Search

KR-20260062252-A - Manufacturing Method Of Cathode Powder, Ceramic Powder, And Lithium Carbonate From A Waste Sintering Vessel

KR20260062252AKR 20260062252 AKR20260062252 AKR 20260062252AKR-20260062252-A

Abstract

The present invention relates to a method for recycling waste calcination containers (waste refractory containers) discarded after calcining cathode materials. Using the present invention, lithium carbonate can be precipitated on the surface of the waste calcination container through immersion and drying, and the lithium carbonate and cathode material powder can be obtained and recycled through delamination. Additionally, the waste calcination container from which the lithium carbonate and cathode material powder have been removed can be crushed and recycled as a ceramic raw material. Furthermore, crude lithium carbonate can be produced by performing a carbonation reaction on the leachate from the immersion container.

Inventors

  • 이정미
  • 이준섭
  • 배효진
  • 송영준

Assignees

  • 한국광해광업공단

Dates

Publication Date
20260507
Application Date
20241028

Claims (8)

  1. Step 1 of preparing the waste plastic container; A second step of immersing the above-mentioned closed firing container in a water tank; A third step of draining the leachate from the above tank to obtain a dehydrated waste calcination vessel; Step 4: Drying the above-mentioned dehydrated waste calcined container; A fifth step of obtaining anode material powder by detaching it from the surface of the above-described dried waste firing container; and Step 6, crushing the waste firing container from which the anode powder has been detached to obtain ceramic powder; A method for recycling waste plastic containers including
  2. A method for recycling waste calcined containers according to claim 1, characterized in that a carbonate aqueous solution or carbon dioxide gas is injected into the leachate of the third stage to precipitate lithium carbonate, and the filtrate obtained by solid-liquid separation is supplied to the water tank of the second stage and used for the water immersion of the waste calcined container.
  3. A method for recycling waste calcined containers according to claim 1, characterized in that the detachment is performed by spraying an abrasive agent at high pressure.
  4. A method for recycling waste calcined containers according to claim 1, wherein the cathode material powder comprises 1 to 10 wt% Li₂O , 5 to 50 wt% Al₂O₃ , 5 to 30 wt% SiO₂, 1 to 15 wt% MgO, 5 to 80 wt% NiO, 1 to 10 wt% MnO, and 1 to 10 wt% Co₂O₃ .
  5. A method for recycling waste calcined containers according to claim 1, wherein the ceramic powder comprises 45 to 65 wt% Al₂O₃ , 20 to 40 wt% SiO₂ , 5 to 20 wt% MgO, 0 to 0.05 wt% NiO , 0 to 0.5 wt% Li₂O, 0 to 0.02 wt% MnO , and 0 to 0.01 wt% Co₂O₃ .
  6. Step 1 of preparing the waste plastic container; A second step of immersing the above-mentioned closed firing container in a water tank; A third step of obtaining leachate from the above tank; A fourth step of injecting an aqueous carbonate solution or carbon dioxide into the above leachate to obtain leachate in which lithium carbonate is precipitated; and Step 5, obtaining solid crude lithium carbonate by separating the solid and liquid phases of the leachate in which the lithium carbonate is precipitated; A method for recycling waste plastic containers including
  7. A method for recycling waste calcined containers according to claim 6, characterized in that the filtrate obtained from the solid-liquid separation of the fifth step is supplied to the water tank of the second step and used for the immersion of the waste calcined container.
  8. A method for recycling waste calcined containers according to claim 6, characterized in that the lithium carbonate has a lithium purity of 50 to 99%.

Description

Manufacturing Method of Cathode Powder, Ceramic Powder, and Lithium Carbonate From a Waste Sintering Vessel The present invention relates to a method for producing cathode material powder, ceramic powder, and lithium carbonate from a waste calcination container. The box-shaped firing vessel (crucible) used in the process of firing cathode materials is called a saggar. Alumina crucibles with an increased MgO content of 10 to 20% are widely used to enhance corrosion resistance against strongly alkaline lithium hydroxide. During the repeated firing of cathode materials, the surface of the aforementioned firing vessel becomes damaged, leaving a significant amount of cathode material residue on the damaged surface. Since this residue contains heavy metals such as nickel, cobalt, and manganese that are harmful to the human body, all of these must be removed in accordance with environmental standards to dispose of the spent firing vessels; failure to do so results in excessive impurities, which limits the possibility of recycling. Although methods have been developed to recover valuable metals such as lithium, nickel, and cobalt from spent firing vessels through chemical processes like acid leaching and to recycle the residues as ceramic raw materials, these processes are limited to simple disposal at low cost due to excessive initial investment costs. The patent documents and references mentioned in this specification are incorporated by reference into this specification to the same extent that each document is individually and clearly identified by reference. FIG. 1 shows a waste firing container of the present invention. FIG. 2 shows a method for obtaining cathode material powder, ceramic powder, and lithium carbonate by recycling waste calcination containers of the present invention. FIG. 3 shows an erosion layer formed on a closed calcination vessel of the present invention and lithium carbonate particles precipitated on the surface of a water-immersed closed calcination vessel. Figure 4 shows the result of detaching the waste firing container of the present invention. Figure 5 shows the lithium carbonate of the present invention. The present invention relates to a method for obtaining cathode material powder, ceramic powder, and lithium carbonate by recycling waste calcination containers (waste refractory containers). The present invention provides a method for detoxifying waste calcination containers at a low cost while simultaneously recovering discarded resources. The firing vessel (refractory casing) of the present invention is composed mainly of Al₂O₃ , SiO₂ , and MgO , and is contained in amounts of 35 to 60 wt%, 25 to 50 wt%, and 5 to 20 wt%, respectively. Table 1 below shows the composition (wt%) of the firing vessel of the present invention. ingredientFiring vessel 1Firing vessel 2Firing vessel 3Firing vessel 4Firing vessel 5Firing vessel 6Firing vessel 7Firing vessel 8Al₂O₃​56.5152.5656.3455.3754.7755.9652.2555.53SiO228.2425.9831.1931.7231.1830.5933.3028.82MgO12.6914.9210.1010.4610.6110.8310.6913.25CaO0.620.580.420.450.320.400.340.51K 2 O0.150.150.200.210.200.220.240.22Na₂O0.180.290.250.230.230.220.230.15NiO0.212.160.050.131.100.220.300.06MnO0.061.170.010.010.010.080.010.02Co3O4​0.030.82ND0.010.100.070.020.01etc1.311.371.441.411.481.412.621.43total100100100100100100100100 FIG. 1 shows the waste calcination container of the present invention. In the present invention, the waste calcination container discarded after calcining the cathode material using regular calcination containers 1 to 8 is collected to obtain cathode material powder, ceramic powder, and crude lithium carbonate. FIG. 2 shows a method for obtaining cathode material powder, ceramic powder, and crude lithium carbonate by recycling the waste calcination container of the present invention. 1. Method for obtaining cathode material powder and ceramic powder by recycling waste firing containers The present invention provides a method for recycling waste calcined containers to obtain anode material powder and ceramic powder, comprising the following steps: Step 1: a step of preparing a waste firing vessel; Step 2: a step of immersing the waste firing vessel in water in a water tank; Step 3: a step of draining leachate from the water tank to obtain a dehydrated waste firing vessel; Step 4: a step of drying the dehydrated waste firing vessel; Step 5: a step of detaching and obtaining anode material powder from the surface of the dried waste firing vessel; and Step 6: a step of crushing the waste firing vessel from which the anode material powder has been detached to obtain ceramic powder. The first step of the method for obtaining cathode material powder and ceramic powder by recycling the above-mentioned waste calcination container is to prepare the waste calcination container. The above-mentioned waste calcination container refers to a crucible used to calcine cathode materials such as NCM. Since cathode materials composed of nickel, cobalt