CN111100990A - Preparation method for preparing lithium ion cathode material by utilizing PTA oxidation section residue - Google Patents
Preparation method for preparing lithium ion cathode material by utilizing PTA oxidation section residue Download PDFInfo
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- CN111100990A CN111100990A CN201911317476.7A CN201911317476A CN111100990A CN 111100990 A CN111100990 A CN 111100990A CN 201911317476 A CN201911317476 A CN 201911317476A CN 111100990 A CN111100990 A CN 111100990A
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- C—CHEMISTRY; METALLURGY
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- 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
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- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
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- C22B23/0415—Leaching processes with acids or salt solutions except ammonium salts solutions
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- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
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- C22B26/12—Obtaining lithium
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- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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Abstract
The invention belongs to the technical field of PTA oxidation residue recovery and treatment, and particularly relates to a preparation method for preparing a lithium ion cathode material by utilizing PTA oxidation section residue, which comprises the following steps: measuring the content of each metal in the residue leaching solution of the PTA oxidation section; then precipitating Fe3+And removing the precipitate; then supplement Co2+、Mn2+、Ni2+、Li+Adding sodium carbonate, filtering, precipitating, drying, and calcining in airObtaining the ternary cathode material LiNi of the lithium ion batteryxMnyCozO2. The method directly converts the metal in the PTA oxidation section residue into the ternary cathode material LiNixMnyCozO2The method has the advantages of simple process, good repeatability, low cost and environmental friendliness.
Description
Technical Field
The invention belongs to the technical field of PTA oxidation residue recovery and treatment, and particularly relates to a preparation method for preparing a lithium ion positive electrode material by utilizing PTA oxidation section residue.
Background
Purified Terephthalic Acid (PTA) is one of important organic chemical raw materials, and is mainly used for producing polyester fibers. China is a large chemical fiber production country, and the discharge amount of PTA refined wastewater is very large, so that the PTA refined wastewater becomes one of important pollution sources of water environment. The PTA oxidation residue is a process of generating Terephthalic Acid (TA) by high-temperature oxidation by taking paraxylene as a raw material, acetic acid as a solvent, cobalt manganese acetate as a catalyst and air as an oxidant in the PTA production process. The residue produced in the PTA oxidation section mainly contains TA solid particles and a catalyst containing cobalt and manganese, and if the cobalt and manganese in the catalyst are effectively recovered, good environmental benefit and economic benefit are brought to the society.
At present, the following two methods are mainly adopted for the recovery of the catalyst:
firstly, adding an extracting agent and a precipitating agent into the leaching solution or using an ion exchange column to selectively separate cobalt and manganese and then recovering the cobalt and manganese as separate metal salts. P204 is a common extracting agent, phosphoryl in P204 is extracted due to a chelate formed by lone pair electron pair energy on an oxygen atom and metal ions, then the P204 is used as a mobile phase, the cobalt and manganese can be effectively separated by adopting multi-stage countercurrent extraction, the metal recovery rate can reach more than 85 percent through optimization, and the cobalt-manganese ratio in an outlet water phase reaches 1000: more than 1 (Zhang cong Ling, Huangningping, Lu Chun moth. P204 extraction separation of cobalt and manganese in catalyst mother liquor [ J]Water treatment techniques, 1993 (02): 31-36.). The method has the advantages of high balancing speed, good separation effect, high processing capacity, high recovery rate and simple operation, but the metal recovery rate of the method is highTo be improved. Carrying out cation exchange on the aqueous solution containing cobalt ions, manganese ions and other trace metal ions by adopting a strong-acid cation exchange resin; fe in the solution2+Complete conversion to Fe3+And is removed during neutralization so that the iron ions are completely removed during neutralization. The recovery rate of the cobalt-manganese catalyst is more than or equal to 95 percent, and the purity of the recovered crystallized and dried cobalt acetate and manganese acetate catalyst is more than or equal to 99.7 percent. The method has the advantages of high cobalt and manganese recovery rate and purity, but the cost is too high.
And secondly, after organic matters are removed from the leaching solution of the catalyst, the leaching solution is recovered in a cobalt-manganese mixed salt form. For example, filtering and washing the oxidation residue with water to obtain an acidic aqueous solution containing cobalt and manganese, adjusting the pH of the filtrate with carbonate to be more than or equal to 8.5, precipitating cobalt and manganese in the form of carbonate, and then adding acetic acid to react with the cobalt-manganese carbonate to obtain the mixed catalyst containing cobalt acetate and manganese acetate. The process is simple, but cannot return to an oxidation section for continuous use, and the economic benefit is poor (Japanese patent FP 0515788). German improved on the basis that Fe is removed by adjusting pH to 5.53+After the removal of impurities, the acetate of cobalt and manganese can be returned to the oxidation section for further use, but the purity of the catalyst affects the effect of the catalyst (German patent GER ofen 2260498). Liu Xicai is treated by adding Na2CO3The pH value of the solution is controlled, so that iron ions, chromium ions, nickel ions and cobalt and manganese ions are selectively precipitated and separated, the purity of the cobalt and manganese catalyst is improved, Co/Mn ions are prevented from being adsorbed by ion exchange, the step of electrolysis is avoided, the treatment process of oxidation section residues is simplified, the recovery rate of the cobalt and manganese catalyst is improved from 70% to 85%, the production cost is reduced by 30%, and the energy consumption is reduced by 40%. The method has the advantages of meeting the requirements of energy conservation and environmental protection and obtaining the maximum filtration benefit, but the recovery rate of cobalt and manganese in the method needs to be further improved (Chinese patent CN 102626646A).
In summary, the existing method for recovering cobalt and manganese in PTA oxidation section residue cannot give consideration to the advantages of low cost, simple process flow, environmental friendliness and the like.
Disclosure of Invention
In order to overcome the defects that the recovery method of cobalt and manganese in PTA oxidation section residues in the prior art cannot give consideration to low cost, simple process and environmental friendliness, the invention provides a preparation method for preparing a lithium ion cathode material by utilizing PTA oxidation section residues, which specifically comprises the following steps:
(1) adding a mixed solution of sulfuric acid and hydrogen peroxide into the PTA oxidation section residue to obtain a leaching solution;
(2) measuring the content of each metal in the leachate obtained in the step (1) by using an ICP (inductively coupled plasma) spectrometry or a titration method;
(3) adding Na according to the content of each metal determined in the step (2)2CO3Adjusting the pH value of the solution to 2-4 to enable Fe3+Formation of Fe (OH)3Separating out, filtering and removing the precipitate;
(4) according to the Co determined in the step (2)2+、Mn2+Concentration, adding Co2+、Mn2+、Ni2+、Li+According to the ternary positive electrode material LiNixMnyCozO2Determining the addition amount of soluble salt by x, y and z values in the solution, and adding Na2CO3Reacting the solution for 2 hours, filtering, precipitating, washing and drying;
(5) ball-milling the solid obtained after drying in the step (4), and then calcining in the air atmosphere to obtain the black solid powder ternary cathode material LiNixMnyCozO2。
Preferably, the concentration of the sulfuric acid in the mixed solution in the step (1) is 2-5mol/L, and the mass concentration of the hydrogen peroxide is 25% -40%.
Preferably, the Co in step (4)2+、Mn2+、Ni2+、Li+The soluble salt of (A) is Co2+、Mn2+、Ni2+、Li+One or more of sulfate, nitrate or acetate.
Adding Na in the step (4)2CO3The amount of the solution is such that Na2CO3With respect to the molar amount of LiNi per molexMnyCozO2The molar weight ratio of the total metals in the alloy is 1.1-1.5.
Preferably, the washing in the step (4) is carried out for a plurality of times by using deionized water; the drying temperature is 80-110 ℃, and the drying time is 24-36 h.
Preferably, the ball milling time in the step (5) is 1 h; the calcining temperature is 850-950 ℃, and the calcining time is 8-12 h.
Preferably, the ternary positive electrode material LiNixMnyCozO2Middle 0<x<2/3,0<y<2/3,0<z<2/3, x + y + z is 1; more preferably, x is 1/3, y is 1/3, and z is 1/3.
Preferably, the ternary positive electrode material LiNixMnyCozO2Has a particle diameter of 5-15 μm.
The invention has the beneficial effects that:
aiming at the defects that organic matters are removed in advance, cobalt and manganese in filtrate are difficult to separate or acetate catalyst prepared by direct recovery has low purity to cause poor catalytic performance and the like in the cobalt and manganese recovery process in the prior art, the method directly converts PTA oxidation section doping into lithium ion battery ternary anode material LiNi through adding corresponding metal ion salt and sodium carbonatexMnyCozO2The method has the advantages of simple preparation process, avoidance of complex processes and high cost for removing organic matters, separating cobalt and manganese, and recovering and preparing acetate catalyst.
Drawings
FIG. 1 is a flow chart of the process for preparing a lithium ion cathode material by utilizing PTA oxidation stage residue according to the present invention;
FIG. 2 shows LiNi, a ternary positive electrode material for a lithium ion battery prepared in example 11/3Mn1/3Co1/3O2XRD pattern of (a);
FIG. 3 shows LiNi, a ternary positive electrode material for a lithium ion battery prepared in example 11/3Mn1/3Co1/3O2SEM picture of (1);
FIG. 4 shows LiNi, a ternary positive electrode material of a lithium ion battery prepared in example 20.5Mn0.2Co0.3O2SEM picture of (1);
FIG. 5 shows LiNi, a ternary positive electrode material of a lithium ion battery prepared in example 31/3Mn1/3Co1/3O2SEM image of (d).
Detailed Description
Example 1
A preparation method for preparing a lithium ion cathode material by utilizing PTA oxidation section residues is shown in figure 1, and specifically comprises the following steps:
adding a mixed solution of sulfuric acid and hydrogen peroxide into PTA oxidation section residues, wherein the concentration of sulfuric acid in the mixed solution is 3mol/L, H2O2The mass concentration is 30%, leaching is carried out to obtain leachate, 5ml of leachate is taken to carry out ICP test, and the obtained metal content is shown in Table 1. As can be seen from Table 1, Co is used in the solution2+And Mn2+Mainly with a small amount of Fe3+、Ni2+And Ca2+. First, 0.5mol/L Na is added2CO3Adjusting the pH value of the solution to 2-4 to enable Fe3+Formation of Fe (OH)3Separating out, filtering and removing the precipitate; according to LiNi1/ 3Mn1/3Co1/3O2The mol ratio of the Li, Mn, Ni and Co is 1.1-1.2: 0.33:0.33:0.33 and Li is replenished2SO4、MnSO4、NiSO4And CoSO4Then 0.5mol/L of Na is added2CO3Solution, Na2CO3The amount of the solution is such that Na2CO3With respect to the molar amount of LiNi per mole1/3Mn1/3Co1/3O2The molar weight ratio of the total metals in the reaction is 1.3, and the reaction is carried out for 2 hours. Filtering the turbid solution, washing precipitates for a plurality of times by using deionized water, measuring the cobalt and manganese content in the filtrate, and calculating the precipitation rates of the cobalt and manganese to be 93.1% and 99.3% respectively by using a difference value; the washed precipitate was transferred to an oven and dried at 100 ℃ overnight. Ball milling the dried block for 1h by using a ball mill, pressing the obtained powder on an oil press into a round piece of about 0.5g, putting the round piece into a corundum boat, transferring the corundum boat into a muffle furnace, and calcining at 5 ℃ for min-1The temperature is programmed to 900 ℃, and then the temperature is maintained at 900 ℃ for 12 hours, and the black solid powder ternary cathode material LiNi is obtained1/3Mn1/3Co1/3O2。
LiNi prepared in this example1/3Mn1/3Co1/3O2XRD was performed, and as shown in FIG. 2, the XRD result showed that the synthesized sample was LiNi1/3Mn1/3Co1/3O2This is consistent with literature reports (Shaju K M, Subba Rao G V, Chowdari B VR. Performance of layered Li (Ni)1/3Co1/3Mn1/3)O2as cathode for Li-ion batteries[J].Electrochimica Acta,2002,48(2):145-151.)。
LiNi prepared in this example1/3Mn1/3Co1/3O2SEM scanning was performed, and LiNi was shown in FIG. 31/3Mn1/3Co1/3O2The particle size of the material is about 5-15 μm.
TABLE 1 content of metals in leachate
Example 2
Adding a mixed solution of sulfuric acid and hydrogen peroxide into PTA oxidation section residues, wherein the concentration of the sulfuric acid in the mixed solution is 2mol/L, H2O2Leaching with a mass concentration of 25% to obtain a leachate, and performing ICP (inductively coupled plasma) test on 5ml of the leachate to obtain metal contents shown in Table 1. As can be seen from Table 1, Co is used in the solution2+And Mn2+Mainly with a small amount of Fe3+、Ni2+And Ca2+. Adding Na firstly2CO3Adjusting the pH to 2-4 to obtain Fe3+Formation of Fe (OH)3Separating out, filtering and removing the precipitate; according to LiNi0.5Mn0.2Co0.3O2The mol ratio of the Li, Mn, Ni and Co is 1.1-1.2: 0.5:0.2:0.3 and LiNO is supplemented3、Mn(NO3)2、Ni(NO3)2And Co (NO)3)2Then adding 1.0mol/L Na2CO3Solution, Na2CO3The amount of the solution is such that Na2CO3With respect to the molar amount of LiNi per mole0.5Mn0.2Co0.3O2The molar weight ratio of the total metals in the reaction is 1.1, and the reaction is carried out for 2 hours. Filtering the turbid solution, washing precipitates for a plurality of times by using deionized water, measuring the cobalt and manganese content in the filtrate, and calculating the precipitation rates of the cobalt and manganese to be 92.7 percent and 98.2 percent respectively by using a difference value; the washed precipitate was transferred to an oven and dried at 80 ℃ overnight. Ball milling the dried block for 1h by using a ball mill, spreading the obtained powder in a corundum boat, transferring the corundum boat to a muffle furnace for calcination, and performing calcination at 5 ℃ for min-1The temperature is programmed to 850 ℃, and then the temperature is kept for 10 hours at 850 ℃, thus obtaining the black solid powder ternary cathode material LiNi0.5Mn0.2Co0.3O2The SEM image is shown in FIG. 4.
Example 3
Adding a mixed solution of sulfuric acid and hydrogen peroxide into PTA oxidation section residues, wherein the concentration of sulfuric acid in the mixed solution is 5mol/L, H2O2Leaching with a mass concentration of 40% to obtain a leachate, and performing ICP (inductively coupled plasma) test on 5ml of the leachate to obtain metal contents shown in Table 1. As can be seen from Table 1, Co is used in the solution2+And Mn2+Mainly with a small amount of Fe3+、Ni2+And Ca2+. Adding Na firstly2CO3Adjusting the pH to 2-4 to obtain Fe3+Formation of Fe (OH)3Separating out, filtering and removing the precipitate; according to LiNi1/3Mn1/3Co1/3O2The mol ratio of the Li, Mn, Ni and Co is 1.1-1.2: 0.33:0.33:0.33 and CH is supplemented3COOLi、Mn(COOCH3)2、Ni(COOCH3)2And Co (COOCH)3)2Then 2.0mol/L of Na is added2CO3Solution, Na2CO3The amount of the solution is such that Na2CO3With respect to the molar amount of LiNi per mole1/3Mn1/3Co1/3O2The molar weight ratio of the total metals in the reaction is 1.5, and the reaction is carried out for 2 hours. Filtering the turbid solution, washing precipitates for a plurality of times by using deionized water, measuring the cobalt and manganese content in the filtrate, and calculating the precipitation rates of the cobalt and manganese to be 93.5 percent and 98.9 percent respectively by using a difference value; the precipitate was transferred to an oven and baked at 110 ℃ overnight. Dried block shapeBall milling the mixture for 1h with a ball mill, spreading the obtained powder in a corundum boat, transferring the corundum boat to a muffle furnace for calcination, and performing calcination at 5 ℃ for min-1The temperature is programmed to 950 ℃, and then the temperature is maintained at 950 ℃ for 11 hours, and the black solid powder ternary cathode material LiNi is obtained1/3Mn1/3Co1/3O2The SEM image is shown in FIG. 5.
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 (9)
1. A preparation method for preparing a lithium ion cathode material by utilizing PTA oxidation section residues is characterized by comprising the following steps:
(1) adding a mixed solution of sulfuric acid and hydrogen peroxide into the PTA oxidation section residue to obtain a leaching solution;
(2) measuring the content of each metal in the leachate obtained in the step (1) by using an ICP (inductively coupled plasma) spectrometry or a titration method;
(3) adding Na according to the content of each metal determined in the step (2)2CO3Adjusting the pH value of the solution to 2-4 to enable Fe3+Formation of Fe (OH)3Separating out, filtering and removing the precipitate;
(4) according to the Co determined in the step (2)2+、Mn2+Concentration, adding Co2+、Mn2+、Ni2+、Li+According to the ternary positive electrode material LiNixMnyCozO2Determining the addition amount of soluble salt by x, y and z values in the solution, and adding Na2CO3Filtering the solution, precipitating, washing and drying;
(5) ball-milling the solid obtained after drying in the step (4), and then calcining in the air atmosphere to obtain the black solid powder ternary cathode material LiNixMnyCozO2。
2. The method for preparing the lithium ion cathode material by utilizing the PTA oxidation section residue as claimed in claim 1, wherein the concentration of sulfuric acid in the mixed solution in the step (1) is 2-5mol/L, and the mass concentration of hydrogen peroxide is 25% -40%.
3. The method for preparing lithium ion cathode material by using PTA oxidation stage residue as claimed in claim 1, wherein the Co in step (4) is used2+、Mn2+、Ni2+、Li+The soluble salt of (A) is Co2+、Mn2+、Ni2+、Li+One or more of sulfate, nitrate or acetate.
4. The method for preparing lithium ion cathode material from PTA oxidation stage residue as claimed in claim 1, wherein Na is added in step (4)2CO3The amount of the solution is such that Na2CO3The ratio of the molar amount of (B) to the total metal molar amount is 1.1-1.5.
5. The method for preparing the lithium ion cathode material by using the PTA oxidation stage residue as claimed in claim 1, wherein the washing in the step (4) is performed several times by using deionized water; the drying temperature is 80-110 ℃, and the drying time is 24-36 h.
6. The method for preparing the lithium ion cathode material by using the PTA oxidation stage residue as claimed in claim 1, wherein the ball milling time in the step (5) is 1 h; the calcining temperature is 850-950 ℃, and the calcining time is 8-12 h.
7. The method for preparing the lithium ion cathode material by using the PTA oxidation stage residue as claimed in claim 1, wherein the ternary cathode material LiNi isxMnyCozO2Middle 0<x<2/3,0<y<2/3,0<z<2/3,x+y+z＝1。
8. The method for preparing the lithium ion cathode material by using the PTA oxidation stage residue as claimed in claim 6, wherein x is 1/3, y is 1/3, and z is 1/3.
9. The method for preparing the lithium ion cathode material by using the PTA oxidation stage residue as claimed in claim 1, wherein the ternary cathode material LiNi isxMnyCozO2Has a particle diameter of 5-15 μm.
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