CN112143265A - Method for preparing carbon black and co-producing copper chloride by using waste enameled wire - Google Patents

Method for preparing carbon black and co-producing copper chloride by using waste enameled wire Download PDF

Info

Publication number
CN112143265A
CN112143265A CN201910578405.6A CN201910578405A CN112143265A CN 112143265 A CN112143265 A CN 112143265A CN 201910578405 A CN201910578405 A CN 201910578405A CN 112143265 A CN112143265 A CN 112143265A
Authority
CN
China
Prior art keywords
copper
carbon
mixture
carbon black
pyrolysis
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201910578405.6A
Other languages
Chinese (zh)
Other versions
CN112143265B (en
Inventor
李会泉
王兴瑞
李少鹏
朱干宇
孙振华
李占兵
关雪
韩艺娇
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Tongling Fuxiang Copper Based Material Technology Co ltd
Institute of Process Engineering of CAS
Original Assignee
Tongling Fuxiang Copper Recycling Co ltd
Institute of Process Engineering of CAS
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Tongling Fuxiang Copper Recycling Co ltd, Institute of Process Engineering of CAS filed Critical Tongling Fuxiang Copper Recycling Co ltd
Priority to CN201910578405.6A priority Critical patent/CN112143265B/en
Publication of CN112143265A publication Critical patent/CN112143265A/en
Application granted granted Critical
Publication of CN112143265B publication Critical patent/CN112143265B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/44Carbon
    • C09C1/48Carbon black
    • C09C1/50Furnace black ; Preparation thereof
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G3/00Compounds of copper
    • C01G3/04Halides
    • C01G3/05Chlorides

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Processing Of Solid Wastes (AREA)

Abstract

The invention provides a method for preparing carbon black and co-producing copper chloride by using waste enameled wires, which comprises the following steps: pyrolyzing the waste enameled wires to obtain a pyrolysis material; cooling and screening the obtained pyrolysis material, and separating to obtain a mixture of the copper simple substance and the copper carbon; reacting the copper-carbon mixture with hydrochloric acid to obtain a copper chloride solution and solid particles; and washing the solid particles, and drying to obtain the carbon black. According to the method, the insulating layer outside the waste enameled wire is converted into the carbon black through pyrolysis, the carbon black contains copper impurities, the copper in the copper-carbon mixture is converted into copper chloride through the dissolution reaction of the copper-carbon mixture and hydrochloric acid, the carbon black is separated from the copper, the content of the impurity ions in the obtained carbon black is as low as 0.3 wt%, and the method is simple to operate and has important industrial popularization value.

Description

Method for preparing carbon black and co-producing copper chloride by using waste enameled wire
Technical Field
The invention relates to the field of environmental protection, relates to a method for recycling waste enameled wires, and particularly relates to a method for preparing carbon black and co-producing copper chloride by using the waste enameled wires.
Background
Enameled wires are the main raw materials of products such as motors, electric appliances and household appliances, and particularly the electric power industry has been continuously and rapidly increased in recent years. The rapid development of household appliances brings a wide field for the application of enameled wires, the usage amount of the enameled wires is increased, and a large amount of waste enameled wires are generated.
The waste enameled wire is composed of disassembled electric appliance copper coils and paint-plating defective goods, so that the waste enameled wire contains abundant copper resources, but cannot be directly used as a copper raw material due to the existence of an insulating paint layer.
The metal copper is widely applied to industries such as electric power, machinery, electronics, electrical appliances, weapons, new energy and the like, while the copper ore resources in China are relatively deficient, and the external dependence is more than 70%, which seriously limits the development of the copper industrial chain in China. The recycling of the waste copper resources becomes an important means for making up the shortage of the copper resources in China, and the recycling of the copper in the waste enameled wires has important practical significance.
CN 108735399A discloses continuous processing equipment to useless circuit board/useless enameled wire based on pyrolysis liquifaction principle, continuous processing equipment includes that inside has furnace and the stove courage in heating chamber of heating chamber, and the stove courage is arranged in the heating intracavity of furnace, and has the heating ring chamber around the stove courage periphery in the heating chamber. The furnace pipe is internally provided with a treatment cavity for performing pyrolysis liquation on the waste circuit board/waste enameled wire, and the treatment cavity sequentially forms a preheating region, a pyrolysis region, a gasification region and an aggregate region along the direction from top to bottom of the treatment cavity; the preheating zone is subjected to dehydration and preheating treatment, organic matters in the waste circuit boards/waste enameled wires are cracked by the pyrolysis zone, coke formed by decomposition is gasified and alloy is separated by the gasification zone, and metal separated from the alloy is gathered by the collection zone; the recycling of metal in the waste circuit board/waste enameled wire is realized, but the coke is directly gasified in the gasification area, and partial copper particles are taken away by the gasification of the coke, so that the loss of copper resources is caused.
CN 104096842A discloses a production process of high-purity copper powder by using waste enameled wires, which sequentially performs sorting, cleaning and spin-drying operations on the waste enameled wires, wherein the sorting operation conditions capillary copper paint with the diameter of 0.04-0.1 mm; sending the picked capillary copper enameled wires into a liquating furnace in a sealed and oxygen-free environment for heating and pyrolysis, and performing forced cooling after pyrolysis; carrying out crushing and winnowing treatment on the furnace burden formed by heating and pyrolyzing the liquating furnace and then cooling to ensure that the furnace burden is coarsely crushed and activated carbon ash generated by pyrolysis is removed; and performing ball milling or turbine self-cooling crushing and screening operation on the furnace burden in sequence to obtain the high-purity copper powder. The method uses crushing and winnowing treatment to treat the activated carbon ash generated by pyrolysis, but the activated carbon ash is mixed with part of copper particles, so that the loss of copper resources is caused.
CN 108039253 a discloses a waste enameled wire paint removing system and an ash pushing mechanism, which are used for adjusting a temperature adjusting mechanism in a smoke exhaust pipeline, the ash pushing system recovers adverse effects caused by deposition adsorption of substances such as dust, carbon black and gas tar in pyrolysis smoke and in the pipeline, the reliability of the enameled wire paint removing system is significantly improved, but the mechanism only pushes away the ash pushing system, and the carbon black generated by pyrolysis is recycled.
A paper entitled "thermally treated waste copper enameled wire for copper recovery" was published by zhangmingke et al, which uses a thermal process to remove the insulating varnish of copper enameled wires, and the overall recovery rate can reach 95% (see document "thermally treated waste copper enameled wire for copper recovery", research on renewable resources, 1994, fifth phase, pages 13-19). However, no study was made on how to separate copper from char in the ash produced by pyrolysis.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a method for preparing carbon black and co-producing copper chloride by using waste enameled wires, which not only can recover copper in the waste enameled wires, but also can deeply separate a copper-carbon mixture generated by pyrolyzing the waste enameled wires to prepare carbon black and copper chloride.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a method for preparing carbon black and co-producing copper chloride by using waste enameled wires, which comprises the following steps:
(1) pyrolyzing the waste enameled wires to obtain a pyrolysis material;
(2) cooling the pyrolysis material obtained in the step (1), and then screening to obtain a mixture of a copper simple substance and copper carbon;
(3) mixing hydrochloric acid with the copper-carbon mixture obtained in the step (2), then carrying out dissolution reaction, and carrying out solid-liquid separation to obtain a copper chloride solution and solid particles;
(4) and (4) washing the solid particles obtained in the step (3), and drying to obtain the carbon black.
According to the invention, a pyrolysis material obtained after pyrolysis of the waste enameled wire is separated, and then the obtained copper-carbon mixture is reacted with hydrochloric acid to obtain a copper chloride solution and solid particles, and the solid particles are washed and dried to obtain the carbon black.
According to the invention, the copper chloride solution and the carbon black are obtained by reacting the copper-carbon mixture with hydrochloric acid, the copper-carbon mixture is recycled, the utilization rate of resources in the waste enameled wire is improved, and the stacking hazard of ash slag generated by pyrolysis of the waste enameled wire is reduced.
Preferably, the temperature of the pyrolysis treatment in the step (1) is 700-900 ℃, for example 700 ℃, 750 ℃, 800 ℃, 850 ℃ or 900 ℃, preferably 750-850 ℃.
Preferably, the pyrolysis treatment in step (1) is carried out for 0.5 to 2 hours, such as 0.5 hour, 0.6 hour, 0.7 hour, 0.8 hour, 0.9 hour, 1 hour, 1.1 hour, 1.2 hour, 1.3 hour, 1.4 hour, 1.5 hour, 1.6 hour, 1.7 hour, 1.8 hour, 1.9 hour or 2 hours, preferably 1 to 1.5 hours.
Preferably, the cooling method in the step (2) comprises spray water cooling.
According to the invention, after pyrolysis of the waste enameled wire, the insulating paint is pyrolyzed to obtain carbon black doped with copper particles, and the obtained carbon black is separated from the surface of a copper simple substance in the waste enameled wire.
Preferably, the cooling in step (2) is completed within 1-20min after the pyrolysis is finished, and may be 1min, 2min, 3min, 4min, 5min, 6min, 7min, 8min, 9min, 10min, 11min, 12min, 13min, 14min, 15min, 16min, 17min, 18min, 19min or 20min, for example.
The cooling is finished within 1-20min after the pyrolysis is finished, namely, the temperature of the pyrolysis material is reduced to room temperature within 1-20min after the pyrolysis is finished by a spray water cooling method, wherein the room temperature comprises 15-30 ℃, and can be 15 ℃, 18 ℃, 20 ℃, 24 ℃, 25 ℃, 27 ℃ or 30 ℃.
The temperature of the carbon black doped with copper particles after pyrolysis is high, and at the moment, the mixture of copper simple substance and copper carbon is easy to separate. If the cooling operation is not performed immediately after the pyrolysis is finished, the temperature of the copper-carbon mixture is naturally reduced, and the copper-carbon mixture is not easily separated from the copper simple substance.
Preferably, the acid of step (3) comprises any one of hydrochloric acid, nitric acid or sulfuric acid or a combination of at least two thereof, typical but non-limiting combinations include a combination of hydrochloric acid and nitric acid, a combination of hydrochloric acid and sulfuric acid, a combination of nitric acid and sulfuric acid or a combination of hydrochloric acid, nitric acid and sulfuric acid.
Preferably, the concentration of the acid in the step (3) is 100-200g/L, such as 100g/L, 110g/L, 120g/L, 130g/L, 140g/L, 150g/L, 160g/L, 170g/L, 180g/L, 190g/L or 200g/L, preferably 120-180 g/L.
Preferably, the temperature of the dissolution reaction in step (3) is 30-50 ℃, for example, 30 ℃, 31 ℃, 32 ℃, 33 ℃, 34 ℃, 35 ℃, 36 ℃, 37 ℃, 38 ℃, 39 ℃, 40 ℃, 41 ℃, 42 ℃, 43 ℃, 44 ℃, 45 ℃, 46 ℃, 47 ℃, 48 ℃, 49 ℃ or 50 ℃, preferably 35-45 ℃.
Preferably, the dissolution reaction time in step (3) is 0.5 to 2 hours, and may be, for example, 0.5h, 0.6h, 0.7h, 0.8h, 0.9h, 1h, 1.1h, 1.2h, 1.3h, 1.4h, 1.5h, 1.6h, 1.7h, 1.8h, 1.9h or 2h, preferably 1 to 1.5 h.
Preferably, the liquid-solid ratio of the hydrochloric acid and the copper-carbon mixture in the step (3) is 3-6mL/g, for example, 3mL/g, 3.5mL/g, 4mL/g, 4.5mL/g, 5mL/g, 5.5mL/g or 6mL/g, preferably 4-5 mL/g.
Preferably, the method further comprises the step of ball milling the copper-carbon mixture to a particle size of 325 mesh or less before mixing the hydrochloric acid with the copper-carbon mixture
Copper and compounds thereof in the copper-carbon mixture obtained by the method are wrapped by carbon, and in order to realize good separation of the copper, copper oxide and carbon black, the copper-carbon mixture is ball-milled by a ball milling method until the granularity is less than or equal to 325 meshes, so that the separation of the carbon black, the copper and the copper oxide is realized, the specific surface area of the copper, the copper oxide and the carbon black is increased, the copper oxide and the carbon black are easier to perform a dissolution reaction, and the efficiency of the dissolution reaction is improved.
The invention improves the specific surface area of copper and carbon black in the copper-carbon mixture by ball milling, so that the copper is easier to perform a dissolution reaction with acid, and the efficiency of the dissolution reaction is improved.
Preferably, the ball milling time is 2 to 5h, for example 2h, 2.5h, 3h, 3.5h, 4h, 4.5h or 5h, preferably 3 to 4 h.
Preferably, the washing in step (4) is washing with water.
Preferably, the liquid-solid ratio of the washing water to the solid particles is (1-3: 1), and may be, for example, 1:1, 1.5:1, 2:1, 2.5:1 or 3: 1.
Preferably, the solution generated after the washing in the step (4) is returned to the step (3) and mixed with acid for dissolution reaction.
Preferably, the drying method in step (4) is a conventional drying method, including but not limited to vacuum drying, air drying or oven drying, and can be reasonably selected by one skilled in the art according to actual needs.
As a preferred technical scheme of the method, the method comprises the following steps:
(1) pyrolyzing the waste enameled wire at the temperature of 700 ℃ and 900 ℃ for 0.5-2h to obtain a pyrolysis material;
(2) spraying water to the pyrolysis material obtained in the step (1) within 1-20min after pyrolysis is finished, then screening to obtain a mixture of a copper simple substance and copper carbon, and ball-milling the mixture of the copper carbon until the granularity is less than or equal to 325 meshes;
(3) mixing hydrochloric acid with the concentration of 100-200g/L and the copper-carbon mixture obtained in the step (2) according to the liquid-solid ratio of 3-6mL/g, then carrying out a dissolution reaction at the temperature of 30-50 ℃ for 0.5-2h, and carrying out solid-liquid separation to obtain a copper chloride solution and solid particles;
(4) and (4) washing the solid particles obtained in the step (3) according to the liquid-solid ratio (1-3) to 1, and drying to obtain the carbon black.
The recitation of numerical ranges herein includes not only the above-recited numerical values, but also any numerical values between non-recited numerical ranges, and is not intended to be exhaustive or to limit the invention to the precise numerical values encompassed within the range for brevity and clarity.
Compared with the prior art, the invention has the beneficial effects that:
the method comprises the steps of firstly converting an insulating layer outside the waste enameled wire into a copper-carbon mixture through pyrolysis, wherein the copper-carbon mixture contains copper and oxides thereof, and converting the copper and the oxides thereof in the copper-carbon mixture into copper chloride through a dissolving reaction of the copper-carbon mixture and hydrochloric acid, so that carbon black and copper are separated.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments.
The copper ion concentration and the chloride ion concentration in the examples and comparative examples of the present invention were measured by ion chromatography.
Example 1
The embodiment provides a method for preparing carbon black and co-producing copper chloride by using waste enameled wires, which comprises the following steps:
(1) pyrolyzing the waste enameled wire for 1h at 800 ℃ in a pyrolysis furnace to obtain a pyrolysis material;
(2) after the pyrolysis material is discharged from the pyrolysis furnace, spraying water to cool to 20 ℃ within 10min, screening to obtain a mixture of a copper simple substance and copper carbon, and ball-milling the mixture of the copper carbon until the granularity is less than or equal to 325 meshes;
(3) mixing hydrochloric acid with the concentration of 150g/L and the copper-carbon mixture obtained in the step (2) after ball milling according to the liquid-solid ratio of 5mL/g, then carrying out dissolution reaction at the temperature of 40 ℃ for 1h, and carrying out solid-liquid separation to obtain a copper chloride solution and solid particles;
(4) and (4) washing the solid particles obtained in the step (3) according to a liquid-solid ratio of 2:1, wherein the copper ion content in the obtained copper chloride solution is 13 wt%, and the chloride ion content in the carbon black is 0.6 wt%.
Example 2
The embodiment provides a method for preparing carbon black and co-producing copper chloride by using waste enameled wires, which comprises the following steps:
(1) pyrolyzing the waste enameled wire for 1.5h at 750 ℃ in a pyrolysis furnace to obtain a pyrolysis material;
(2) after the pyrolysis material is discharged from the pyrolysis furnace, spraying water to cool to 25 ℃ within 15min, screening to obtain a mixture of a copper simple substance and copper carbon, and ball-milling the mixture of the copper carbon until the granularity is less than or equal to 325 meshes;
(3) mixing hydrochloric acid with the concentration of 180g/L and the copper-carbon mixture obtained in the step (2) after ball milling according to the liquid-solid ratio of 4mL/g, then carrying out dissolution reaction at the temperature of 45 ℃ for 1h, and carrying out solid-liquid separation to obtain a copper chloride solution and solid particles;
(4) and (4) washing the solid particles obtained in the step (3) according to the liquid-solid ratio of 2.5:1, wherein the copper ion content in the obtained copper chloride solution is 10.7 wt%, and the chloride ion content in the carbon black is 0.3 wt%.
Example 3
The embodiment provides a method for preparing carbon black and co-producing copper chloride by using waste enameled wires, which comprises the following steps:
(1) pyrolyzing the waste enameled wire for 1h at 850 ℃ in a pyrolysis furnace to obtain a pyrolysis material;
(2) after the pyrolysis material is discharged from the pyrolysis furnace, spraying water to cool to 25 ℃ within 5min, screening to obtain a mixture of a copper simple substance and copper carbon, and ball-milling the mixture of the copper carbon until the granularity is less than or equal to 325 meshes;
(3) mixing hydrochloric acid with the concentration of 120g/L and the copper-carbon mixture obtained in the step (2) after ball milling according to the liquid-solid ratio of 5mL/g, then carrying out dissolution reaction at the temperature of 35 ℃ for 1.5h, and carrying out solid-liquid separation to obtain a copper chloride solution and solid particles;
(4) and (4) washing the solid particles obtained in the step (3) according to the liquid-solid ratio of 1.5:1, wherein the copper ion content in the obtained copper chloride solution is 17 wt%, and the chloride ion content in the carbon black is 0.3 wt%.
Example 4
The embodiment provides a method for preparing carbon black and co-producing copper chloride by using waste enameled wires, which comprises the following steps:
(1) pyrolyzing the waste enameled wires for 2 hours at 700 ℃ in a pyrolysis furnace to obtain a pyrolysis material;
(2) after the pyrolysis material is discharged from the pyrolysis furnace, spraying water to cool to 25 ℃ within 20min, screening to obtain a mixture of a copper simple substance and copper carbon, and ball-milling the mixture of the copper carbon until the granularity is less than or equal to 325 meshes;
(3) mixing hydrochloric acid with the concentration of 100g/L and the copper-carbon mixture obtained in the step (2) after ball milling according to the liquid-solid ratio of 6mL/g, then carrying out dissolution reaction at the temperature of 30 ℃ for 2h, and carrying out solid-liquid separation to obtain a copper chloride solution and solid particles;
(4) and (4) washing the solid particles obtained in the step (3) according to a liquid-solid ratio of 1:1, wherein the copper ion content in the obtained copper chloride solution is 16 wt%, and the chloride ion content in the carbon black is 1 wt%.
Example 5
The embodiment provides a method for preparing carbon black and co-producing copper chloride by using waste enameled wires, which comprises the following steps:
(1) pyrolyzing the waste enameled wires for 0.5h at 900 ℃ in a pyrolysis furnace to obtain a pyrolysis material;
(2) after the pyrolysis material is discharged from the pyrolysis furnace, spraying water to cool to 25 ℃ within 20min, screening to obtain a mixture of a copper simple substance and copper carbon, and ball-milling the mixture of the copper carbon until the granularity is less than or equal to 325 meshes;
(3) mixing hydrochloric acid with the concentration of 200g/L and the copper-carbon mixture obtained in the step (2) after ball milling according to the liquid-solid ratio of 3mL/g, then carrying out dissolution reaction at the temperature of 50 ℃ for 0.5h, and carrying out solid-liquid separation to obtain a copper chloride solution and solid particles;
(4) and (4) washing the solid particles obtained in the step (3) according to a liquid-solid ratio of 3:1, wherein the copper ion content in the obtained copper chloride solution is 9 wt%, and the chloride ion content in the carbon black is 0.3 wt%.
Example 6
This example provides a method for co-production of copper chloride from carbon black using waste enameled wire, which is the same as example 5 except that the hydrochloric acid concentration in step (3) is 240 g/L.
The content of copper ions in the finally obtained copper chloride solution is 7 wt%, the content of chloride ions in the carbon black is 0.5 wt%, and when the concentration of hydrochloric acid is 240g/L, copper in the copper-carbon mixture reacts with the hydrochloric acid to generate cuprous chloride, the cuprous chloride is difficult to dissolve, the further dissolution reaction of copper is influenced, the conversion rate of copper is reduced, and the purity of the obtained carbon black is reduced.
Example 7
This example provides a method for co-production of copper chloride from carbon black using waste enameled wire, which is the same as example 3 except that the hydrochloric acid concentration in step (3) is 80 g/L.
The content of copper ions in the finally obtained copper chloride solution is 8 wt%, the content of chloride ions in the carbon black is 0.8%, but when the concentration of hydrochloric acid is 80g/L, copper in the copper-carbon mixture cannot be completely converted into copper chloride, and the purity of the obtained carbon black is reduced.
Comparative example 1
This comparative example provides a method for recycling a waste enameled wire, which is the same as example 1 except that the acid used in step (3) is sulfuric acid having a concentration of 150 g/L.
The reaction of concentrated sulfuric acid with copper produces insoluble CuS, which is difficult to dissolve and affects the further dissolution reaction of copper, making the dissolution reaction unable to proceed smoothly.
Comparative example 2
This comparative example provides a method for recycling a waste enameled wire, which is the same as example 1 except that the acid used in step (3) is nitric acid having a concentration of 150 g/L.
The copper ion content of the obtained copper nitrate solution is 11 wt%, and the nitrate ion content of the carbon black is 10 wt%.
The nitric acid and the copper-carbon mixture generate a large amount of nitric oxide toxic gas during reaction, which is not beneficial to environmental protection.
In conclusion, the insulating layer outside the waste enameled wire is converted into the carbon black through pyrolysis, the carbon black contains copper impurities, the copper in the copper-carbon mixture is converted into the copper chloride through the dissolution reaction of the copper-carbon mixture and the acid, the carbon black is separated from the copper, the content of the impurity ions in the obtained carbon black is as low as 0.3 wt%, and the method is simple to operate and has important industrial popularization value.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are only exemplary embodiments of the present invention, and are not intended to limit the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (10)

1. A method for preparing carbon black and co-producing copper chloride by using waste enameled wires is characterized by comprising the following steps:
(1) pyrolyzing the waste enameled wires to obtain a pyrolysis material;
(2) cooling the pyrolysis material obtained in the step (1), and then screening to obtain a mixture of a copper simple substance and copper carbon;
(3) mixing hydrochloric acid with the copper-carbon mixture obtained in the step (2), then carrying out dissolution reaction, and carrying out solid-liquid separation to obtain a copper chloride solution and solid particles;
(4) and (4) washing the solid particles obtained in the step (3), and drying to obtain the carbon black.
2. The method as claimed in claim 1, wherein the temperature of the pyrolysis treatment in step (1) is 700-900 ℃, preferably 750-850 ℃;
preferably, the pyrolysis treatment of step (1) is carried out for a period of time ranging from 0.5 to 2 hours, preferably from 1 to 1.5 hours.
3. The method of claim 1 or 2, wherein the cooling of step (2) comprises spray water cooling.
4. The method of claim 3, wherein the cooling of step (2) is completed within 1-20min after the pyrolysis is completed.
5. The method according to any one of claims 1 to 4, wherein the concentration of the hydrochloric acid in step (3) is 200g/L, preferably 120 g/L.
6. The process according to any one of claims 1 to 5, wherein the temperature of the dissolution reaction of step (3) is 30 to 50 ℃, preferably 35 to 45 ℃;
preferably, the dissolving reaction time of the step (3) is 0.5-2h, preferably 1-1.5 h;
preferably, the liquid-solid ratio of the hydrochloric acid and the copper-carbon mixture in the step (3) is 3-6mL/g, and preferably 4-5 mL/g.
7. The method of any one of claims 1-6, further comprising the step of ball milling the copper char mixture to a particle size of 325 mesh or less prior to mixing the hydrochloric acid with the copper char mixture.
8. The method according to claim 7, characterized in that the ball milling time is 2-5h, preferably 3-4 h.
9. The method according to any one of claims 1 to 8, wherein the washing of step (4) is washing with water;
preferably, the liquid-solid ratio of the washing water to the solid particles is (1-3): 1.
10. A method according to any of claims 1-9, characterized in that the method comprises the steps of:
(1) pyrolyzing the waste enameled wire at the temperature of 700 ℃ and 900 ℃ for 0.5-2h to obtain a pyrolysis material;
(2) spraying water to the pyrolysis material obtained in the step (1) within 1-20min after pyrolysis is finished, then screening to obtain a mixture of a copper simple substance and copper carbon, and ball-milling the mixture of the copper carbon until the granularity is less than or equal to 325 meshes;
(3) mixing hydrochloric acid with the concentration of 100-200g/L and the copper-carbon mixture obtained in the step (2) according to the liquid-solid ratio of 3-6mL/g, then carrying out a dissolution reaction at the temperature of 30-50 ℃ for 0.5-2h, and carrying out solid-liquid separation to obtain a copper chloride solution and solid particles;
(4) and (4) washing the solid particles obtained in the step (3) according to the liquid-solid ratio (1-3) to 1, and drying to obtain the carbon black.
CN201910578405.6A 2019-06-28 2019-06-28 Method for preparing carbon black and co-producing copper chloride by using waste enameled wire Active CN112143265B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201910578405.6A CN112143265B (en) 2019-06-28 2019-06-28 Method for preparing carbon black and co-producing copper chloride by using waste enameled wire

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201910578405.6A CN112143265B (en) 2019-06-28 2019-06-28 Method for preparing carbon black and co-producing copper chloride by using waste enameled wire

Publications (2)

Publication Number Publication Date
CN112143265A true CN112143265A (en) 2020-12-29
CN112143265B CN112143265B (en) 2022-03-22

Family

ID=73891677

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201910578405.6A Active CN112143265B (en) 2019-06-28 2019-06-28 Method for preparing carbon black and co-producing copper chloride by using waste enameled wire

Country Status (1)

Country Link
CN (1) CN112143265B (en)

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102936663A (en) * 2012-11-21 2013-02-20 王恒傲 Smelting process for copper
CN104096842A (en) * 2014-07-16 2014-10-15 阙龙翔 High-purity copper powder production process utilizing waste copper enameled wires
CN106064826A (en) * 2016-06-02 2016-11-02 东莞市广华化工有限公司 A kind of method and apparatus utilizing wiring board acidic etching waste liquid to reclaim copper resource
CN107406909A (en) * 2015-04-08 2017-11-28 艺康美国股份有限公司 Leaching agent for metal recovery
CN108039253A (en) * 2017-12-11 2018-05-15 湖南顶立科技有限公司 A kind of enameled wire depainting system and ash-pulling machine structure
CN108752982A (en) * 2018-05-16 2018-11-06 中国科学院过程工程研究所 A kind of processing method of cupric carbon black

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102936663A (en) * 2012-11-21 2013-02-20 王恒傲 Smelting process for copper
CN104096842A (en) * 2014-07-16 2014-10-15 阙龙翔 High-purity copper powder production process utilizing waste copper enameled wires
CN107406909A (en) * 2015-04-08 2017-11-28 艺康美国股份有限公司 Leaching agent for metal recovery
CN106064826A (en) * 2016-06-02 2016-11-02 东莞市广华化工有限公司 A kind of method and apparatus utilizing wiring board acidic etching waste liquid to reclaim copper resource
CN108039253A (en) * 2017-12-11 2018-05-15 湖南顶立科技有限公司 A kind of enameled wire depainting system and ash-pulling machine structure
CN108752982A (en) * 2018-05-16 2018-11-06 中国科学院过程工程研究所 A kind of processing method of cupric carbon black

Also Published As

Publication number Publication date
CN112143265B (en) 2022-03-22

Similar Documents

Publication Publication Date Title
CN101775505B (en) Method and device for extracting lithium from lapidolite by chloridizing roasting method
CN101486462B (en) Preparation of titanium carbide micro powder
CN107758670B (en) Preparation method of boron carbide superfine powder
CN112142353B (en) Method for efficiently and harmlessly treating aluminum ash
CN103910344A (en) Preparation method of hexagonal boron nitride
Zhu et al. Recycling valuable metals from spent lithium‐ion batteries using carbothermal shock method
CN102616848A (en) Production method and production system for vanadium pentoxide
CN105645397A (en) Superfine-structure graphite for EDM (electrical discharge machining) and preparation method of superfine-structure graphite for EDM
CN112299849A (en) Method for preparing battery carbon rod by using regenerated graphite
CN112143265B (en) Method for preparing carbon black and co-producing copper chloride by using waste enameled wire
CN113793933B (en) Lithium sulfide for solid electrolyte and preparation method and application thereof
CN107902663B (en) Method and device for producing water glass by using industrial silicon byproduct micro silicon powder and waste heat
CN103667705A (en) Comprehensive utilization method for boric sludge waste
CN104692387B (en) A kind of method using silicon containing biomass as raw material low temperature preparation nanometer silicon carbide and preparation-obtained nanometer silicon carbide
CN107954718B (en) Boron carbide smelting device and preparation method of boron carbide
KR102063810B1 (en) Method for manufacturing lithiumchlorid and device of the same
CN114560960B (en) Method for preparing levoglucosan by catalytic pyrolysis of cellulose
CN102808091A (en) Method for preparing high-purity titanium
CN103643042A (en) Comprehensive utilization method of lead slag
CN101514025B (en) Method for preparing ultra pure magnesium oxide powder
CN103436757A (en) Magnesium-phosphorus intermediate alloy and preparation method thereof
CN106904619B (en) Using copper ashes as fe olivine material of major ingredient and preparation method thereof
CN114057194A (en) Method for preparing barium carbide and producing acetylene
KR101550136B1 (en) Recovery Method Of Aluminium Compound And PMMA From Waste Artificial Marble By Physical And Chemical Treatment
CN105800572A (en) Method for efficiently producing hexagonal boron nitride and co-producing sodium metaborate from borax

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant
CP01 Change in the name or title of a patent holder

Address after: 244000 Tongling Qisheng metal recycling resources Co., Ltd., Jinqiao Industrial Park, Yi'an District, Tongling City, Anhui Province

Patentee after: Tongling Fuxiang copper based material technology Co.,Ltd.

Patentee after: Institute of Process Engineering, Chinese Academy of Sciences

Address before: 244000 Tongling Qisheng metal recycling resources Co., Ltd., Jinqiao Industrial Park, Yi'an District, Tongling City, Anhui Province

Patentee before: TONGLING FUXIANG COPPER RECYCLING Co.,Ltd.

Patentee before: Institute of Process Engineering, Chinese Academy of Sciences

CP01 Change in the name or title of a patent holder