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CN113953093B - Ilmenite collecting agent preparation method based on modified plant asphalt - Google Patents

Ilmenite collecting agent preparation method based on modified plant asphalt Download PDF

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Publication number
CN113953093B
CN113953093B CN202111200585.8A CN202111200585A CN113953093B CN 113953093 B CN113953093 B CN 113953093B CN 202111200585 A CN202111200585 A CN 202111200585A CN 113953093 B CN113953093 B CN 113953093B
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collecting agent
ilmenite
asphalt
liquid alkali
modified plant
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CN113953093A (en
Inventor
黄齐茂
左芬
朱言卓
胡骆兴
龚慧敏
席静
周航
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Wuhan Institute of Technology
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Wuhan Institute of 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
    • B03D1/001Flotation 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
    • B03D2203/04Non-sulfide ores

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

Abstract

The invention discloses a preparation method of an ilmenite collecting agent based on modified plant asphalt, which comprises the steps of carrying out hydroxylation reaction on plant asphalt and liquid alkali in a high-pressure reaction kettle for 1-2 h; cooling to 80-100deg.C, adding complexing agent and surfactant, stirring and mixing to obtain collecting agent; the raw materials are as follows in percentage by mass: 52-58% of plant asphalt, 25% of liquid alkali, 2-8% of complexing agent and 12-18% of surfactant; the invention adopts vegetable cotton oil asphalt containing more double bonds, and vegetable cotton oil asphalt containing a certain number of hydroxyl groups to carry out hydroxylation reaction to obtain polyhydroxy mixture. The hydroxyl and ilmenite ions have certain chelation effect, and chelating adsorption occurs on the surface of minerals, so that the ilmenite has better selectivity.

Description

Ilmenite collecting agent preparation method based on modified plant asphalt
Technical Field
The invention belongs to the technical field of mineral processing, and particularly relates to a preparation method of an ilmenite collecting agent.
Background
With the development of society, titanium metal gradually plays an important role in a series of high-end technical fields such as aerospace, marine ships and the like, and becomes a strategic resource for supporting the development of important fields. Most of the titanium elements in nature exist in the form of ilmenite (iron titanate, feO.2TiO 2 compound). Ilmenite is a major mineral species with industrial and economic value. China is a country with very abundant ilmenite reserves, the reserves reach the second world, but most ilmenite has the characteristic of lean and fine impurities, in order to effectively realize the flotation separation of various minerals, the wettability of the surfaces of the minerals must be artificially controlled through a flotation reagent, the floatable difference among the minerals is enlarged, the effective separation of titanium concentrate and gangue minerals is realized, and the high-efficiency separation of lean and fine impurities ilmenite is realized. The conventional flotation collector has low sorting efficiency. Therefore, the research on the flotation collector with high efficiency and good cost performance of ilmenite is particularly important.
Disclosure of Invention
The invention aims to provide a preparation method of a high-efficiency ilmenite collecting agent based on modified plant asphalt, which is characterized in that low-cost plant asphalt, liquid alkali, deionized water, a complexing agent and a surfactant are modified and compounded to obtain the ilmenite collecting agent with excellent cost performance.
In order to achieve the above purpose, the following technical scheme is adopted:
the preparation method of the ilmenite collecting agent based on the modified plant asphalt comprises the following steps:
Carrying out hydroxylation reaction on plant asphalt and liquid alkali in a high-pressure reaction kettle for 1-2 h;
Cooling to 80-100deg.C, adding complexing agent and surfactant, stirring, and mixing to obtain collecting agent.
According to the scheme, the raw materials are as follows in percentage by mass:
52-58% of plant asphalt, 25% of liquid alkali, 2-8% of complexing agent and 12-18% of surfactant.
According to the scheme, the plant asphalt is plant cotton oil asphalt.
According to the scheme, the liquid alkali is industrial liquid alkali with concentration of 32wt% or 45wt% potassium hydroxide solution.
According to the scheme, the complexing agent is benzyl arsinic acid or benzyl hydroxamic acid.
According to the scheme, the surfactant is at least one of sodium dodecyl benzene sulfonate, sodium fatty alcohol polyoxyethylene ether sulfate and coco diethanolamide.
Compared with the conventional ilmenite collecting agent, the invention has the following beneficial effects:
Vegetable cotton oil asphalt contains more double bonds, and meanwhile, vegetable cotton oil asphalt contains a certain number of hydroxyl groups, and a polyhydroxy mixture is obtained after hydroxylation reaction. The hydroxyl and ilmenite ions have certain chelation effect, and chelating adsorption occurs on the surface of minerals, so that the ilmenite has better selectivity. The surfactant molecules adsorb to the mine surface in the mine liquor, changing the surface tension of the liquor. The collector can effectively improve the enrichment of titanium ore, increase the selectivity, and has low price and easy preparation.
Detailed Description
The following examples further illustrate the technical aspects of the present invention, but are not intended to limit the scope of the present invention.
The invention provides a preparation method of an ilmenite collecting agent based on modified plant asphalt, which comprises the following specific processes:
Carrying out hydroxylation reaction on plant asphalt and liquid alkali in a high-pressure reaction kettle for 1-2 h;
Cooling to 80-100deg.C, adding complexing agent and surfactant, stirring, and mixing to obtain collecting agent.
Wherein the raw materials are as follows in percentage by mass:
52-58% of plant asphalt, 25% of liquid alkali, 2-8% of complexing agent and 12-18% of surfactant.
The vegetable asphalt used in the specific embodiment is vegetable cotton oil asphalt; the liquid alkali is industrial liquid alkali with concentration of 32 weight percent or 45 weight percent potassium hydroxide solution; the complexing agent is benzyl arsinic acid or benzyl hydroxamic acid; the surfactant is at least one of sodium dodecyl benzene sulfonate, sodium fatty alcohol polyoxyethylene ether sulfate and coco diethanolamide.
Example 1
The high-efficiency ilmenite collecting agent comprises the following raw materials in percentage by mass: 58% of vegetable cotton oil asphalt, 24% of industrial liquid alkali, 2% of benzyl arsenical acid and 16% of sodium dodecyl benzene sulfonate.
Firstly, slowly adding vegetable cotton oil asphalt and prepared industrial liquid alkali into a high-pressure reaction kettle for hydroxylation reaction for 1h, stirring and adding benzyl arsinic acid and sodium dodecyl benzene sulfonate after the reaction is completely cooled to 90 ℃, and continuously stirring until the mixture is uniformly mixed to obtain the collecting agent.
The ilmenite collecting agent is prepared by adopting the collecting agent, and the raw ore with 23.44 percent of flotation grade is subjected to flotation, so that the grade of the titanium concentrate reaches 47.1 percent, and a good index with 85.63 percent of recovery rate is obtained.
Example 2
The high-efficiency ilmenite collecting agent comprises the following raw materials in percentage by mass: 57% of vegetable cotton oil asphalt, 24% of industrial liquid alkali, 3% of benzyl arsenical acid and 16% of coconut diethanolamide.
Firstly, slowly adding vegetable cotton oil asphalt and prepared industrial liquid alkali into a high-pressure reaction kettle for hydroxylation reaction for 1.1h, stirring and adding benzyl arsinic acid and cocoyl diethanolamide after the reaction is completely cooled to 90 ℃, and continuously stirring until the mixture is uniformly mixed to obtain the collector.
The ilmenite collecting agent is prepared by adopting the collecting agent, and the raw ore with 23.44 percent of flotation grade is subjected to flotation, so that the grade of the titanium concentrate reaches 47.34 percent, and a good index with 85.54 percent of recovery rate is obtained.
Example 3
The high-efficiency ilmenite collecting agent comprises the following raw materials in percentage by mass: 57% of vegetable cotton oil asphalt, 24% of prepared potassium hydroxide solution with concentration of 45%, 4% of benzyl arsinic acid and 15% of sodium dodecyl benzene sulfonate.
Firstly, slowly adding vegetable cotton oil asphalt and prepared 45% potassium hydroxide solution into a high-pressure reaction kettle for hydroxylation reaction for 2 hours, stirring and adding benzyl arsinic acid and sodium dodecyl benzene sulfonate after the reaction is completely cooled to 90 ℃, and continuously stirring until the mixture is uniformly mixed to obtain the collector.
The ilmenite collecting agent is prepared by adopting the collecting agent, and the raw ore with 23.44 percent of flotation grade is subjected to flotation, so that a good index of the grade of the titanium concentrate reaching 47.39 percent and the recovery rate reaching 85.46 percent is obtained.
Example 4
The high-efficiency ilmenite collecting agent comprises the following raw materials in percentage by mass: 56% of vegetable cotton oil asphalt, 24% of industrial liquid alkali, 4% of benzoic hydroxamic acid and 16% of fatty alcohol polyoxyethylene ether sodium sulfate.
Firstly, slowly adding vegetable cotton oil asphalt and industrial liquid alkali into a high-pressure reaction kettle for hydroxylation reaction for 1.2 hours, stirring and adding benzoic hydroxamic acid and fatty alcohol polyoxyethylene ether sodium sulfate after the reaction is completely cooled to 90 ℃, and continuously stirring until the mixture is uniformly mixed to obtain the collecting agent.
The ilmenite collecting agent is prepared by adopting the collecting agent, and the raw ore with 23.44 percent of flotation grade is subjected to flotation, so that the grade of the titanium concentrate reaches 47.52 percent, and a good index with 85.33 percent of recovery rate is obtained.
Example 5
The high-efficiency ilmenite collecting agent comprises the following raw materials in percentage by mass: 56% of vegetable pitch, 24% of prepared 45% concentration potassium hydroxide solution, 7% of benzyl arsinic acid and 13% of fatty alcohol polyoxyethylene ether sodium sulfate.
Firstly, slowly adding vegetable cotton oil asphalt and prepared 45% potassium hydroxide solution into a high-pressure reaction kettle for hydroxylation reaction for 1.9h, stirring and adding benzyl arsinic acid and fatty alcohol polyoxyethylene ether sodium sulfate after the reaction is completely cooled to 90 ℃, and continuously stirring until the mixture is uniformly mixed to obtain the collector.
The ilmenite collecting agent is prepared by adopting the collecting agent, and the raw ore with 23.44 percent of flotation grade is subjected to flotation, so that the grade of the titanium concentrate reaches 47.87 percent, and a good index with 85.17 percent of recovery rate is obtained.
Example 6
The high-efficiency ilmenite collecting agent comprises the following raw materials in percentage by mass: 56% of vegetable pitch, 24% of industrial liquid alkali, 8% of benzyl arsenical acid and 12% of coco diethanolamide.
Firstly, slowly adding vegetable cotton oil asphalt and industrial liquid alkali into a high-pressure reaction kettle for hydroxylation reaction for 1.5h, stirring and adding benzyl arsinic acid and cocoyl diethanolamide after the reaction is completely cooled to 90 ℃, and continuously stirring until the mixture is uniformly mixed to obtain the collecting agent.
The ilmenite collecting agent is prepared by adopting the collecting agent, and the raw ore with 23.44 percent of flotation grade is subjected to flotation, so that the grade of the titanium concentrate reaches 48.02 percent, and a good index with 84.97 percent of recovery rate is obtained.
Example 7
The high-efficiency ilmenite collecting agent comprises the following raw materials in percentage by mass: 55% of vegetable asphalt, 24% of industrial liquid alkali, 5% of benzyl arsinic acid and 16% of sodium dodecyl benzene sulfonate.
Firstly, slowly adding vegetable cotton oil asphalt and industrial liquid alkali into a high-pressure reaction kettle for hydroxylation reaction for 1.2 hours, stirring and adding benzyl arsinic acid and sodium dodecyl benzene sulfonate after the reaction is completely cooled to 90 ℃, and continuously stirring until the mixture is uniformly mixed to obtain the collecting agent.
The ilmenite collecting agent is prepared by adopting the collecting agent, and the raw ore with 23.44 percent of flotation grade is subjected to flotation, so that a good index of the grade of the titanium concentrate reaching 47.82 percent and the recovery rate reaching 84.86 percent is obtained.
Example 8
The high-efficiency ilmenite collecting agent comprises the following raw materials in percentage by mass: 55% of vegetable asphalt, 24% of industrial liquid alkali, 6% of benzoic hydroxamic acid and 15% of fatty alcohol polyoxyethylene ether sodium sulfate.
Firstly, slowly adding vegetable cotton oil asphalt and industrial liquid alkali into a high-pressure reaction kettle for hydroxylation reaction for 1.4 hours, stirring and adding benzoic hydroxamic acid and fatty alcohol polyoxyethylene ether sodium sulfate after the reaction is completely cooled to 90 ℃, and continuously stirring until the mixture is uniformly mixed to obtain the collecting agent.
The ilmenite collecting agent is prepared by adopting the collecting agent, and the raw ore with 23.44 percent of flotation grade is subjected to flotation, so that the grade of the titanium concentrate reaches 47.74 percent, and a good index with 84.72 percent of recovery rate is obtained.
Example 9
The high-efficiency ilmenite collecting agent comprises the following raw materials in percentage by mass: 55% of vegetable asphalt, 24% of prepared potassium hydroxide solution with the concentration of 45%, 7% of benzohydroxamic acid and 13% of fatty alcohol polyoxyethylene ether sodium sulfate.
Firstly, slowly adding vegetable cotton oil asphalt and prepared 45% potassium hydroxide solution into a high-pressure reaction kettle for hydroxylation reaction for 2 hours, stirring and adding the benzoic hydroxamic acid and the fatty alcohol polyoxyethylene ether sodium sulfate after the reaction is completely cooled to 90 ℃, and continuously stirring until the mixture is uniformly mixed to obtain the collector.
The ilmenite collecting agent is prepared by adopting the collecting agent, and the raw ore with 23.44 percent of flotation grade is subjected to flotation, so that the grade of the titanium concentrate reaches 47.95 percent, and a good index with 84.61 percent of recovery rate is obtained.
Example 10
The high-efficiency ilmenite collecting agent comprises the following raw materials in percentage by mass: 54% of vegetable pitch, 24% of industrial liquid alkali, 6% of benzyl arsenical acid and 16% of sodium dodecyl benzene sulfonate.
Firstly, slowly adding vegetable cotton oil asphalt and industrial liquid alkali into a high-pressure reaction kettle for hydroxylation reaction for 1.7h, stirring and adding benzyl arsinic acid and sodium dodecyl benzene sulfonate after the reaction is completely cooled to 90 ℃, and continuously stirring until the mixture is uniformly mixed to obtain the collecting agent.
The ilmenite collecting agent is prepared by adopting the collecting agent, and the raw ore with 23.44 percent of flotation grade is subjected to flotation, so that the grade of the titanium concentrate reaches 47.57 percent, and a good index with 84.57 percent of recovery rate is obtained.
Example 11
The high-efficiency ilmenite collecting agent comprises the following raw materials in percentage by mass: 53% of vegetable pitch, 24% of industrial liquid alkali, 7% of benzoic hydroxamic acid and 16% of coco diethanolamide.
Firstly, slowly adding vegetable cotton oil asphalt and industrial liquid alkali into a high-pressure reaction kettle for hydroxylation reaction for 1.6 hours, stirring and adding benzoic hydroxamic acid and coco diethanolamide after the reaction is completely cooled to 90 ℃, and continuously stirring until the mixture is uniformly mixed to obtain the collecting agent.
The ilmenite collecting agent is prepared by adopting the collecting agent, and the raw ore with 23.44 percent of flotation grade is subjected to flotation, so that the grade of the titanium concentrate reaches 47.95 percent, and a good index with 84.42 percent of recovery rate is obtained.
Example 12
The high-efficiency ilmenite collecting agent comprises the following raw materials in percentage by mass: 52% of vegetable pitch, 24% of prepared potassium hydroxide solution with concentration of 45%, 8% of benzyl arsinic acid and 16% of fatty alcohol polyoxyethylene ether sodium sulfate.
Firstly, slowly adding vegetable cotton oil asphalt and prepared 45% potassium hydroxide solution into a high-pressure reaction kettle for hydroxylation reaction for 1.8h, stirring and adding benzyl arsinic acid and fatty alcohol polyoxyethylene ether sodium sulfate after the reaction is completely cooled to 90 ℃, and continuously stirring until the mixture is uniformly mixed to obtain the collector.
The ilmenite collecting agent is prepared by adopting the collecting agent, and the raw ore with 23.44 percent of flotation grade is subjected to flotation, so that a good index of the grade of the titanium concentrate reaching 48.13 percent and the recovery rate reaching 82.17 percent is obtained.

Claims (4)

1. The preparation method of the ilmenite collecting agent based on the modified plant asphalt is characterized by comprising the following steps of:
vegetable cotton oil asphalt and liquid alkali are subjected to hydroxylation reaction in a high-pressure reaction kettle for 1-2 h;
Cooling to 80-100deg.C, adding complexing agent and surfactant, stirring and mixing to obtain collecting agent;
the raw materials are as follows in percentage by mass:
52-58% of vegetable cotton oil asphalt, 25% of liquid alkali, 2-8% of complexing agent and 12-18% of surfactant.
2. A process for preparing an ilmenite collector based on modified plant asphalt according to claim 1, wherein the liquid alkali is an industrial liquid alkali with a concentration of 32wt% or a 45wt% potassium hydroxide solution.
3. The method for preparing an ilmenite collecting agent based on modified plant asphalt according to claim 1, wherein the complexing agent is benzyl arsinic acid or benzoic hydroxamic acid.
4. The method for preparing the ilmenite collecting agent based on the modified plant asphalt according to claim 1, wherein the surfactant is at least one of sodium dodecyl benzene sulfonate, sodium fatty alcohol polyoxyethylene ether sulfate and coco diethanolamide.
CN202111200585.8A 2021-10-15 2021-10-15 Ilmenite collecting agent preparation method based on modified plant asphalt Active CN113953093B (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103331212A (en) * 2013-07-12 2013-10-02 武汉工程大学 Carbonate phosphorite reverse flotation collecting agent and preparation method thereof
CN105750091A (en) * 2014-12-16 2016-07-13 乐山顺辰科技有限公司 Mineral floatation colleting agent and manufacturing method thereof

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9266120B2 (en) * 2013-10-01 2016-02-23 Ecolab Usa Inc Collectors for mineral flotation
CN105880034B (en) * 2016-04-22 2019-02-05 北京矿冶研究总院 Ilmenite chelating collector
CN107442295A (en) * 2017-09-28 2017-12-08 四川有色金砂选矿药剂有限公司 Ilmenite collecting agent and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103331212A (en) * 2013-07-12 2013-10-02 武汉工程大学 Carbonate phosphorite reverse flotation collecting agent and preparation method thereof
CN105750091A (en) * 2014-12-16 2016-07-13 乐山顺辰科技有限公司 Mineral floatation colleting agent and manufacturing method thereof

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