CN107520063B - Preparation method and application of rare earth ore flotation collector - Google Patents
Preparation method and application of rare earth ore flotation collector Download PDFInfo
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- CN107520063B CN107520063B CN201710941687.2A CN201710941687A CN107520063B CN 107520063 B CN107520063 B CN 107520063B CN 201710941687 A CN201710941687 A CN 201710941687A CN 107520063 B CN107520063 B CN 107520063B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D1/00—Flotation
- B03D1/001—Flotation agents
- B03D1/018—Mixtures of inorganic and organic compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D2201/00—Specified effects produced by the flotation agents
- B03D2201/02—Collectors
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D2203/00—Specified materials treated by the flotation agents; specified applications
- B03D2203/02—Ores
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- Inorganic Chemistry (AREA)
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Abstract
The invention provides a preparation method and application of a rare earth ore flotation collector, and belongs to the technical field of ore dressing. The preparation method comprises the following steps: (1) the method comprises the following steps of (1) mixing illegal cooking oil, methanol and concentrated sulfuric acid in a mass ratio: methanol: 1.0-1.2% of concentrated sulfuric acid: 1.1-1.8: 0.05-0.09, stirring and reacting for 5-12 hours at the temperature of 60-90 ℃ to obtain a product 1; (2) the preparation method comprises the following steps of (1) mixing hydroxylamine hydrochloride, water and sodium hydroxide according to the mass ratio: water: 1.0 to 1.3% of sodium hydroxide: 6.4-9.3: 1.9-2.4, stirring and reacting for 1-3 hours at 20-30 ℃ to obtain a product 2; (3) and (3) mixing the product 1 with the product 1: and (3) the product 2 is 1.0-1.2: and (3) adding 0.28-0.48 of the obtained product into the product 2, and stirring and reacting for 4-6 hours at the temperature of 40-60 ℃ to obtain the collecting agent. The invention relates to a rare earth ore efficient flotation collector, which solves the problems of complex production process flow and unsatisfactory rare earth ore concentrate grade and recovery rate indexes caused by high cost, poor selectivity and difficult operation in production of the conventional flotation collector.
Description
Technical Field
The invention relates to the technical field of mineral separation, in particular to a preparation method and application of a rare earth ore flotation collector.
Background
Rare earth is widely distributed in the earth crust, and the rare earth is in various types, and more than 250 types of rare earth-containing minerals are found. However, only a dozen kinds of minerals having industrial value include monazite, bastnaesite, bastnasite, beryllite, ytalite, aurite, xenotime, limonitite, etc., among which monazite, bastnaesite and xenotime are the most important and the most productive 3 kinds of rare earth minerals. The rare earth resource reserves in China are rich, and according to the data published by the Federal geological survey bureau in 2010 and 2014, the rare earth resource reserves in China are 5500 ten thousand tons and account for about 40-50% of the total reserves in the world. The rare earth resources in China are mainly distributed in inner Mongolia, Sichuan, Jiangxi, Shuangguang, Fujian and the like, wherein the Bayunebo iron-rare earth ore deposit is the ore deposit which has been found out in China to have the largest resource amount, and the resource amount accounts for about 96 percent of the total amount of the whole country. In industrial production, flotation is one of the most common and most effective methods for sorting rare earth ores, wherein a flotation collector is a key factor influencing the flotation effect. At present, hydroximic acid collecting agents are mainly used for flotation of rare earth ores, but the conventional hydroximic acid collecting agents have the defects of high cost, poor selectivity and collecting performance and high medicament toxicity. Therefore, research and development of novel efficient flotation collectors are of great significance to development and utilization of rare earth ore resources and sustainable development of related industries.
Disclosure of Invention
The invention provides a preparation method and application of a rare earth ore flotation collector, aiming at the problems of high cost, poor selectivity and collecting property, high medicament toxicity and the like of the collector in the existing rare earth ore flotation.
The preparation method comprises the following steps:
(1) the method comprises the following steps of (1) mixing illegal cooking oil, methanol and concentrated sulfuric acid in a mass ratio: methanol: 1.0-1.2% of concentrated sulfuric acid: 1.1-1.8: 0.05-0.09, stirring and reacting for 5-12 hours at the temperature of 60-90 ℃ to obtain a product 1;
(2) the preparation method comprises the following steps of (1) mixing hydroxylamine hydrochloride, water and sodium hydroxide according to the mass ratio: water: 1.0 to 1.3% of sodium hydroxide: 6.4-9.3: 1.9-2.4, stirring and reacting for 1-3 hours at 20-30 ℃ to obtain a product 2;
(3) and (3) mixing the product 1 with the product 1: and (3) the product 2 is 1.0-1.2: and 0.28-0.48, adding the mixture into the product 2, and stirring and reacting for 4-6 hours at 40-60 ℃ to obtain the rare earth ore flotation collector.
The process of carrying out the rare earth ore flotation by using the prepared collecting agent comprises the following steps:
firstly, grinding raw ore rare earth ore until monomer is dissociated, then adding an inhibitor, adding the collecting agent obtained in the step (3), and finally adding a foaming agent to collect the rare earth ore, wherein the total using amount of the collecting agent is as follows: 1000 to 9000 g/t.
Wherein the pH value of the flotation pulp is 8-13, and the pH value of the pulp is adjusted by sodium carbonate or sodium hydroxide.
The inhibitor is water glass, and the total dosage of the water glass is 2000-8000 g/t.
The foaming agent is one of No. 2 oil or methyl isobutyl carbinol, and the total consumption of the foaming agent is 60-600 g/t.
In the flotation process, the used collecting agent is added by using stock solution.
The technical scheme of the invention has the following beneficial effects:
in the scheme, the raw materials are wide in source, the production process is simple, the dispersibility is good, the environment is friendly, and the method has the following specific advantages:
(1) the raw material swill-cooked dirty oil has wide sources and low cost, and the production process can fully utilize the swill-cooked dirty oil threatening the environment and food safety, thereby realizing the dual effects of pollution control and comprehensive utilization;
(2) the production process is simple, belongs to a green and environment-friendly process, is easy to realize industrialization, and has wide application prospect;
(3) the collecting agent has good selectivity, good dispersibility and small influence of temperature, is easy to dissolve in water, has good separation effect at normal temperature, and can reach excellent flotation indexes.
Detailed Description
In order to make the technical problems, technical solutions and advantages to be solved by the present invention clearer, the following detailed description is given with reference to specific embodiments.
The invention provides a preparation method and application of a rare earth ore flotation collector, aiming at the problems of high cost, poor selectivity and collecting property, high medicament toxicity and the like of the existing collector in the rare earth ore flotation.
Example 1
One example of the preparation method of the rare earth ore flotation collector comprises the following steps:
(1) the method comprises the following steps of (1) mixing illegal cooking oil, methanol and concentrated sulfuric acid in a mass ratio: methanol: concentrated sulfuric acid is 1.0: 1.1: 0.05, stirring and reacting for 5 hours at the temperature of 60 ℃ to obtain a product 1;
(2) the preparation method comprises the following steps of (1) mixing hydroxylamine hydrochloride, water and sodium hydroxide according to the mass ratio: water: sodium hydroxide ═ 1.0: 6.4: 1.9, stirring and reacting for 1 hour at the temperature of 20 ℃ to obtain a product 2;
(3) and (3) mixing the product 1 with the product 1: product 2 ═ 1.0: 0.28, adding the mixture into the product 2, and stirring and reacting for 4 hours at 40 ℃ to obtain the rare earth ore flotation collector.
Example 2
Another example of the preparation method of the rare earth ore flotation collector comprises the following steps:
(1) the method comprises the following steps of (1) mixing illegal cooking oil, methanol and concentrated sulfuric acid in a mass ratio: methanol: concentrated sulfuric acid is 1.2: 1.8: 0.09, stirring and reacting for 12 hours at 90 ℃ to obtain a product 1;
(2) the preparation method comprises the following steps of (1) mixing hydroxylamine hydrochloride, water and sodium hydroxide according to the mass ratio: water: sodium hydroxide ═ 1.3: 9.3: 2.4, mixing, stirring and reacting for 3 hours at the temperature of 30 ℃ to obtain a product 2;
(3) and (3) mixing the product 1 with the product 1: product 2 ═ 1.2: 0.48 is added into the product 2, and is stirred and reacts for 6 hours at the temperature of 60 ℃, and the rare earth ore flotation collector is obtained.
Example 3
The embodiment is an application example of the rare earth ore flotation collector in the flotation of rare earth ore.
Grinding ore until mineral monomers are dissociated, adding sodium carbonate to adjust the pH value of ore pulp to 8, then adding 4100g/t of sodium silicate as an inhibitor, then adding 3200g/t of the collecting agent prepared in example 1, finally adding 58g/t of foaming agent No. 2 oil to perform rough flotation on the rare earth ore, adding 600g/t of the collecting agent and 25g/t of No. 2 oil in scavenging, adding 550g/t of sodium silicate in primary concentration, and adding 350g/t of sodium silicate in secondary concentration. The result shows that the rare earth ore can be effectively and efficiently floated by adopting the medicament conditions, and the flotation rare earth concentrate containing the REO 66.92% and having the recovery rate of 90.16% is obtained by once roughing, once scavenging and twice concentrating under the condition that the REO content of the ore is 10.18%.
Example 4
The embodiment is another application example of the rare earth ore flotation collector in the flotation of rare earth ore.
Grinding ore until mineral monomers are dissociated, adding sodium carbonate to adjust the pH value of ore pulp to 9, then adding 1200g/t of water glass as an inhibitor, then adding 1300g/t of a collecting agent prepared in example 1, finally adding 88g/t of foaming agent No. 2 oil to perform rough flotation on the rare earth ore, adding 600g/t of water glass, 600g/t of the collecting agent and 50g/t of No. 2 oil in scavenging, adding 340g/t of water glass in primary concentration, adding 120g/t of water glass in secondary concentration, and adding 120g/t of water glass in tertiary concentration. The result shows that the rare earth ore can be effectively and efficiently floated by adopting the medicament conditions, and the flotation rare earth concentrate containing 61.04 percent of REO and having the recovery rate of 92.19 percent is obtained by once roughing, once scavenging and three times of concentration under the condition that the REO content of the ore is 3.68 percent.
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (1)
1. A preparation method of a rare earth ore flotation collector is characterized by comprising the following steps: the method comprises the following steps:
(1) the method comprises the following steps of (1) mixing illegal cooking oil, methanol and concentrated sulfuric acid in a mass ratio: methanol: 1.0-1.2% of concentrated sulfuric acid: 1.1-1.8: 0.05-0.09, stirring and reacting for 5-12 hours at the temperature of 60-90 ℃ to obtain a product 1;
(2) the preparation method comprises the following steps of (1) mixing hydroxylamine hydrochloride, water and sodium hydroxide according to the mass ratio: water: 1.0 to 1.3% of sodium hydroxide: 6.4-9.3: 1.9-2.4, stirring and reacting for 1-3 hours at 20-30 ℃ to obtain a product 2;
(3) and (3) mixing the product 1 with the product 1: and (3) the product 2 is 1.0-1.2: 0.28-0.48, adding the mixture into the product 2, and stirring and reacting for 4-6 hours at 40-60 ℃ to obtain the rare earth ore flotation collector;
the application of the rare earth ore flotation collector specifically comprises the following steps: firstly, grinding raw ore rare earth ore until monomer is dissociated, then adding an inhibitor, adding the collecting agent obtained in the step (3), and finally adding a foaming agent to collect the rare earth ore, wherein the total using amount of the collecting agent is as follows: 1000-9000 g/t;
the pH value of the flotation pulp is 8-13, and the pH value of the pulp is adjusted through sodium carbonate or sodium hydroxide;
the inhibitor is water glass, and the total dosage of the water glass is 2000-8000 g/t;
the foaming agent is one of No. 2 oil or methyl isobutyl carbinol, and the total consumption of the foaming agent is 60-600 g/t.
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110813540B (en) * | 2019-10-24 | 2021-11-26 | 商洛学院 | Collecting agent composition for flotation and recovery of monazite from zircon heavy sand |
| CN110813541B (en) * | 2019-10-24 | 2021-05-28 | 商洛学院 | Collector combination for flotation of monazite and xenotime from fine-grained seashore placer |
| CN110947520A (en) * | 2019-10-28 | 2020-04-03 | 中国地质科学院矿产综合利用研究所 | Collecting agent for reverse flotation of medium-low grade collophanite, preparation method and application |
| CN110976096B (en) * | 2019-11-15 | 2021-05-14 | 南华大学 | Beneficiation method for rare earth ore |
Citations (7)
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| JPS55119456A (en) * | 1979-03-08 | 1980-09-13 | Dowa Mining Co Ltd | Floatation method of bastnaesite |
| JPS60238173A (en) * | 1984-05-12 | 1985-11-27 | Kobe Steel Ltd | Flotation of rare earth mineral |
| CN86100710A (en) * | 1986-01-24 | 1987-08-05 | 冶金工业部包头稀土研究院 | A kind of synthesis technique of rare earth catching agent |
| CN1114596A (en) * | 1994-07-07 | 1996-01-10 | 金仲农 | Method for preparation of collecting agent of oxidized ore |
| CN1403204A (en) * | 2001-09-11 | 2003-03-19 | 上海第二工业大学 | RE mineral floating process |
| CN102500465A (en) * | 2011-11-22 | 2012-06-20 | 广州有色金属研究院 | Benefication method for bastnaesite |
| CN107185723A (en) * | 2017-07-26 | 2017-09-22 | 平顶山华兴浮选工程技术服务有限公司 | A kind of low-grade bauxite direct flotation collecting agent and preparation method thereof |
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2017
- 2017-10-11 CN CN201710941687.2A patent/CN107520063B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS55119456A (en) * | 1979-03-08 | 1980-09-13 | Dowa Mining Co Ltd | Floatation method of bastnaesite |
| JPS60238173A (en) * | 1984-05-12 | 1985-11-27 | Kobe Steel Ltd | Flotation of rare earth mineral |
| CN86100710A (en) * | 1986-01-24 | 1987-08-05 | 冶金工业部包头稀土研究院 | A kind of synthesis technique of rare earth catching agent |
| CN1114596A (en) * | 1994-07-07 | 1996-01-10 | 金仲农 | Method for preparation of collecting agent of oxidized ore |
| CN1403204A (en) * | 2001-09-11 | 2003-03-19 | 上海第二工业大学 | RE mineral floating process |
| CN102500465A (en) * | 2011-11-22 | 2012-06-20 | 广州有色金属研究院 | Benefication method for bastnaesite |
| CN107185723A (en) * | 2017-07-26 | 2017-09-22 | 平顶山华兴浮选工程技术服务有限公司 | A kind of low-grade bauxite direct flotation collecting agent and preparation method thereof |
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