CN111515029B - Collecting agent for separating monazite and ilmenite and using method thereof - Google Patents

Collecting agent for separating monazite and ilmenite and using method thereof Download PDF

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CN111515029B
CN111515029B CN202010363725.2A CN202010363725A CN111515029B CN 111515029 B CN111515029 B CN 111515029B CN 202010363725 A CN202010363725 A CN 202010363725A CN 111515029 B CN111515029 B CN 111515029B
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monazite
ilmenite
parts
flotation
concentrate
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CN111515029A (en
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陈江安
董文
余文
钟金根
黎春
韦梦翔
王美乔
匡敬忠
邱廷省
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Fujian Wensheng Mining Co ltd
Hainan Haituo Mining Co ltd
Hainan Wensheng High Tech Materials Co ltd
Shenghe Resources Lianyungang New Material Technology Co ltd
Jiangxi University of Science and Technology
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Fujian Wensheng Mining Co ltd
Hainan Haituo Mining Co ltd
Hainan Wensheng High Tech Materials Co ltd
Jiangxi University of Science and Technology
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION 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
    • B03DFLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D1/00Flotation
    • B03D1/02Froth-flotation processes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION 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
    • B03DFLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D1/00Flotation
    • B03D1/001Flotation agents
    • B03D1/018Mixtures of inorganic and organic compounds
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION 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
    • B03DFLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D2201/00Specified effects produced by the flotation agents
    • B03D2201/02Collectors
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION 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
    • B03DFLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D2203/00Specified materials treated by the flotation agents; specified applications
    • B03D2203/02Ores
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00Technologies for solid waste management
    • Y02W30/50Reuse, recycling or recovery technologies
    • Y02W30/52Mechanical processing of waste for the recovery of materials, e.g. crushing, shredding, separation or disassembly

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  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

The invention provides a collecting agent for sorting monazite and ilmenite and a using method thereof, wherein the collecting agent comprises 10-15 parts of tall oil, 25-35 parts of oxidized paraffin soap, 40-50 parts of palm oil, 10-15 parts of fatty acid methyl ester sodium sulfonate and 10-15 parts of sodium hydroxide; performing microwave pretreatment on tall oil, oxidized paraffin soap, palm oil and fatty acid methyl ester sodium sulfonate, and then mixing and stirring at 70-85 ℃; and adding sodium hydroxide, and mixing at 85-100 ℃ to obtain the collector. The invention adopts a novel microwave pre-activation pretreatment mode on equipment to replace a direct reaction kettle reaction, thereby reducing saponification time, reducing production cost and having better collecting effect. By using the collecting agent, the comprehensive grade P of monazite concentrate can be improved to more than 10.29 percent, the operation recovery rate P can be improved to more than 88.03 percent, and the comprehensive grade TiO of ilmenite can be improved2Improves the recovery rate to over 50.00 percent and the operation recovery rate of TiO2The yield is improved to more than 96.22 percent, and the economic benefit is good.

Description

Collecting agent for separating monazite and ilmenite and using method thereof
Technical Field
The invention belongs to the technical field of mineral separation, and particularly relates to a mineral separation process for separating monazite and ilmenite from seashore placer, in particular to a collecting agent for separating monazite and ilmenite and a using method thereof.
Background
The seaside placer is a very important deposit in the mineral resources of Hainan and Guangxi in China, and the deposit is accompanied by zirconite, monazite and the like with extremely large reserves besides abundant ilmenite reserves. Foreign sources of this type are also abundant elsewhere, typically in australia, malaysia, the united states, south africa, brazil, india, mozzarex, etc.
In the process of magnetic separation of ilmenite, because monazite has certain weak magnetism, a small amount of monazite is often contained in ilmenite concentrate, and because monazite contains P, the content of P required in the ilmenite concentrate is below 0.1%, the quality of fine ilmenite is reduced, and because monazite is reduced, the economic benefit of production enterprises is also reduced. The removal of monazite from ilmenite is therefore one of the essential ways to increase efficiency. Therefore, the method has important theoretical significance and practical application value for strengthening the research on the beneficiation technology of the ilmenite resources.
At present, few documents are reported on the ore dressing process of ilmenite floatation monazite, and a sodium oleate floatation method is mainly adopted and is carried out under strong acid or strong alkali. Because of the influence of the current environmental protection measures, strong acid and strong alkali are not suitable for the recovery of valuable metals such as monazite and the like at present. The Yangtong flotation operation is carried out on zirconite and monazite in ilmenite in a certain seashore placer in Hainan province. Under the condition that the raw ore contains TREO 6.12% and the pH value is more than 12, the monazite rough concentrate with TREO 9.12% and the recovery rate of 85.71% is obtained by adding the sodium oleate collecting agent.
Disclosure of Invention
In view of the defects of the prior art, the invention provides a collecting agent for separating monazite and ilmenite and a using method thereof, aiming at improving the effective separation of monazite in ilmenite at a natural pH value.
The scheme of the invention is as follows:
a collecting agent for separating monazite and ilmenite comprises the following raw materials in parts by weight:
Figure BDA0002475986930000011
Figure BDA0002475986930000021
the collector is prepared by the following method:
(1) performing microwave pretreatment on tall oil, oxidized paraffin soap, palm oil and fatty acid methyl ester sodium sulfonate, and then mixing and stirring at 70-85 ℃; the microwave power is 5-10 kg/kw, and the microwave frequency is 2000-3000 MHz;
(2) and adding sodium hydroxide, and mixing at 85-100 ℃.
Preferably, the collecting agent for sorting monazite and ilmenite comprises the following raw materials in parts by weight:
Figure BDA0002475986930000022
preferably, the microwave pretreatment time is 5-10 minutes.
Preferably, after the sodium hydroxide is added in the step (2), the mixture is mixed for 1.5 to 2.5 hours at the temperature of 85 to 100 ℃.
The invention also specifically provides a method for separating monazite and ilmenite by using the collector, which comprises the following steps:
(1) roughing
The roughing condition is as follows: carrying out flotation on the raw materials; the mass concentration of the flotation ore pulp is 40-60%, the flotation time is 15-25 min, and the using amount of a collecting agent is 250-300 g/t raw material; the dosage of the inhibitor is 500-700 g/t of raw material; the dosage of the activating agent is 150-180 g/t of raw material; the amount of the foaming agent is 35-40 g/t of raw material; obtaining monazite roughing concentrate and tailings;
(2) refining
And (3) carrying out concentration on the monazite rough concentrate under the concentration conditions: the flotation mass concentration is 30-50%, the flotation time is 10-15 min, and the collecting agent consumption is 100-150 g/t monazite rough concentrate; the using amount of the inhibitor is 300-500 g/t monazite roughing concentrate; the using amount of the activating agent is 50-60 g/t monazite roughing concentrate; the amount of the foaming agent is 21-25 g/t monazite roughing concentrate; and obtaining monazite concentrate and tailings.
Preferably, in the using method step (1), after 5-10 min of flotation, polyethylene glycol and sodium benzoate are added, and flotation is carried out for 10-15 min, so as to obtain monazite rougher concentrate and tailings.
Preferably, the dosage of the polyethylene glycol is 30-35 g/t of raw material, and the dosage of the sodium benzoate is 30-40 g/t of raw material.
Preferably, in the flotation process of the invention, the inhibitor is water glass, the activator is copper sulfate, and the foaming agent is # 2 oil.
Compared with the prior art, the invention has the beneficial effects that:
the invention adopts a novel microwave pre-activation pretreatment mode on equipment to replace a direct reaction kettle reaction, reduces saponification time, reduces generation cost and has better collecting effect.
Secondly, in the process, cheap palm oil and the like in the market are adopted, so that the collecting agent product is more economical.
Thirdly, the partyCompared with the known technology, the method comprehensively improves the monazite grade, improves the comprehensive grade P of the monazite concentrate to more than 10.29 percent, improves the operation recovery rate P to more than 88.03 percent, and improves the comprehensive grade TiO of the ilmenite2Improves the recovery rate to over 50.00 percent and the operation recovery rate of TiO2The yield is improved to more than 96.22 percent, and the economic benefit is good.
The invention also discovers in the original process that the sodium benzoate and the polyethylene glycol are used in the roughing process, so that the selective enrichment effect of different minerals at a solid-liquid-gas three-phase interface can be improved, the separation effect of monazite and ilmenite is enhanced, the separation efficiency is improved, the comprehensive grade P of monazite concentrate is improved to be more than 17.64 percent, the operation recovery rate P is improved to be more than 96.07 percent, and the comprehensive grade TiO of ilmenite is improved2Improves the recovery rate to over 60.50 percent and the operation recovery rate of TiO2The yield is improved to more than 98.36 percent.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
In order to better understand the technical content of the invention, specific examples are provided below to further illustrate the invention.
Example 1 preparation of collector
(1) According to the weight portion, 10 portions of tall oil, 25 portions of oxidized paraffin soap, 50 portions of palm oil and 15 portions of fatty acid methyl ester sodium sulfonate are taken for microwave pretreatment for 10 minutes, the microwave power is 10kg/kw, and the microwave frequency is 2000MHZ. Then mixing and stirring the mixture in a reaction kettle at 85 ℃.
(2) Then, 10 parts of sodium hydroxide was added thereto, and the mixture was saponified at 100 ℃ for 1.5 hours.
Example 2 preparation of collectors
(1) According to the weight portion, taking 25 portions of tall oil, 35 portions of oxidized paraffin soap, 40 portions of palm oil and 10 portions of fatty acid methyl ester sodium sulfonate, and carrying out microwave pretreatment for 5 minutes with the microwave power of 5kg/kw and the microwave frequency of 3000MHZ. Then mixed and stirred in a reaction kettle at 70 ℃.
(2) Then, 15 parts of sodium hydroxide was added thereto, and the mixture was saponified at 85 ℃ for 2.5 hours.
Example 3 flotation process of monazite and ilmenite
The raw material is rough concentrate of Mosangbicg ilmenite of Hainan Haitou mining Co Ltd, wherein the rough concentrate contains TiO250.26 percent and contains 0.98 percent of P. Wherein ilmenite is the main component, and part of monazite, zircon and a small amount of garnet are also included.
The flotation adopts a mode of once roughing and once fine selection. The flotation scheme is shown in figure 1.
(1) Roughing
The roughing condition is as follows: the flotation concentration is 40-60%, the flotation time is 15min, the collecting agent is the collecting agent in the embodiment 1, and the using amount is 250 g/t; the inhibitor is water glass, and the dosage is 500 g/t; the activating agent is copper sulfate, and the dosage is 150 g/t; the foaming agent is 2# oil, and the dosage is 40 g/t; and obtaining monazite rougher concentrate and tailings.
(2) Refining
And (4) carrying out coarse concentration on the monazite concentrate. The selection conditions are as follows: the flotation concentration is 30-50%, the flotation time is 10min, the collecting agent is the collecting agent in the embodiment 1, and the using amount is 100 g/t; the inhibitor is water glass, and the dosage is 300 g/t; the activating agent is copper sulfate, and the dosage is 50 g/t; the foaming agent is 2# oil, and the dosage is 21 g/t; and obtaining monazite concentrate and tailings. The tailings are qualified ilmenite, and the concentrate is qualified monazite.
Example 4 flotation process of monazite and ilmenite
The raw material is rough concentrate of Australian ilmenite of Fujian Wensheng mining Co Ltd, wherein the rough concentrate contains TiO247.38 percent and contains P1.14 percent. Wherein ilmenite is the main component, and part of monazite, zircon and a small amount of garnet are also included.
The flotation adopts a mode of one-time roughing and one-time fine selection
(1) Roughing
The roughing condition is as follows: the flotation concentration is 45-55%, the flotation time is 16min, the collecting agent is the collecting agent in the embodiment 1, and the using amount is 300 g/t; the inhibitor is water glass, and the dosage is 700 g/t; the activating agent is copper sulfate, and the dosage is 150 g/t; the foaming agent is No. 2 oil, and the dosage is 35 g/t; and obtaining monazite rougher concentrate and tailings.
(2) Refining
And (4) carrying out coarse concentration on the monazite concentrate. The selection conditions are as follows: the flotation concentration is 30-40%, the flotation time is 10min, the collecting agent is the collecting agent in the embodiment 1, and the using amount is 150 g/t; the inhibitor is water glass, and the dosage is 500 g/t; the activating agent is copper sulfate, and the dosage is 50 g/t; the foaming agent is 2# oil, and the dosage is 25 g/t; and obtaining monazite concentrate and tailings. The tailings are qualified ilmenite, and the concentrate is qualified monazite.
Example 5 flotation process for monazite and ilmenite
The flotation adopts a mode of once roughing and once fine selection.
(1) Roughing
The roughing condition is as follows: the flotation concentration is 50-60%, the flotation time is 25min, the collecting agent is the collecting agent in the embodiment 1, and the using amount is 300 g/t; the inhibitor is water glass, and the dosage is 600 g/t; the activating agent is copper sulfate, and the dosage is 180 g/t; the foaming agent is No. 2 oil, and the dosage is 35 g/t; and obtaining monazite rougher concentrate and tailings.
(2) Beneficiation of
And (4) carrying out coarse concentration on the monazite concentrate. The selection conditions are as follows: the flotation concentration is 30-50%, the flotation time is 15min, the collecting agent is the collecting agent in the embodiment 1, and the using amount is 100 g/t; the inhibitor is water glass, and the dosage is 300 g/t; the activating agent is copper sulfate, and the dosage is 60 g/t; the foaming agent is 2# oil, and the dosage is 25 g/t; and obtaining monazite concentrate and tailings. The tailings are qualified ilmenite, and the concentrate is qualified monazite.
Example 6
The main differences between example 6 and example 3 are:
in the step (1), after flotation is carried out for 10min, polyethylene glycol 600 and sodium benzoate are added, and flotation is carried out for 10min to obtain monazite rougher concentrate and tailings; the dosage of the polyethylene glycol is 35g/t, and the dosage of the sodium benzoate is 30 g/t.
Example 7
The main differences between example 7 and example 3 are:
in the step (1), after 5min of flotation, adding polyethylene glycol 600 and sodium benzoate, and performing flotation for 10min to obtain monazite rougher concentrate and tailings; the dosage of the polyethylene glycol is 30g/t, and the dosage of the sodium benzoate is 40 g/t.
Comparative example 1
A conventional sodium oleate flotation process is employed.
Comparative example 2
The main differences between comparative example 2 and example 3 are:
tall oil, oxidized paraffin soap, palm oil and sodium fatty acid methyl ester sulfonate were not pretreated with microwave.
Comparative example 3
The main differences between comparative example 3 and example 3 are:
replacing palm oil with soybean oil; the oxidized paraffin soap was replaced with sodium dodecylbenzenesulfonate.
The comprehensive grade and the operation recovery rate of the products obtained in the above examples and comparative examples are detected and counted, and the results are shown in table 1.
TABLE 1
Figure BDA0002475986930000061
The results show that:
by adopting the novel collecting agent, the raw ore can contain TiO247.38-50.37%, separating the monazite concentrate and the comprehensive grade TiO with comprehensive grade P of 10.29-17.64% and operation recovery rate of 88.03-96.07% from ilmenite containing 0.98-1.14% of P250.00-60.50% of ilmenite concentrate with the operation recovery rate of 96.30-98.36%. And after the novel collecting agent is used, in the final filtering and drying process of the ilmenite concentrate product, substances such as sodium oleate and the like are not added, so that the final removal of the medicine is simple and easy, and the effect is good. In the final wastewater treatment process, the water glass is less in consumption, so that the water is more easily precipitated in the purification process of water, and the method is a clean production and environment-friendly method.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.

Claims (8)

1. A collecting agent for separating monazite and ilmenite is characterized by comprising the following raw materials in parts by weight:
10-15 parts of tall oil
25-35 parts of oxidized paraffin soap
40-50 parts of palm oil
10-15 parts of fatty acid methyl ester sodium sulfonate
10-15 parts of sodium hydroxide;
the collector is prepared by the following method:
(1) performing microwave pretreatment on tall oil, oxidized paraffin soap, palm oil and fatty acid methyl ester sodium sulfonate, and then mixing and stirring at 70-85 ℃; the microwave power is 5-10 kw/kg, and the microwave frequency is 2000-3000 MHz;
(2) and adding sodium hydroxide, and mixing at 85-100 ℃.
2. A collector for use in the separation of monazite and ilmenite as claimed in claim 1, which includes the following parts by weight of the raw materials:
10 portions of tall oil
Oxidized paraffin wax soap 25 parts
50 portions of palm oil
15 parts of fatty acid methyl ester sodium sulfonate
10 parts of sodium hydroxide.
3. The collector for sorting monazite and ilmenite as claimed in claim 1, wherein the microwave pretreatment time is 5-10 minutes.
4. The collector for separating monazite and ilmenite as claimed in claim 1, wherein the sodium hydroxide is added in the step (2) and then mixed for 1.5-2.5 hours at the temperature of 85-100 ℃.
5. A method of sorting monazite, ilmenite using the collector of claim 1, characterised by the steps of:
(1) roughing
The roughing condition is as follows: carrying out flotation on the raw materials; the mass concentration of the flotation ore pulp is 40-60%, the flotation time is 15-25 min, and the using amount of a collecting agent is 250-300 g/t raw material; the dosage of the inhibitor is 500-700 g/t of raw material; the dosage of the activating agent is 150-180 g/t of raw material; the amount of the foaming agent is 35-40 g/t of raw material; obtaining monazite roughing concentrate and tailings;
(2) refining
And (3) carrying out concentration on the monazite rough concentrate under the concentration conditions: the flotation mass concentration is 30-50%, the flotation time is 10-15 min, and the collecting agent consumption is 100-150 g/t monazite roughing concentrate; the using amount of the inhibitor is 300-500 g/t monazite roughing concentrate; the using amount of the activating agent is 50-60 g/t monazite roughing concentrate; the amount of the foaming agent is 21-25 g/t monazite roughing concentrate; and obtaining monazite concentrate and tailings.
6. The method for separating monazite and ilmenite from the collecting agent of claim 1, according to claim 5, wherein in the step (1), after 5-10 min of flotation, polyethylene glycol and sodium benzoate are added, and flotation is carried out for 10-15 min, so that monazite rougher concentrate and tailings are obtained.
7. The method for separating monazite and ilmenite by using the collector as claimed in claim 1, according to claim 6, wherein the dosage of the polyethylene glycol is 30-35 g/t of raw material, and the dosage of the sodium benzoate is 30-40 g/t of raw material.
8. A method of sorting monazite and ilmenite as claimed in any one of claims 5 to 7 using a collector as claimed in claim 1, characterised in that the suppressor is water glass, the activator is copper sulphate and the frothing agent is 2# oil.
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CN112774850B (en) * 2020-12-28 2022-09-13 海南文盛新材料科技股份有限公司 Ore dressing process for sorting monazite by using grading jigger

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