CN111018223A - Method for realizing zero discharge of wastewater in process of producing rare earth chloride from monazite - Google Patents
Method for realizing zero discharge of wastewater in process of producing rare earth chloride from monazite Download PDFInfo
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- CN111018223A CN111018223A CN201911364314.9A CN201911364314A CN111018223A CN 111018223 A CN111018223 A CN 111018223A CN 201911364314 A CN201911364314 A CN 201911364314A CN 111018223 A CN111018223 A CN 111018223A
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B60/00—Obtaining metals of atomic number 87 or higher, i.e. radioactive metals
- C22B60/02—Obtaining thorium, uranium, or other actinides
- C22B60/0204—Obtaining thorium, uranium, or other actinides obtaining uranium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B60/00—Obtaining metals of atomic number 87 or higher, i.e. radioactive metals
- C22B60/02—Obtaining thorium, uranium, or other actinides
- C22B60/0291—Obtaining thorium, uranium, or other actinides obtaining thorium
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
- C02F1/048—Purification of waste water by evaporation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/16—Nature of the water, waste water, sewage or sludge to be treated from metallurgical processes, i.e. from the production, refining or treatment of metals, e.g. galvanic wastes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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Abstract
The invention belongs to the technical field of rare earth ore monazite smelting and wastewater treatment, and particularly relates to a method for realizing zero discharge of wastewater in the process of producing rare earth chloride from monazite. 5 kinds of process wastewater including mother liquor separated by trisodium phosphate crystallization, acid insoluble slag washing residual water, U-poor acidified water, Th extraction residual water phase and Th saturated pickling water do not enter a wastewater treatment system and are returned for use; uniformly feeding the iron-repellent precipitation mother liquor and Th lean acidified water into an acidic wastewater collecting tank; the U precipitation mother liquor and the Th reverse extraction precipitation mother liquor enter an alkaline wastewater collecting tank; acid wastewater and alkaline wastewater flow together into a neutralization tank, pH is adjusted to be within the range of 10.5-12 by adding lime milk, uranium and thorium elements are fully precipitated, finally, the wastewater is evaporated to dryness, and residues are sealed and stored. The invention directly recycles the waste water with use value in the process or recycles the waste water after treatment, and a small amount of waste water without use value is evaporated to dryness by a multi-effect evaporator, thereby finally realizing the purpose of zero discharge of the waste water.
Description
Technical Field
The invention belongs to the technical field of rare earth ore monazite smelting and wastewater treatment, and particularly relates to a method for realizing zero discharge of wastewater in the process of producing rare earth chloride from monazite.
Background
Monazite is one of the most widely distributed and important rare earth minerals, is rich in rare earth, uranium, thorium and other precious resources, and has a chemical expression of (Ce, La and Th) PO4. For a long time, monazite concentrates have been used mainly for the extraction of rare earths and phosphorus, the wastes of which are produced during the conventional processThe water is generally treated by neutralization, biochemical treatment, flocculation, filtration and the like to reach the national discharge standard of industrial wastewater. The preferential dissolving slag after the monazite is used for extracting the rare earth chloride and the phosphorus is generally treated in a landfill or warehouse entry and sealing mode. A Limited liability company of the original new nuclear gold material in Hunan comprehensively recovers uranium-thorium resources from the excellent molten slag, and belongs to the first time in China, and a main process and a wastewater treatment process of the limited liability company do not have reference and reference points.
Disclosure of Invention
The invention aims to provide a method for realizing zero discharge of wastewater in the process of producing rare earth chloride from monazite, which classifies, utilizes and treats the wastewater and finally achieves the aim of zero discharge of the wastewater.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a method for zero discharge of wastewater in the process of producing rare earth chloride from monazite comprises the following steps of 5 process wastewater including mother liquor separated by crystallization of trisodium phosphate, acid-insoluble slag washing residual water, U-lean acidified water, Th extraction residual water phase and Th saturated pickling water, which do not enter a wastewater treatment system and are returned to be used; uniformly feeding the iron-repellent precipitation mother liquor and Th lean acidified water into an acidic wastewater collecting tank; the U precipitation mother liquor and the Th reverse extraction precipitation mother liquor enter an alkaline wastewater collecting tank; acid wastewater and alkaline wastewater flow together into a neutralization tank, pH is adjusted to be within the range of 10.5-12 by adding lime milk, uranium and thorium elements are fully precipitated, finally, the wastewater is evaporated to dryness, and residues are sealed and stored.
Acid wastewater and alkaline wastewater flow into a neutralization tank together in a ratio of 1: 1.
and finally, discharging the wastewater into a multi-effect evaporator to be dried by distillation, and sealing the slag in a tailing pond.
The beneficial effects obtained by the invention are as follows:
the invention directly recycles the waste water with use value in the process or recycles the waste water after treatment, and a small amount of waste water without use value is evaporated to dryness by a multi-effect evaporator, thereby finally realizing the purpose of zero discharge of the waste water. The whole production process meets the requirement of environmental protection.
Drawings
FIG. 1 is a flow chart of a method for zero discharge of wastewater in the process of producing rare earth chloride from monazite.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments.
As shown in figure 1, the method for zero discharge of wastewater in the process of producing rare earth chloride from monazite comprises the following steps: 9 kinds of process wastewater are generated in the process of producing rare earth chloride from monazite and comprehensively recovering uranium-thorium resources, and the process wastewater is respectively treated in the following modes: the method comprises the following steps of (1) separating mother liquor by crystallization of trisodium phosphate, washing residual water of acid-insoluble slag, U-lean acidified water, Th extraction water phase, Th saturated pickling water and other 5 kinds of process wastewater, wherein the components of the wastewater are relatively clean or the magazine components are similar to the properties of system materials, and the wastewater in the intermediate process does not enter a wastewater treatment system and can be returned to the system for use or returned for use after treatment; uniformly feeding the iron-repellent precipitation mother liquor and Th lean acidified water (part of the Th lean acidified water) into an acidic wastewater collecting tank; the U precipitation mother liquor and the Th reextraction precipitation mother liquor (part of the U precipitation mother liquor and the Th reextraction precipitation mother liquor) enter an alkaline wastewater collecting tank; acid wastewater and alkaline wastewater flow together into a neutralization tank (the proportion is adjustable and is usually 1: 1), and the pH is adjusted to be in the range of 10.5-12 by adding lime milk, so that the uranium-thorium element is fully precipitated (CaU)2O7、U(OH)4) Finally, the waste water is discharged into a multi-effect evaporator to be dried by distillation, and the slag enters a tailing warehouse to be sealed and stored. The whole process has no wastewater discharge, and the aims of environmental protection and clean production are fulfilled.
The invention provides a process for zero discharge of wastewater. The process for producing rare earth chloride by decomposing monazite with alkali and dissolving monazite with hydrochloric acid has been in practical use in the domestic rare earth industry for many years. Environmental protection pressure of the generated optimal-solution slag due to enrichment of uranium and thorium elements is increasingly shown, and the uranium and the thorium have great recycling values as strategic national resources. The invention is established on the project of monazite production rare earth chloride and comprehensive recovery of uranium-thorium resource of the limited liability company of the nuclear gold raw new material in Hunan, and adopts a brand new process to comprehensively utilize and treat various waste water generated in the production process, thereby finally achieving the purpose of zero emission. In general, 9 kinds of process wastewater are generated in the process of producing rare earth chloride from monazite and comprehensively recovering uranium thorium resources,the respective treatment modes are as follows: the method comprises the following steps of (1) separating mother liquor by crystallization of trisodium phosphate, washing residual water of acid-insoluble slag, U-lean acidified water, Th extraction water phase, Th saturated pickling water and other 5 kinds of process wastewater, wherein the components of the wastewater are relatively clean or the magazine components are similar to the properties of system materials, and the wastewater in the intermediate process does not enter a wastewater treatment system and can be returned to the system for use or returned for use after treatment; uniformly feeding the iron-repellent precipitation mother liquor and Th lean acidified water (part of the Th lean acidified water) into an acidic wastewater collecting tank; the U precipitation mother liquor and the Th reextraction precipitation mother liquor (part of the U precipitation mother liquor and the Th reextraction precipitation mother liquor) enter an alkaline wastewater collecting tank; acid wastewater and alkaline wastewater flow together into a neutralization tank (the proportion is adjustable and is usually 1: 1), and the pH is adjusted to be in the range of 10.5-12 by adding lime milk, so that the uranium-thorium element is fully precipitated (CaU)2O7、U(OH)4) Finally, the waste water is discharged into a multi-effect evaporator to be dried by distillation, and the slag enters a tailing warehouse to be sealed and stored. The whole process has no wastewater discharge, and the aims of environmental protection and clean production are fulfilled.
The invention finally realizes the purpose of zero discharge of wastewater through the in-process recycling of a process wastewater system, the respective collection of acid-base wastewater, the neutralization of the acid-base wastewater, the pH adjustment of lime milk, the precipitation of radioactive elements such as uranium, thorium and the like, and multiple-effect evaporation; after desiliconization treatment, returning to alkali for decomposition; washing residual water by acid-insoluble residues, and completely returning to complete dissolution to prepare hydrochloric acid; u is poor in acidified water, about 80 percent of the U is recycled, and about 20 percent of the U returns to the full-solution section; returning the Th raffinate water phase to preferential dissolution to recover rare earth chloride, irregularly adjusting the pH to 4.5 by using an alkali adding cake, removing metal ions such as U, Th, Fe, Al, Zr, Ti, Sn and the like, and discarding slag; the Th saturated pickling water returns to the hydrochloric acid preferential dissolution section; all the iron reaction agent precipitation mother liquor enters an acid wastewater collection tank; th is poor in acidified water and recycled, and about 10% of the Th is poor in acidified water and enters an acidic wastewater collecting tank; the U precipitation mother liquor enters an alkaline wastewater collecting tank; and (3) returning 76% of the Th back-extraction precipitation mother liquor to a system for utilization, and feeding the rest 24Th precipitation mother liquor into an alkaline wastewater collecting tank. Acid wastewater and alkaline wastewater are converged and enter a neutralization tank according to a proportion, certain lime milk is added, the pH is adjusted to 10.5-12, and radioactive elements such as uranium, thorium and the like are precipitated. And finally, the wastewater enters a multi-effect evaporator to be dried by distillation, and the residual slag enters a tailing warehouse to be sealed and stored.
Example 1
1t monazite provided by a rare earth enterprise in Hunan province is used for treating wastewater in the following way:
acid wastewater and alkaline wastewater are converged and enter a neutralization tank according to a certain proportion, certain lime milk (16 percent by mass) is added, the pH is adjusted to 10.5-12, and radioactive elements such as uranium, thorium and the like are precipitated. The waste water after radioactive element precipitation enters a multi-effect evaporator to be evaporated to dryness, and the residual slag enters a tailing pond to be sealed and stored. Example results: the aim of zero discharge of waste water is fulfilled.
Example 2
1t monazite provided by a rare earth enterprise in Jiangxi treats wastewater in the way of the embodiment 1, and the aim of zero discharge of wastewater is fulfilled.
Claims (3)
1. A method for realizing zero discharge of wastewater in the process of producing rare earth chloride from monazite is characterized by comprising the following steps: 5 kinds of process wastewater including mother liquor separated by trisodium phosphate crystallization, acid insoluble slag washing residual water, U-poor acidified water, Th extraction residual water phase and Th saturated pickling water do not enter a wastewater treatment system and are returned for use; uniformly feeding the iron-repellent precipitation mother liquor and Th lean acidified water into an acidic wastewater collecting tank; the U precipitation mother liquor and the Th reverse extraction precipitation mother liquor enter an alkaline wastewater collecting tank; acid wastewater and alkaline wastewater flow together into a neutralization tank, pH is adjusted to be within the range of 10.5-12 by adding lime milk, uranium and thorium elements are fully precipitated, finally, the wastewater is evaporated to dryness, and residues are sealed and stored.
2. The method for realizing zero discharge of wastewater in the process of producing rare earth chloride from monazite according to claim 1, which is characterized in that: acid wastewater and alkaline wastewater flow into a neutralization tank together in a ratio of 1: 1.
3. the method for realizing zero discharge of wastewater in the process of producing rare earth chloride from monazite according to claim 1, which is characterized in that: and finally, discharging the wastewater into a multi-effect evaporator to be dried by distillation, and sealing the slag in a tailing pond.
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| CN201911364314.9A CN111018223A (en) | 2019-12-26 | 2019-12-26 | Method for realizing zero discharge of wastewater in process of producing rare earth chloride from monazite |
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| CN201911364314.9A CN111018223A (en) | 2019-12-26 | 2019-12-26 | Method for realizing zero discharge of wastewater in process of producing rare earth chloride from monazite |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB674400A (en) * | 1949-07-21 | 1952-06-25 | Produits Chim Terres Rares Soc | Treatment of monazite |
| US20100018347A1 (en) * | 2006-10-05 | 2010-01-28 | Holden Charles S | Separation of radium and rare earth elements from monazite |
| CN102491554A (en) * | 2011-12-01 | 2012-06-13 | 核工业北京化工冶金研究院 | Method for treating alkali wastewater containing uranium |
| CN105906099A (en) * | 2016-06-08 | 2016-08-31 | 长沙赛恩斯环保科技有限公司 | Rapid treating method for rare earth radioactive wastewater |
| CN109607909A (en) * | 2018-11-27 | 2019-04-12 | 核工业北京化工冶金研究院 | A kind of high ammonia nitrogen uranium containing manganese wastewater treatment method |
-
2019
- 2019-12-26 CN CN201911364314.9A patent/CN111018223A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB674400A (en) * | 1949-07-21 | 1952-06-25 | Produits Chim Terres Rares Soc | Treatment of monazite |
| US20100018347A1 (en) * | 2006-10-05 | 2010-01-28 | Holden Charles S | Separation of radium and rare earth elements from monazite |
| CN102491554A (en) * | 2011-12-01 | 2012-06-13 | 核工业北京化工冶金研究院 | Method for treating alkali wastewater containing uranium |
| CN105906099A (en) * | 2016-06-08 | 2016-08-31 | 长沙赛恩斯环保科技有限公司 | Rapid treating method for rare earth radioactive wastewater |
| CN109607909A (en) * | 2018-11-27 | 2019-04-12 | 核工业北京化工冶金研究院 | A kind of high ammonia nitrogen uranium containing manganese wastewater treatment method |
Non-Patent Citations (3)
| Title |
|---|
| 张建国等: "某铀矿山酸性工艺废水处理研究", 《铀矿冶》 * |
| 方星等: "《矿山土地复垦理论与方法》", 31 August 2015, 地质出版社 * |
| 潘自强: "《中国裂变核能矿产资源可持续发展战略研究》", 30 April 2016, 中国原子能出版社 * |
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