOLIDS FROM SOLIDS BY SIEVING, SCREENING, SIFTING OR BY USING GAS CURRENTS; SEPARATING BY OTHER DRY METHODS APPLICABLE TO BULK MATERIAL, e.g. LOOSE ARTICLES FIT TO BE HANDLED LIKE BULK MATERIAL
    • B07B4/00—Separating solids from solids by subjecting their mixture to gas currents
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B07—SEPARATING SOLIDS FROM SOLIDS; SORTING
    • B07B—SEPARATING SOLIDS FROM SOLIDS BY SIEVING, SCREENING, SIFTING OR BY USING GAS CURRENTS; SEPARATING BY OTHER DRY METHODS APPLICABLE TO BULK MATERIAL, e.g. LOOSE ARTICLES FIT TO BE HANDLED LIKE BULK MATERIAL
    • B07B7/00—Selective separation of solid materials carried by, or dispersed in, gas currents
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B13/00—Obtaining lead
    • C22B13/04—Obtaining lead by wet processes
    • C22B13/045—Recovery from waste materials
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B19/00—Obtaining zinc or zinc oxide
    • C22B19/20—Obtaining zinc otherwise than by distilling
    • C22B19/24—Obtaining zinc otherwise than by distilling with leaching with alkaline solutions, e.g. ammonia
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B19/00—Obtaining zinc or zinc oxide
    • C22B19/20—Obtaining zinc otherwise than by distilling
    • C22B19/26—Refining solutions containing zinc values, e.g. obtained by leaching zinc ores
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
    • C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
    • C25C1/16—Electrolytic production, recovery or refining of metals by electrolysis of solutions of zinc, cadmium or mercury
    • 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
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

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  • Engineering & Computer Science (AREA)
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  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Mechanical Engineering (AREA)
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Abstract

The invention relates to a method for purifying and synergistically recovering lead and zinc by using waste tire pyrolysis carbon black, which comprises the following steps of: sorting to remove impurities, leaching heavy metals such as lead, zinc and the like in alkaline solution, purifying lead-rich zinc leachate, electrodepositing the purified zinc-rich electrolyte and the like. Separating and removing impurities to obtain crude carbon black with ash content of less than 3%; adding the crude carbon black into a sodium hydroxide solution, and carrying out processes of leaching, filtering, washing, drying and the like under the ultrasonic condition to finally obtain a pure carbon black product and a lead-rich and zinc-rich solution. The lead and zinc can be recovered by replacement-electrodeposition of the lead-rich and zinc-rich solution. The method has the characteristics of simple process, easy operation, clean process and the like, the obtained carbon black has good quality, and simultaneously, the heavy metals of lead and zinc are recovered, so that secondary pollution is avoided, and high-quality utilization of the waste tire cracking carbon black is realized.

Description

Method for purifying and recovering lead and zinc by waste tire cracking carbon black
Technical Field
The invention relates to a method for purifying and recovering lead and zinc by waste tire pyrolysis carbon black in coordination, which belongs to the field of resource utilization of solid waste and recovery of nonferrous metals, in particular to a method for directly leaching the waste tire pyrolysis carbon black and recovering lead and zinc under normal pressure and alkalinity.
Background
With the development of the automobile industry and the transportation industry in China, the yield of waste tires is increased year by year, and the waste tires become another pollution source of solid wastes in China. The yield of the waste tires in China in 2013 is about 1080 ten thousand tons, and the yield of the waste tires is expected to exceed 2000 ten thousand tons in 2020. At present, the method for recycling the waste tires comprises retreading, recycling and cracking. The retreaded tire can realize the recycling of the waste tire, but the retreaded tire has higher requirement on the integrity of the waste tire, and the retreaded tire still is solid waste after being scrapped, so that the problem of waste tire pollution is not fundamentally solved. The recycling is mainly to manufacture the reclaimed rubber powder and the reclaimed rubber, but the reclaimed rubber has high production energy consumption and serious environmental pollution, the production process of the reclaimed rubber powder has serious environmental secondary pollution, the product has limited application and unsatisfactory economy. The waste tyre is cracked to be degraded under the condition of oxygen deficiency or oxygen-free condition, and pyrolytic oil, steel wires, cracked slag and non-condensable gas are produced. The recovery rate of the waste tire cracking slag can reach 30-36%, and a large amount of cracking slag is piled up, so that the environmental risk and safety problems can be caused; the cracking slag is generally used as fuel of power plants and boilers, the utilization value is not high, the problem of secondary pollution exists, and the problems of low industrial application rate and the like exist when the cracking slag is used as active carbon. The society has strongly called for the emergence of new technologies for how to utilize waste tire cracked slag with high quality.
At present, due to the fact that various organic and inorganic additives are added in the production process of tires, and the inorganic additives are condensed on the surface of carbon black to form ash in the cracking process of waste tires, researches show that Zn, Pb, Si, Al and the like in the ash are main elements of the ash, so that the particle size of the carbon black is increased, the surface is rough, the specific surface area is increased, and the use value of the waste tire cracking slag as commercial carbon black is reduced. The traditional method for modifying the waste tire cracking slag mainly comprises graft modification and acid-base modification, and a large amount of waste liquid containing zinc and lead is generated in the modification process, so that secondary pollution is caused.
The invention patent CN109504134A discloses a method for preparing a carbon black product by adding an alkaline agent into carbon black prepared by a catalytic cracking method, then neutralizing, drying after neutralization, adding concentrated sulfuric acid, oxidizing the carbon black, then adding isocyanate to bond with hydroxyl on the surface of the carbon black, mixing the carbon black and water in a premixer, granulating, and drying by a drying kiln to obtain a finished product. The method provides a method for utilizing the cracking slag, but the method consumes a large amount of acid, alkali and organic solvent, generates heavy metal wastewater and has high treatment cost.
According to patent CN102504619A, the method comprises acid washing and alkali washing, and the carbon black subjected to acid washing and alkali washing is subjected to acid washing again. Through the purification process, the ash content of the carbon black is reduced from 18.7% to 2.6%, the volatile component is reduced from 9.5% to 5.0%, the reinforcing performance of the carbon black to rubber exceeds that of semi-reinforcing carbon black and basically reaches the reinforcing level of N330, and acid washing filtrate generated in the production process can be adjusted and then recycled into a purification system.
The research of Zhao Youcai et al shows that lead and zinc components have high solubility in strong alkaline solution, and patent No. CN101012514A discloses a method for producing metallic lead and zinc by using waste residue containing lead and zinc or low-grade lead-zinc oxide ore, which adopts strong alkaline leaching, lead and zinc enter into solution, then filtering, directly electrolyzing filtrate to obtain crude lead, and electrolyzing electrolyte after lead electrolysis to obtain metallic zinc powder. Patent No. CN1858275A, the invention can adapt to the treatment of various zinc oxide ores, zinc mud, zinc dross, zinc ash, zinc dust with zinc and lead grade above 5%, and the mixture of the above materials, the zinc and lead in the zinc oxide ores, the zinc mud, the zinc dross, the zinc ash and the zinc dust are dissolved by strong alkaline solution, then the lead and the zinc in the solution are respectively precipitated by precipitator, the process flow is simple, the control is easy, the equipment is simple, and the investment is low. The method is suitable for treating zinc oxide ores, zinc mud, zinc dross, zinc ash, zinc dust and mixtures of the materials, and is not definitely suitable for treating the waste tire cracking slag.
The invention adopts sodium hydroxide solution to leach the crude carbon black after impurity removal under the ultrasonic wave auxiliary condition, the lead leaching rate is more than 90 percent, the zinc leaching rate is about 95 percent, the primary leaching solution is continuously filtered and added with the crude carbon black to lead and zinc to be gathered in the sodium hydroxide solution, and zinc powder is adopted to precipitate the lead and then metal zinc is recovered by an electrodeposition method. The purification of the waste tire cracking carbon black not only improves the quality of the carbon black, but also recovers zinc and lead, and improves the resource utilization rate. The performance of the carbon black obtained by the method is similar to that of N330. The method has the characteristics of simple process, easy operation, clean process and the like.
Disclosure of Invention
In order to make up for the defects of the prior art, the invention aims to provide the method for purifying and synergistically recovering the lead and the zinc by the waste tire cracking carbon black, and the method has the advantages of high leaching rate of the zinc and the lead, thorough recycling of the solution and no discharge. The problem of heavy metal secondary pollution caused by traditional acid-base washing is solved, the quality of the carbon black is improved, and heavy metals of lead and zinc are recovered.
The invention aims to realize the following technical scheme, and discloses a method for purifying and synergistically recovering lead and zinc by using waste tire pyrolysis carbon black, which has the technical key points that: the method comprises the following steps:
(1) separation and impurity removal process
Grinding the carbon black cracked by the waste tires into powder, and separating heavy material silt, light material nylon and fiber by adopting a compound dry separator with the concentration degree of more than 95 percent to obtain crude carbon black with the impurity content of less than 3 percent;
(2) leaching process
a. Primary leaching out
Mixing 100g of the crude carbon black with 500ml of 300-12M sodium hydroxide solution, and then performing primary leaching, wherein primary filtration is performed after leaching time is 2-4h at the ultrasonic frequency of 80-130KHz and the temperature of the sodium hydroxide solution of 25-45 ℃, so as to obtain primary filtrate and primary filter residue respectively;
b. secondary leaching out
Returning the primary filtrate to primary leaching, adding the primary filter residue into a dilute alkaline solution for secondary leaching, and filtering, wherein the dilute alkaline solution is a 1-2M sodium hydroxide solution, the solid-to-liquid ratio or the weight ratio of the primary filter residue to the dilute alkaline solution is 1:3-4, and secondary filtering is performed to obtain secondary filtrate and secondary filter residue;
c. washing machine
Returning the secondary filtrate to secondary leaching, washing the secondary filter residue, wherein the washing water is industrial water, the temperature of the washing water is 40-45 ℃, directly washing a small amount of filter press for multiple times without discharging after secondary filter pressing, wherein the number of times is at least 2-3, washing the secondary filter residue to be neutral to obtain tertiary filter residue and tertiary filtrate, and returning the tertiary filtrate to secondary leaching; drying the filter residue for the third time to obtain a carbon black product;
repeating the steps, namely adding the crude carbon black into the sodium hydroxide solution in the primary leaching again, repeatedly leaching for multiple times to obtain primary zinc-rich lead-rich filtrate, wherein the primary zinc-rich filtrate is Pb in the primary filtrate2+Is 27-53g/L, Zn2+At 44-90g/L, the primary zinc-rich lead-rich filtrate enters a purification process;
(3) purification step
Adding zinc powder into the primary zinc-rich and lead-rich filtrate, wherein the dosage of the zinc powder is 1.05-1.1 times of the theoretical amount of impurity removal reaction, and filtering after lead is replaced to obtain crude lead and zinc-rich electrolyte;
(4) electrodeposition step
The anode adopts a lead-silver alloy plate, the cathode adopts an aluminum plate, the concentration of zinc ions is 71-95g/L, the temperature is 30-50 ℃, the bath voltage is 2-4V, and the current density is 50-150A/m2The concentration of soluble alcohols is 20-30g/L, electrolysis is carried out for 1-10h, the concentration of zinc ions in the electrolyte at the end point of electrodeposition is 10-15g/L, and the electrolyte returns to leaching for one time after electrodeposition.
The working principle of the invention is as follows:
the leaching process comprises the following steps: the sodium hydroxide solution mainly undergoes the following reaction in the leaching of crude carbon black:
ZnO+2NaOH=Na2Zn(OH)4
PbO+H2O+2NaOH=Na2Pb(OH)4
SiO2+2NaOH=Na2SiO3+H2O
the purification process comprises the following steps: zn + Pb2+=Pb+Zn2+,Zn+M2+=M+Zn2+Wherein M represents other mercury, copper and the like which are not active to zincA metal.
The process of the electrodeposition working procedure: zn2+-2e=Zn
4OH—-2e=2H2O+O2↑
The invention has the beneficial effects that:
(1) the invention adopts a compound dry separation technology, and the concentration degree is high and is more than 95 percent; the technology breaks through the original technical current situation that air is used as a separation medium, the novel dry separation equipment adopts a gas-solid two-phase mixed medium formed by fine coal (authigenic medium) contained in the selected pyrolysis carbon black and air to separate, and does not adopt air as the separation medium, so that the separation material has a wide particle size range, and compared with the condition that the traditional winnowing method can only separate narrow particle size grades, the novel winnowing machine can separate the particle size range of 80-0 mm. The separation efficiency is high, the air quantity is only 1/3 of the traditional winnowing, the buoyancy effect generated by the interaction of high-density particles is fully utilized, and the granularity of the discharged heavy material silt can be reduced.
(2) According to the invention, the waste tire cracking carbon black is leached by using a medium-concentration sodium hydroxide solution under an ultrasonic-assisted condition, so that the problem that heavy metals in the carbon black are difficult to separate out under normal pressure is solved, zinc oxide and lead oxide in the carbon black are dissolved in a strong alkali solution, high-pressure conditions are not required, the characteristics of a hydrometallurgy process are combined, recyclable zinc and recyclable lead are generated from leaching solution, and the electrolyzed leaching solution can be recycled.
(3) The method utilizes the waste tire cracking carbon black with low lead content and high zinc content as a raw material, accumulates lead and zinc in leaching solution by leaching the carbon black for multiple times, produces crude lead by adding simple substance zinc powder for replacement, improves the content of zinc in the leaching solution, and provides conditions for subsequent electrodeposition.
(4) The method not only obtains high-quality carbon black, but also recovers heavy metals of zinc and lead, realizes resource recycling, avoids secondary pollution, and has better economic benefit.
(5) Simple process, easy operation and clean process.
Drawings
FIG. 1 is a schematic process flow diagram of the purification and recovery of lead and zinc from waste tire cracking carbon black.
Detailed Description
300kg of pyrolytic carbon black from a certain waste tire pyrolysis enterprise in Hunan is shown in Table 1.
TABLE 1 analysis of the composition of pyrolytic crude carbon black of waste tires
Composition (I) Zn Pb Si Al Ca Fe
Content (%) 4.65 2.95 0.45 0.34 0.4 0.42
And (3) grinding the carbon black cracked from the waste tire, and separating heavy material silt, light material nylon and fiber by adopting a compound dry separator with the concentration degree of more than 95% to obtain crude carbon black with the impurity content of less than 3% for later use.
Example 1
(1) Proportioning 1000g of crude carbon black and 3000 ml of 5000-plus-one sodium hydroxide solution with the concentration of 10.5M, leaching for 2-4h under the condition of the ultrasonic frequency of 80-130KHz and the temperature of 40 ℃, filtering for the first time to obtain primary filtrate and primary filter residue respectively, returning the primary filtrate to the primary leaching, adding the primary filter residue into 1M of dilute alkaline solution, performing secondary filtration after secondary leaching, returning the secondary filtrate to the secondary leaching, washing the secondary filter residue in a filter press by industrial water with the temperature of 45 ℃ for 3 times until the secondary filter residue is neutral to obtain third filter residue, and drying the third filter residue to obtain a carbon black product. The washing water returns to the secondary leaching. Adding crude carbon black into the primary leaching solution again, repeatedly leaching for 10-15 times, and obtaining Pb in the primary filtrate2+40.28g/L, Zn2+Entering a purification process at 80.87 g/L; the comprehensive leaching rate of lead is more than 90 percent, and the comprehensive leaching rate of zinc is more than 95 percent;
(2) a purification process; adding zinc powder into the primary lead-rich and zinc-rich filtrate, wherein the using amount of the zinc powder is 1.05 times of the theoretical amount, and filtering after lead is replaced to obtain crude lead and zinc-rich electrolyte;
(3) an electrodeposition step; the anode adopts a lead-silver alloy plate, the cathode adopts an aluminum plate, and the zinc ion concentration is 94g/L, the temperature is 32-35 ℃, the cell voltage is 2-4V, and the current density is 120-2The concentration of the soluble glycerol is 20-30g/L, the electrolyte is electrolyzed for 7h at the circulation speed of 3-4L/min, 388.82g of metal zinc is obtained on a cathode plate, the concentration of zinc ions in the electrolyte is 11.24g/L at the end point of electrodeposition, and the electrolyte returns to leaching for one time after electrodeposition.
Example 2
(1) A leaching process; mixing 500g of waste tire cracked crude carbon black with 4000mL of 10M sodium hydroxide, putting the mixture into an ultrasonic extractor, reacting for 3h at the temperature of 40 ℃ at the frequency of 100KHz, filtering, adding 500g of crude carbon black into filtrate, supplementing 10mol/L of sodium hydroxide solution to 4000mL, putting the mixture into an ultrasonic extractor again, reacting for 3h at the normal temperature at the frequency of 100KHz, filtering, repeating the steps for 15 times, wherein the lead leaching efficiency is 85 percent, and the zinc leaching efficiency is 90 percent. And (3) washing the secondary filter residue in a filter press for 2-3 times by using a water washing process at the temperature of 40 ℃, washing to be neutral, and drying at the temperature of 105 ℃ to obtain the carbon black product.
(2) A purification process; adding zinc powder into the primary zinc-rich and lead-rich filtrate, wherein the using amount of the zinc powder is 1.1 times of the theoretical amount, and filtering after lead is replaced to obtain crude lead and zinc-rich electrolyte; the zinc concentration of the zinc-rich electrolyte is 95 g/L.
(3) An electrodeposition step; the anode adopts a lead-silver alloy plate, the cathode adopts an aluminum plate, electrolysis is carried out for 5 hours under the conditions of 45-55 ℃, current density of 60-80A/square meter, tank voltage of 3-3.5V, ethanol concentration of 25-30g/L and electrolyte circulation speed of 4L/min, 194.37g of metal zinc is obtained on the cathode plate, the concentration of zinc ions in the electrolyte is 11.78g/L at the end point of electrodeposition, and the electrolyte returns to leaching for one time after electrodeposition.
Example 3
(1) Leaching and (2) purifying; the test conditions were the same as in example 1;
(3) an electrodeposition step; the anode adopts a lead-silver alloy plate, the cathode adopts an aluminum plate, the electrolysis is carried out for 5 hours under the conditions of 45-50 ℃, the current density of 50-80A/square meter, the cell voltage of 3-3.5V and the circulation speed of the electrolyte of 4L/min, 390.17g of metal zinc is obtained on the cathode plate, the concentration of zinc ions in the electrolyte is 10.08g/L at the end point of the electrodeposition, and the electrolyte returns to leaching for one time after the electrodeposition.
Example 4
(1) Leaching and (2) purifying; the test conditions were the same as in example 2;
(3) an electrodeposition step; the anode adopts a lead-silver alloy plate, the cathode adopts an aluminum plate, the current density is 50-80A/square meter at 45-47 ℃, the cell voltage is 3-3.5V, the soluble reagents are glycerol and ethanol, the concentration of the glycerol is 15-18g/L, the concentration of the ethanol is 5-8g/L, the circulation speed of the electrolyte is 4L/min, the electrolysis is carried out for 5h, 195.56g of metal zinc is obtained on the cathode plate, the concentration of zinc ions in the electrolyte is 10.08g/L at the end point of the electrodeposition, and the electrolyte returns to leaching once after the electrodeposition.
(5) Performance index of carbon black product
The performance of the carbon black products made for the four cases of the present invention is compared to commercial carbon blacks and other carbon blacks made using acid and base washing methods as shown in table 2.
TABLE 2 comparison of the properties of the carbon blacks obtained according to the invention with those of the carbon blacks N330 and N660
Item Example 1 Example 2 Example 3 Example 4 Carbon Black N330 Carbon Black N660
Specific surface area for nitrogen adsorption/(m 2/g) 73 74 73 72 83 35
Iodine absorption value/(m)2/g） 65 65 65 58 82 36
DBP oil absorption/(mL/100 g) 85 89 89 85 102 90
Reduction by heating/% 1.2 1.3 1.2 1.3 ≤2.5 ≤3.0
Ash content% ≤1.55 ≤1.56 ≤1.57 ≤1.60 ≤0.5 ≤0.5
pH value 6.8 6.9 6.9 6.9 6.5 -
As is clear from Table 2, the carbon black obtained by the present invention is inferior to the carbon blacks N330 and N660 in the reinforcing property as a whole to the reinforcing property of N660 although the whole reinforcing property is inferior to that of N330.

Claims (2)

1. A method for purifying and recovering lead and zinc by waste tire cracking carbon black is characterized by comprising the following steps: the method comprises the following steps:
(1) separation and impurity removal process
Grinding the carbon black cracked by the waste tires into powder, and separating heavy material silt, light material nylon and fiber by adopting a compound dry separator with the concentration degree of more than 95 percent to obtain crude carbon black with the impurity content of less than 3 percent;
(2) leaching process
a. Primary leaching out
Mixing 100g of the crude carbon black with 500ml of 300-12M sodium hydroxide solution, and then performing primary leaching, wherein primary filtration is performed after the leaching time is 2-4h at the ultrasonic frequency of 80-130KHz and the temperature of the sodium hydroxide solution of 25-45 ℃, so as to obtain primary filtrate and primary filter residue respectively;
b. secondary leaching out
Returning the primary filtrate to primary leaching, adding the primary filter residue into a dilute alkaline solution for secondary leaching, and filtering, wherein the dilute alkaline solution is a 1-2M sodium hydroxide solution, the solid-to-liquid ratio or the weight ratio of the primary filter residue to the dilute alkaline solution is 1:3-4, and secondary filtering is performed to obtain secondary filtrate and secondary filter residue;
c. washing machine
The secondary filtrate is returned to secondary leaching, the secondary filter residue is washed, the washing water is industrial water, the temperature of the washing water is 40-45 ℃, and the secondary filter pressing is adopted, and then the filter press is directly washed in a filter press for many times without discharging materials; washing the secondary filter residue to be neutral to obtain a tertiary filter residue and a tertiary filtrate, and returning the tertiary filtrate to secondary leaching; drying the filter residue for the third time to obtain a carbon black product;
repeating the steps, namely adding the crude carbon black into the sodium hydroxide solution in the primary leaching again, repeatedly leaching for multiple times to obtain primary zinc-rich lead-rich filtrate, wherein the primary zinc-rich filtrate is Pb in the primary filtrate2+Is 27-53g/L, Zn2+44-90g/L, and the primary zinc-rich lead-rich filtrate enters a purification process;
(3) purification step
Adding zinc powder into the primary zinc-rich and lead-rich filtrate, wherein the dosage of the zinc powder is 1.05-1.1 times of the theoretical amount of impurity removal reaction, and filtering after lead is replaced to obtain crude lead and zinc-rich electrolyte;
(4) electrodeposition step
The anode adopts a lead-silver alloy plate, the cathode adopts an aluminum plate, the concentration of zinc ions is 71-94g/L, the temperature is 30-50 ℃, the bath voltage is 2-4V, and the current density is 50-150A/m2The concentration of soluble alcohol is 20-30g/L, the soluble alcohol is one or two of soluble glycerol and ethanol, electrolysis is carried out for 1-10h, the concentration of zinc ions in the electrolyte at the end point of electrodeposition is 10-15g/L, and the electrolyte returns to leaching for one time after electrodeposition.
2. The method for purifying and synergistically recovering lead and zinc from the waste tire cracking carbon black as claimed in claim 1, is characterized in that: and in the leaching procedure, the leaching is repeated for 10-20 times to obtain a primary zinc-rich lead-rich filtrate.
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