CN110028042B - Method for recycling waste cathode carbon blocks of electrolytic aluminum electrolysis cell - Google Patents
Method for recycling waste cathode carbon blocks of electrolytic aluminum electrolysis cell Download PDFInfo
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Abstract
The invention discloses a recycling method of waste cathode carbon blocks of an aluminum electrolytic cell, which comprises the steps of crushing, color sorting, crushing and ball milling raw materials of the waste cathode carbon blocks of the aluminum electrolytic cell to obtain carbon powder, then adding a 5A type or 10X type zeolite molecular sieve which accounts for 5-20 wt% of the mass of the carbon powder and has the granularity of less than 2mm, carrying out heat treatment at 800-1600 ℃ for 30-120 min, adding 98 wt% of concentrated sulfuric acid which is hot at 80-120 ℃ into an obtained fluorine-containing solid product, and introducing generated HF gas into deionized water for absorption and condensation to obtain a hydrofluoric acid product. The invention takes the zeolite molecular sieve as a heat treatment reaction material, simultaneously plays the role of a catalyst and a dispersing agent, has advanced process and obvious advantages, obtains a hydrofluoric acid product with high added value on the premise of realizing zero emission of harmful gas, and has remarkable environmental benefit and economic benefit.
Description
Technical Field
The invention belongs to the technical field of comprehensive utilization of electrolytic aluminum industrial solid wastes. In particular to a method for harmlessly treating waste cathode carbon blocks of an electrolytic aluminum cell and effectively recovering carbon and fluorine resources in the waste cathode carbon blocks.
Background
The electrolytic aluminum industry in China has kept a high growth rate since the 21 st century. The service life of the electrolytic cell for the electrolysis of the aluminum oxide is limited, overhaul is carried out every 3-5 years, and the waste cathode carbon block is one of main wastes generated by overhaul of the electrolytic cell and is a fluorine-containing dangerous solid waste generated in the electrolytic process.
The aluminum electrolysis capacity of China is 4500 ten thousand tons, the actual yield exceeds 3600 ten thousand tons and accounts for more than 50 percent of the global aluminum electrolysis capacity in 2017. In the process of aluminum electrolysis production, the carbon cathode expands due to the permeation of fluorine-containing salt, and further causes the damage and the rejection of the electrolytic cell. The aluminum electrolytic cell generally needs to be stopped for overhaul after about 4 to 6 years of use, all waste cell lining materials (overhaul residues for short) are taken out, and the waste cathode carbon blocks account for about 50 percent of the overhaul residues. The overhaul slag is solid waste inevitable in the production process of electrolytic aluminum, and 10-30 kg of overhaul slag is generated for each 1 ton of electrolytic aluminum. The electrolytic aluminum overhaul slag is specified as dangerous solid waste (category: HW48) in the national records of dangerous waste, and the waste tank lining is already listed as the national records of dangerous waste HW32 inorganic fluoride waste, HW33 inorganic cyanide waste. In the waste cathode carbon blocks for aluminum electrolysis, the carbon material accounts for 30-70%, the balance is electrolyte, mainly Na3[ AlF6], NaF, CaF2, MgF2, LiF, AlF3, NaCN, Na4[ Fe (CN)6], and the like, and a small amount of Al, Al4C3, AlN, Na, and the like, the substances have solubility and reaction activity with water and can generate harmful or flammable gases such as HF, HCN, H2, CH4, NH3 and the like, and fluorine-containing and cyanogen-containing compounds entering the environment can cause great harm to the health and growth of human beings, animals and plants. Therefore, the research on the comprehensive utilization technology of the waste cathode carbon blocks of the aluminum electrolytic cell is not only the content of resource recovery, but also the requirement of environmental protection, and meets the requirement of the sustainable development strategy of China.
The waste cathode carbon block is a valuable resource rich in highly graphitized carbon and fluorine-containing electrolyte. Therefore, how to thoroughly eliminate the harm of fluoride and cyanide in the aluminum electrolysis waste cathode carbon block and realize the harmlessness and resource recycling of the aluminum electrolysis waste cathode carbon block is an industry difficult need to overcome, and the technical experts in the industry and production front-line personnel carry out years of continuous research and research aiming at the difficult problem, the treatment is carried out by methods such as alkaline leaching or ultrasonic-assisted flotation pressure alkaline leaching (CN106745137A, CN106077038A, CN106077040A, CN106587122A, CN101817521A, CN106086938A and CN105821445A), acid treatment or ultrasonic-assisted flotation pressure acid treatment (CN106077037A, CN106077036A, CN106180118A and CN101984984A), combination of alkaline leaching and acid leaching and fly ash (CN107162061A), heat preservation and cyanogen removal combined flotation to obtain carbon slag and electrolyte slag and heating to remove carbon (CN106064813A, CN105964659A and CN107313073A), high-temperature calcination (CN102989744A, CN105964660A, CN106517209A, CN107904621A, CN106147910A, CN100542702C, CN101054693A, CN107628614A, CN105642649A, CN106185818A and CN106269787A), water leaching (CN105772486A, CN107377592A, CN105728440A and CN106166560A), chemical precipitation (CN105327933A) and the like.
From the prior technical results, the harmless and resource treatment and utilization of the waste cathode carbon block of the aluminum electrolytic cell are divided into two main categories of wet treatment and high-temperature treatment of aqueous solution. The wet treatment involves water washing (leaching), alkali treatment, acid-alkali combination, combined flotation process and the like, mainly aims at recovering electrolyte and carbon, and adopts an oxidant to decompose cyanide into harmless gas substances in the wet treatment. The high-temperature treatment technology mainly aims at harmlessness, and uses the waste cathode as fuel to burn, or adopts the combination of technologies such as high temperature, vacuum and the like to respectively recycle the electrolyte or the carbon material, so that the cyanogen-containing compound is oxidized and decomposed into harmless gas substances at high temperature.
From the prior technical achievements, the wet treatment and high-temperature treatment of the waste cathode carbon block of the aluminum electrolytic cell still have the following problems, such as that a large amount of salt-containing and fluorine-containing wastewater generated in the wet treatment is not effectively treated, and secondary pollution is caused; generated H 2 、CH 4 、NH 3 The gas is not controlled and utilized, and the generated HF causes serious pollution; the recovered electrolyte and carbon material have high impurity content and can not be directly utilized; the difficulty of process control is high due to the influence of factors such as the difference of the capacity and the age of the electrolytic aluminum tank, the fluctuation of components, the granularity of powder and the like; a large amount of tail gas carrying HF and dust is generated in the high-temperature treatment; the electrolyte is not completely recovered, and part of the electrolyte remains in the carbon material or the slag; the melting agglomeration of the electrolyte with low melting point occurs in the furnace, which causes the incomplete combustion residue of the carbon material to be larger, and the melting agglomeration of the electrolyte in the furnace causes the deterioration of the production working condition and the poor production stability.
Disclosure of Invention
The invention aims to provide a new technical scheme aiming at the defects of the existing aluminum electrolysis waste cathode carbon block treatment scheme. The scheme combines the pyrogenic process treatment and the wet process treatment, carries out harmless treatment and resource utilization on the waste cathode carbon blocks of the aluminum electrolytic cell aiming at the characteristic that the waste cathode carbon blocks contain fluoride, obtains hydrofluoric acid products with high added value on the premise of realizing zero emission of harmful gas, further solves the environmental protection problem of solid waste and generates considerable economic benefit.
The main component of the zeolite molecular sieve is SiO 2 And Al 2 O 3 The compound of the isoalumino silica and the carbon block can react with the following components:
C(NaF)+O 2 →NaF+CO 2 ↑ (1)
2NaCN+(2X+5)/2O 2 →2Na 2 O+2CO 2 ↑+2NO x ↑ (2)
2CaO+SiO 2 →Ca 2 SiO 4 (3)
2NaF+CaO+2SiO 2 +Al 2 O 3 →CaF+2NaAlSiO 4 (4)
2NaF+3CaO+SiO 2 +11Al 2 O 3 →Ca 2 SiO 4 ·CaF 2 +2NaAl 11 O 17 (5)
the technical scheme for solving the technical problems is as follows:
a method for recycling waste cathode carbon blocks of an electrolytic aluminum cell is characterized by comprising the following steps: crushing the waste cathode carbon blocks into carbon powder with the granularity of less than 45 meshes by using a crusher and a ball mill, and adding 5A type or 10X type zeolite molecular sieves with the mass of 5-20 wt% of the carbon powder and the granularity of less than 2mm into the carbon powder to obtain uniformly mixed solid powder; carrying out high-temperature heat treatment on the mixed solid powder at the temperature of 800-1600 ℃ for 30-120 min; CO produced by heat treatment 2 、NO x Introducing the gas into 10 percent NaOH solution for absorption to obtain Na 2 CO 3 、NaNO 3 Recovering the salt solution; adding 98 wt% concentrated sulfuric acid at 80-120 ℃ into the fluorine-containing solid obtained after heat treatment to obtain the solid, mixed salt solution and HF gasThree products, wherein the solid product is carbon powder for recycling; the liquid is mixed salt solution, 20 percent NaOH solution is added to adjust the pH of the solution to 7 to obtain Na 2 SO 4 Recovering the solution; and introducing HF gas into deionized water for absorption and condensation to obtain a hydrofluoric acid product.
In the present invention, the zeolite molecular sieve used is a 5A type zeolite molecular sieve.
The invention takes the zeolite molecular sieve as a heat treatment reaction material, simultaneously plays the role of a catalyst and a dispersing agent, has advanced process and obvious advantages, obtains a hydrofluoric acid product with high added value on the premise of realizing zero emission of harmful gas, and has remarkable environmental benefit and economic benefit.
Drawings
FIG. 1 is a process flow diagram of the method for recycling waste cathode carbon blocks of an aluminum electrolytic cell. The raw material is waste cathode carbon blocks of the aluminum electrolytic cell; the mixed solid is a solid material obtained by uniformly mixing powdered carbon and a zeolite molecular sieve after crushing and ball milling; the solid is a fluorine-containing solid product after heat treatment; the gas is mixed gas generated by heat treatment; the liquid is a mixed salt solution obtained after the wet treatment by adding hot concentrated sulfuric acid.
Detailed Description
The present invention will be further described with reference to the following examples, but it should be noted that the scope of the present invention is not limited to these examples.
Example 1
A method for recycling waste cathode carbon blocks of an electrolytic aluminum electrolysis cell comprises the following steps: crushing the waste cathode carbon blocks into carbon powder with the granularity of less than 45 meshes by using a crusher and a ball mill, and adding 5 wt% of the carbon powder, namely 0.5g of 5A-type zeolite molecular sieve with the granularity of less than 2mm, into 10g of the carbon powder to obtain uniformly mixed solid powder; carrying out high-temperature heat treatment on the mixed solid powder at 800 ℃ for 30 min; CO produced by heat treatment 2 、NO x Introducing the gas into 10 percent NaOH solution for absorption to obtain Na 2 CO 3 、NaNO 3 Recovering the salt solution; adding 98 wt% concentrated sulfuric acid at 80 deg.C into the fluorine-containing solid obtained after heat treatment to obtain solidThree products of a substance, a mixed salt solution and HF gas, wherein the solid product is carbon powder for recycling; the liquid is mixed salt solution, 20 percent NaOH solution is added to adjust the pH of the solution to 7 to obtain Na 2 SO 4 Recovering the solution; introducing HF gas into deionized water for absorption and condensation to obtain a hydrofluoric acid product, wherein the recovery rate of fluorine in the waste carbon blocks is 81.3%.
Example 2
A method for recycling waste cathode carbon blocks of an electrolytic aluminum electrolysis cell comprises the following steps: crushing the waste cathode carbon blocks into carbon powder with the granularity of less than 45 meshes by using a crusher and a ball mill, and adding 10g of the carbon powder into 10g of the carbon powder, wherein the mass of the carbon powder is 20 wt%, namely 2.0g of 10X-type zeolite molecular sieve with the granularity of less than 2mm, so as to obtain uniformly mixed solid powder; carrying out high-temperature heat treatment on the mixed solid powder at 1600 ℃ for 120 min; CO produced by heat treatment 2 、NO x Introducing the gas into 10 percent NaOH solution for absorption to obtain Na 2 CO 3 、NaNO 3 Recovering the salt solution; adding 98 wt% concentrated sulfuric acid at 120 ℃ into the fluorine-containing solid obtained after heat treatment to obtain three products, namely a solid, a mixed salt solution and HF gas, wherein the solid product is carbon powder for recycling; the liquid is mixed salt solution, 20 percent NaOH solution is added to adjust the pH of the solution to 7 to obtain Na 2 SO 4 Recovering the solution; introducing HF gas into deionized water for absorption and condensation to obtain a hydrofluoric acid product, wherein the recovery rate of fluorine in the waste carbon blocks is 82.7%.
Example 3
A method for recycling waste cathode carbon blocks of an electrolytic aluminum electrolysis cell comprises the following steps: crushing the waste cathode carbon blocks into carbon powder with the granularity of less than 45 meshes by using a crusher and a ball mill, and adding 10 wt% of the carbon powder, namely 2.0g of 5A-type zeolite molecular sieve with the granularity of less than 2mm, into 20g of the carbon powder to obtain uniformly mixed solid powder; carrying out high-temperature heat treatment on the mixed solid powder at the temperature of 1000 ℃ for 80 min; CO produced by heat treatment 2 、NO x Introducing the gas into 10 percent NaOH solution for absorption to obtain Na 2 CO 3 、NaNO 3 Recovering the salt solution; in the heat treatmentAdding 98 wt% concentrated sulfuric acid at 110 ℃ into the obtained fluorine-containing solid to obtain three products, namely a solid product, a mixed salt solution and HF gas, wherein the solid product is carbon powder for recycling; the liquid is mixed salt solution, 20 percent NaOH solution is added to adjust the pH of the solution to 7 to obtain Na 2 SO 4 Recovering the solution; introducing HF gas into deionized water for absorption and condensation to obtain a hydrofluoric acid product, wherein the recovery rate of fluorine in the waste carbon blocks is 84.1%.
Example 4
A method for recycling waste cathode carbon blocks of an electrolytic aluminum electrolysis cell comprises the following steps: crushing the waste cathode carbon blocks into carbon powder with the granularity of less than 45 meshes by using a crusher and a ball mill, and adding 10X-type zeolite molecular sieves with the mass of 8 wt% of the carbon powder and the granularity of less than 2mm into 30g of the carbon powder to obtain uniformly mixed solid powder; carrying out high-temperature heat treatment on the mixed solid powder at 1200 ℃ for 60 min; CO generated by heat treatment 2 、NO x Introducing the gas into 10 percent NaOH solution for absorption to obtain Na 2 CO 3 、NaNO 3 Recovering the salt solution; adding 98 wt% concentrated sulfuric acid at 100 ℃ into the fluorine-containing solid obtained after heat treatment to obtain three products, namely a solid, a mixed salt solution and HF gas, wherein the solid product is carbon powder for recycling; the liquid is mixed salt solution, 20 percent NaOH solution is added to adjust the pH of the solution to 7 to obtain Na 2 SO 4 Recovering the solution; and introducing HF gas into deionized water for absorption and condensation to obtain a hydrofluoric acid product, wherein the fluorine recovery rate in the waste carbon block is 83.5%.
Claims (2)
1. A method for recycling waste cathode carbon blocks of an electrolytic aluminum cell is characterized by comprising the following steps: crushing the waste cathode carbon blocks into carbon powder with the granularity of less than 45 meshes by using a crusher and a ball mill, and adding 5A type or 10X type zeolite molecular sieves with the mass of 5-20 wt% of the carbon powder and the granularity of less than 2mm into the carbon powder to obtain uniformly mixed solid powder; carrying out high-temperature heat treatment on the mixed solid powder at the temperature of 800-1600 ℃ for 30-120 min; CO produced by heat treatment 2 、NO x Introducing gas into 10% NaOH solution for absorptionCollecting to obtain Na 2 CO 3 、NaNO 3 Recovering the salt solution; adding 98 wt% concentrated sulfuric acid at 80-120 ℃ into the fluorine-containing solid obtained after heat treatment to obtain three products, namely a solid, a mixed salt solution and HF gas, wherein the solid product is carbon powder for recycling; the liquid is mixed salt solution, 20 percent NaOH solution is added to adjust the pH of the solution to 7 to obtain Na 2 SO 4 Recovering the solution; and introducing HF gas into deionized water for absorption and condensation to obtain a hydrofluoric acid product.
2. The method for recycling waste cathode carbon blocks of an electrolytic aluminum electrolysis cell according to claim 1, wherein the zeolite molecular sieve is a 5A type zeolite molecular sieve.
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| CN104743560A (en) * | 2013-12-25 | 2015-07-01 | 贵州大学 | Method for preparing silicon/aluminium series product by taking gangue as raw material |
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| CN1785537A (en) * | 2005-11-28 | 2006-06-14 | 中国铝业股份有限公司 | Treatment method of aluminium electrolytic bath waste cathode carbon blook innocuousnes |
| CN104743560A (en) * | 2013-12-25 | 2015-07-01 | 贵州大学 | Method for preparing silicon/aluminium series product by taking gangue as raw material |
| CN108941167A (en) * | 2018-08-01 | 2018-12-07 | 湘潭大学 | Mechanochemistry conversion and recovery method in a kind of waste cathode of aluminum electrolytic cell carbon block containing sodium, fluorochemical |
| CN109047285A (en) * | 2018-08-01 | 2018-12-21 | 湘潭大学 | Containing sodium, the method for transformation of fluorochemical and system in a kind of waste cathode of aluminum electrolytic cell carbon block |
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