Method for extracting aluminum, silicon oxide and rare earth from waste rare earth polishing powder

A rare earth polishing powder, silicon oxide technology, applied in the directions of silicon oxide, silicon dioxide, polishing compositions containing abrasives, etc., can solve the problems of incapable of industrialized production, inability to cover production costs, consumption, etc.

Active Publication Date: 2019-01-15
湖南景翌湘台环保高新技术开发有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, there are related patents on the recycling of waste rare earth polishing powder, such as the Chinese patent "Method for Extracting Rare Earth Oxides from Polishing Powder Waste" (publication number: 108531735A), which discloses the preparation of rare earth salts by acid leaching-extraction back-extraction-precipitation - The process of preparing rare earth oxides by burning rare earth salts, in the first step of acid leaching, due to the subsequent extraction, the acidity at the end of the leaching is low, which will lead to a low leaching rate of rare earths
At the same time, during acid leaching, after aluminum ions and rare earth ions enter the solution, because these two ions will be extracted at the same time during the extraction process, multi-stage extraction and separation are required, and the cost is high. At the same time, aluminum ions are likely to cause poisoning of the extractant, making the price The performance of the expensive extractant gradually declines until it fails, and the extractant needs to be saponified and consumes a large amount of sodium hydroxide, resulting in a high cost of the entire process. In actual production, it is difficult to realize industrial production due to cost problems; Chinese patent "A method for preparing lanthanum cerium oxalate from waste rare earth polishing powder" (publication number: 102659559B) discloses that lanthanum cerium oxalate is obtained by sulfuric acid leaching and oxalic acid precipitation, but the aluminum in waste rare earth polishing powder is neutralized Mixed with gypsum, aluminum resources are not fully utilized; the Chinese patent "A Method for Clear and Segmented Recovery of Rare Earth Elements from Rare Earth Polishing Powder Waste Slag" (publication number: 104060111A) discloses a method for segmental recovery of rare earth elements In the second stage of recovery, concentrated sulfuric acid is used for leaching to produce ceric sulfate, but in the first stage, lanthanum and praseodymium are preferentially dissolved with low-concentration hydrochloric acid, and about 30% of cerium will enter the leach solution. There are lanthanum ions, cerium ions, aluminum ions in the solution. Ions and praseodymium ions have complex components, and it is difficult to separate lanthanum and cerium. Concentrated sulfuric acid is used for further dissolution to produce ceric sulfate, which is reprecipitated and burned to obtain cerium oxide. However, in practice, the leachate is a mixture of lanthanum sulfate and cerium sulfate, and the separation cost High, does not meet the conditions for industrialization
[0005] The existing technology lacks the overall idea of ​​completely separating silicon oxide, aluminum and rare earth in the waste rare earth polishing powder and transforming them into three products. Therefore, the production cost cannot be covered due to lack of full utilization of resources in process design and product design. , resulting in the inability to industrialize production, and can only stay in the laboratory stage. For example, when acid is used in the first stage, due to concerns about the cost of subsequent wastewater treatment, the amount of acid (sulfuric acid, hydrochloric acid, or nitric acid, etc.) cannot be excessively large, resulting in the first step The leaching rate of rare earth and aluminum is low and requires repeated leaching, the process route is long, the cost is high, and the additional impact caused by the insufficient amount of acid is that the content of rare earth in the leaching slag is too high, which not only causes waste of rare earth resources, but also causes leaching. The aluminum content in the slag is also too high, resulting in low silicon oxide content in the leached slag, which cannot be used and forms new solid waste

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] A method for extracting aluminum, silicon oxide and rare earth from waste rare earth polishing powder, comprising the following steps:

[0028] (1) Pretreatment process: remove the woven bags and other sundries in the waste rare earth polishing powder and crush them.

[0029] (2) Put the treated waste rare earth polishing powder into the reaction tank, add concentrated hydrochloric acid to react, the initial ratio of waste powder and hydrochloric acid is controlled at 1:4 by weight, and add concentrated hydrochloric acid during the reaction to control the entire During the reaction process, the content of hydrochloric acid is not less than 4M, maintain high acid leaching, and moderately heat, control the temperature at 100-110°C, and the reaction time is 2-4 hours.

[0030] (3) After the high-acid leaching is completed, filter and wash the filter cake to obtain silica leaching residue and leachate. The content of silica powder produced in this step is 60-64%.

[0031](...

Embodiment 2

[0039] (1) Pretreatment process: remove woven bags and other sundries in the waste rare earth polishing powder and crush them.

[0040] (2) Put the treated waste rare earth polishing powder into the reaction tank, add concentrated hydrochloric acid to react, the initial ratio of waste powder and hydrochloric acid is controlled at 1:6 by weight, and add concentrated hydrochloric acid during the reaction to control the entire During the reaction process, the content of hydrochloric acid is not less than 4M, maintain high acid leaching, and moderately heat, control the temperature at 100-140°C, and the reaction time is 3-4 hours.

[0041] (3) After the high-acid leaching is completed, filter and wash the filter cake to obtain silica leaching residue and leaching liquid. The content of silica powder produced in this step is 66-72%.

[0042] (4) Add water to the silicon oxide leaching slag to adjust the slurry, control the concentration of the slurry to 15-25%, and slowly pump it i...

Embodiment 3

[0050] A method for extracting aluminum, silicon oxide and rare earth from waste rare earth polishing powder, comprising the following steps:

[0051] (1) Pretreatment process: remove woven bags and other sundries in the waste rare earth polishing powder and crush them.

[0052] (2) Put the treated waste rare earth polishing powder into the reaction tank, add concentrated hydrochloric acid to react, the initial ratio of waste powder and hydrochloric acid is controlled at 1:5 by weight, and add concentrated sulfuric acid during the reaction to control the entire During the reaction process, the content of sulfuric acid is not less than 6M, maintain high acid leaching, and moderately heat, control the temperature at 120-180°C, and the reaction time is 2-4 hours.

[0053] (3) After the high-acid leaching is completed, filter and wash the filter cake to obtain silica leaching residue and leaching liquid. The content of silica powder produced in this step is 70-75%.

[0054] (4) A...

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Abstract

The invention discloses a method for extracting aluminum, silicon oxide and rare earth from waste rare earth polishing powder. The method comprises the following steps that (1) strong acid is added into the pretreated waste rare earth polishing powder, the aluminum and the rare earth are dissolved, and silicon oxide powder is left in leaching residues; (2) the leaching residues containing the silicon oxide powder are washed and purified so as to obtain the silicon oxide powder; (3) a precipitant is added into a leachate so as to precipitate the rare earth, and filtering is carried out so as toobtain a rare earth salt and an aluminum salt solution; (4) after the aluminum salt solution is neutralized, standing and settling are carried out for 2-12 hours so as to obtain an aluminum-containing product; and (5) the rare-earth salt is subjected to fluorination and is burnt so as to prepare rare earth polishing powder. According to the method, silicon, aluminum and the rare earth in the waste rare earth polishing powder are comprehensively recovered to form the superfine silicon oxide powder, the aluminum salt and the rare earth polishing powder, no solid waste is generated, and all valuable elements are utilized.

Description

technical field [0001] The invention belongs to the technical field of solid waste recycling, and in particular relates to a method for extracting aluminum, silicon oxide and rare earth from waste rare earth polishing powder. Background technique [0002] In recent years, with the rapid popularization and replacement of mobile phones and the widespread use of flat screens and automotive central control screens, more than 100,000 tons of waste rare earth polishing powder solid waste is produced every year. From the perspective of chemical composition, waste rare earth polishing powder The content of alumina in rare earth polishing powder is generally 15-25%, the content of silicon oxide is 30-60%, and the content of rare earth oxide is 15-50%. The polishing process is a process with a high degree of cleanliness. The rare earth polishing powder and optical glass used at the same time are all high-purity raw materials and components. The waste rare earth polishing powder produc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B7/00C22B59/00C22B21/00C01B33/18C09G1/02
CPCC01B33/18C09G1/02C22B7/007C22B21/0023C22B59/00Y02P10/20
Inventor 解付兵刘宜德翟海军曹莹周霜艳王鑫赵永曾宪军朱湘怀欧阳书径
Owner 湖南景翌湘台环保高新技术开发有限公司
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