CN108745653B - Ilmenite collecting agent and preparation method thereof - Google Patents
Ilmenite collecting agent and preparation method thereof Download PDFInfo
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- CN108745653B CN108745653B CN201810339474.7A CN201810339474A CN108745653B CN 108745653 B CN108745653 B CN 108745653B CN 201810339474 A CN201810339474 A CN 201810339474A CN 108745653 B CN108745653 B CN 108745653B
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- ilmenite
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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
- B03D2203/04—Non-sulfide ores
Abstract
The invention relates to an ilmenite collecting agent and a preparation method thereof, wherein the ilmenite collecting agent comprises the following raw materials in parts by weight: 25-40 parts of styrene phosphonic acid; 4-10 parts of 2-hydroxy-5-nonyl acetophenone oxime; 5-12 parts of a compound surfactant; 35-43 parts of oxidized paraffin soap; 80-95 parts of higher fatty acid soap; 10-20 parts of sodium hydroxide; 10-20 parts of water; wherein the weight ratio of the sodium hydroxide to the water is 1: 0.9-1.2. Compared with the prior art, the invention has the beneficial effects that: the collecting and matching of styrene phosphonic acid and 2-hydroxy-5-nonyl acetophenone oxime and the adoption of the compound surfactant enhance the system stability, so that the collecting capacity of the collecting agent is obviously enhanced, the collecting agent can have better collecting capacity for ilmenite with the particle size below-0.154 mm, the utilization rate of ilmenite resources is improved, the ore grinding standard is reduced, and the production cost is effectively controlled.
Description
Technical Field
The invention belongs to the field of beneficiation reagents, and particularly relates to an ilmenite collecting agent and a preparation method thereof.
Background
The titanium resource of China now occupies the first part of the world, and accounts for about 64 percent of the mined reserve of the world, the reserve accounts for about 48 percent of the titanium reserve of the world, more than 20 provinces, cities and municipalities in China have titanium ores, wherein 98.9 percent of the titanium ores are ilmenite, only about 1 percent of the titanium ores are rutile, the Chinese titanium resource is mainly distributed in the Panxi region, the reserve of the titanium resource (calculated as TiO 2) is 8.7 hundred million tons, accounts for 35.17 percent of the proven reserve of the world, and accounts for more than 90.54 percent of the proven reserve of China. The titanium resource is second to the iron, aluminum and magnesium resources listed in the 4 th position, so the research on the ilmenite flotation, especially the research and application of a flotation reagent, is of great significance.
The traditional ilmenite collecting agent is only suitable for flotation of fine-fraction ilmenite and is not suitable for flotation of coarse-fraction ilmenite. Specifically, the traditional ilmenite collecting agent can only effectively recover ilmenite with the grain size below-0.074 mm, and ilmenite with the grain size above +0.074mm is basically thrown away as tailings, so that in order to improve the ilmenite recovery rate, the grinding time is generally increased to grind the ilmenite below-0.074 mm, and the grinding energy consumption is high, the grinding efficiency is low and the production efficiency is low. Therefore, there is a need to provide a new ilmenite collecting agent, so that the effectively recovered fraction of ilmenite is increased, and ilmenite with coarse fraction (-below 0.154mm fraction) can also be effectively recovered, thereby achieving the purposes of improving ilmenite flotation efficiency, reducing energy consumption and reducing production cost.
Disclosure of Invention
The invention provides an ilmenite collecting agent and a preparation method thereof, and aims to solve the technical problems of resource waste, production cost increase and the like caused by the fact that the ilmenite collecting agent in the prior art cannot effectively recover ilmenite with a relatively large grain size.
The technical scheme for solving the technical problems is as follows: an ilmenite collecting agent is composed of the following raw materials in parts by weight: 25-40 parts of styrene phosphonic acid; 4-10 parts of 2-hydroxy-5-nonyl acetophenone oxime; 5-12 parts of a compound surfactant; 35-43 parts of oxidized paraffin soap; 80-95 parts of higher fatty acid soap; 10-20 parts of sodium hydroxide; 10-20 parts of water; wherein the weight ratio of the sodium hydroxide to the water is 1: 0.9-1.2.
On the basis of the technical scheme, the invention can also have the following specific selection or better scheme.
Specifically, the compound surfactant is prepared by fully mixing an anionic surfactant and a cationic surfactant according to the weight ratio of 1: 0.8-1.2.
The invention relates to a collecting agent for collecting fine ilmenite, which is characterized in that an anion surfactant and a cation surfactant are compounded for the first time to serve as an effective component of the collecting agent, and the compounded surfactant can form more stable bubbles and liquid drops in a solution, so that the effect is lasting during flotation, and the collecting of the collecting agent on the fine ilmenite is enhanced and ensured.
Preferably, the anionic surfactant is sodium octyl sulfate or sodium dodecyl benzene sulfonate, and the cationic surfactant is octyl trimethyl ammonium bromide or octyl trimethyl ammonium chloride.
Most preferably, the compound surfactant is prepared by fully mixing sodium octyl sulfate and octyl trimethyl ammonium chloride according to the weight ratio of 1: 1.
It should be noted that the compound surfactant prepared by fully mixing the sodium octyl sulfate and the octyl trimethyl ammonium chloride according to the weight ratio of 1: 1 has the best effect on enhancing the collecting capacity of the collecting agent, wherein the octyl ammonium trichloride is not only a cationic surfactant, but also a metal extractant, so that the compound surfactant has a better gain effect on collecting ilmenite.
Specifically, the higher fatty acid soap is sodium palmitate or sodium stearate.
On the basis of the technical scheme, the invention also provides a preparation method of the ilmenite collecting agent, which comprises the following steps:
weighing the raw materials according to the weight parts, putting the weighed sodium hydroxide and water into a reaction kettle to mix into a sodium hydroxide aqueous solution, then adding the weighed styrene phosphonic acid and 2-hydroxy-5-nonyl acetophenone oxime, uniformly stirring, then adding the weighed compound surfactant, oxidized paraffin soap and higher fatty acid soap, heating until the fatty acid soap is in a molten state, and uniformly stirring to obtain the high-performance soap.
Compared with the prior art, the invention has the beneficial effects that:
1) the collecting and matching of styrene phosphonic acid and 2-hydroxy-5-nonyl acetophenone oxime and the adoption of the compound surfactant enhance the system stability, so that the collecting capability of the collecting agent is obviously enhanced, the collecting agent can have better collecting capability on ilmenite with the particle size below-0.154 mm, the utilization rate of ilmenite resources is improved, the ore grinding standard is reduced, and the production cost is effectively controlled;
2) all raw materials contained in the collecting agent have the characteristics of low price and easy obtainment, and the production method is simple and easy for large-scale production.
Detailed Description
The technical solutions provided by the present invention are further described in detail with reference to the following specific embodiments, which are only used for explaining the present invention and are not used for limiting the scope of the present invention.
In order to avoid redundancy, the medicaments used in the following examples and comparative examples are all commercial products unless otherwise specified, and the methods used are conventional methods adopted in the art unless otherwise specified.
Example 1
An ilmenite collecting agent, which is prepared by the following method:
respectively weighing 150Kg of water, 160Kg of sodium hydroxide, 360Kg of styrene phosphonic acid, 80Kg of 2-hydroxy-5-nonyl acetophenone oxime, 390Kg of oxidized paraffin soap, 860Kg of sodium stearate, 40Kg of octyl sodium sulfate and 40Kg of octyl trimethyl ammonium chloride, putting the weighed sodium hydroxide and water into a reaction kettle to mix into a sodium hydroxide aqueous solution, then adding the weighed styrene phosphonic acid and the 2-hydroxy-5-nonyl acetophenone oxime, uniformly stirring, then adding the weighed complex surfactant, the oxidized paraffin soap and the higher fatty acid soap, heating until the fatty acid soap is in a molten state, and uniformly stirring to obtain the compound surfactant.
Example 2
An ilmenite collecting agent, which is prepared by the following method:
respectively weighing 120Kg of water, 100Kg of sodium hydroxide, 250Kg of styrene phosphonic acid, 40Kg of 2-hydroxy-5-nonyl acetophenone oxime, 350Kg of oxidized paraffin soap, 800Kg of sodium stearate, 25Kg of sodium octyl sulfate and 25Kg of octyl trimethyl ammonium chloride, putting the weighed sodium hydroxide and water into a reaction kettle to mix into a sodium hydroxide aqueous solution, then adding the weighed styrene phosphonic acid and the 2-hydroxy-5-nonyl acetophenone oxime, uniformly stirring, then adding the weighed complex surfactant, the oxidized paraffin soap and the higher fatty acid soap, heating until the fatty acid soap is in a molten state, and uniformly stirring to obtain the compound surfactant.
Example 3
An ilmenite collecting agent, which is prepared by the following method:
respectively weighing 240Kg of water, 200Kg of sodium hydroxide, 400Kg of styrene phosphonic acid, 100Kg of 2-hydroxy-5-nonyl acetophenone oxime, 430Kg of oxidized paraffin soap, 950Kg of sodium stearate, 60Kg of sodium octyl sulfate and 60Kg of octyl trimethyl ammonium chloride, putting the weighed sodium hydroxide and water into a reaction kettle to mix into a sodium hydroxide aqueous solution, then adding the weighed styrene phosphonic acid and the 2-hydroxy-5-nonyl acetophenone oxime, uniformly stirring, then adding the weighed complex surfactant, the oxidized paraffin soap and the higher fatty acid soap, heating until the fatty acid soap is in a molten state, and uniformly stirring to obtain the compound surfactant.
Example 4
An ilmenite collecting agent, which is prepared by the following method:
respectively weighing 117Kg of water, 130Kg of sodium hydroxide, 380Kg of styrene phosphonic acid, 60Kg of 2-hydroxy-5-nonyl acetophenone oxime, 350Kg of oxidized paraffin soap, 820Kg of sodium palmitate, 50Kg of sodium dodecyl sulfate and 50Kg of octyl trimethyl ammonium bromide, putting the weighed sodium hydroxide and water into a reaction kettle to mix into a sodium hydroxide aqueous solution, then adding the weighed styrene phosphonic acid and 2-hydroxy-5-nonyl acetophenone oxime, uniformly stirring, then adding the weighed complex surfactant, oxidized paraffin soap and higher fatty acid soap, heating until the fatty acid soap is in a molten state, and uniformly stirring to obtain the compound surfactant.
Example 5
An ilmenite collecting agent, which is prepared by the following method:
respectively weighing 180Kg of water, 180Kg of sodium hydroxide, 300Kg of styrene phosphonic acid, 40Kg of 2-hydroxy-5-nonyl acetophenone oxime, 430Kg of oxidized paraffin soap, 900Kg of sodium stearate, 55Kg of sodium octyl sulfate and 55Kg of octyl trimethyl ammonium bromide, putting the weighed sodium hydroxide and water into a reaction kettle to mix into a sodium hydroxide aqueous solution, then adding the weighed styrene phosphonic acid and the 2-hydroxy-5-nonyl acetophenone oxime, uniformly stirring, then adding the weighed complex surfactant, the oxidized paraffin soap and the high-grade fatty acid soap, heating until the fatty acid soap is in a molten state, and uniformly stirring to obtain the compound surfactant.
Comparative example 1
Compared with example 1, the compound does not contain 2-hydroxy-5-nonyl acetophenone oxime.
Comparative example 2
The contents of sodium octyl sulfate and octyl trimethyl ammonium chloride are different only compared to example 1, in this comparative example the content of sodium octyl sulfate is 80Kg and the content of octyl trimethyl ammonium chloride is zero.
Comparative example 3
The contents of sodium octyl sulfate and octyl trimethyl ammonium chloride are different only compared to example 1, the content of sodium octyl sulfate is zero and the content of octyl trimethyl ammonium chloride is 80Kg in this comparative example.
The collectors obtained in examples 1 to 5 and comparative examples 1 to 3 were used to perform flotation on a batch of ilmenite samples (the raw ore contains 18.15 wt% of titanium dioxide) divided into several portions, and standard methods were used in the flotation, including the steps of grinding, size mixing, adding the corresponding collector, and the like, and finally the content of titanium dioxide in the ilmenite concentrate obtained by flotation and the recovery rate of titanium dioxide were calculated, as shown in the following table:
in addition, after the tailings are carefully analyzed, the tailings after flotation by using the collectors in the examples 1 to 5 are found to have less content of the active ingredients of the ilmenite with the size fraction ranging from +0.077mm to-0.154 mm in the corresponding tailings, namely the tailings are effectively collected; the ilmenite collecting agent provided by the invention can effectively collect ilmenite with a relatively large size fraction, so that the grade of the ilmenite concentrate is improved, and the recovery rate is improved.
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 (4)
1. An ilmenite collecting agent is characterized by comprising the following raw materials in parts by weight: 25-40 parts of styrene phosphonic acid; 4-10 parts of 2-hydroxy-5-nonyl acetophenone oxime; 5-12 parts of a compound surfactant; 35-43 parts of oxidized paraffin soap; 80-95 parts of higher fatty acid soap; 10-20 parts of sodium hydroxide; 10-20 parts of water; wherein the weight ratio of the sodium hydroxide to the water is 1: 0.9-1.2, the compound surfactant is prepared by fully mixing an anionic surfactant and a cationic surfactant according to the weight ratio of 1: 0.8-1.2, the anionic surfactant is sodium octyl sulfate or sodium dodecyl benzene sulfonate, and the cationic surfactant is octyl trimethyl ammonium bromide or octyl trimethyl ammonium chloride.
2. An ilmenite collector according to claim 1, wherein the compounded surfactant is formed by thoroughly mixing sodium octyl sulfate and octyl trimethyl ammonium chloride in a weight ratio of 1: 1.
3. An ilmenite collector according to claim 1 or claim 2, wherein the higher fatty acid soap is sodium palmitate or sodium stearate.
4. A method of producing an ilmenite collector according to any one of claims 1 to 3, characterized by comprising the steps of:
weighing the raw materials according to the parts by weight, putting the weighed sodium hydroxide and water into a reaction kettle to mix into a sodium hydroxide aqueous solution, then adding the weighed styrene phosphonic acid and 2-hydroxy-5-nonyl acetophenone oxime, uniformly stirring, then adding the weighed compound surfactant, oxidized paraffin soap and higher fatty acid soap, heating until the fatty acid soap is in a molten state, and uniformly stirring to obtain the high-performance soap.
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| CN201810339474.7A CN108745653B (en) | 2018-04-16 | 2018-04-16 | Ilmenite collecting agent and preparation method thereof |
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| CN201810339474.7A CN108745653B (en) | 2018-04-16 | 2018-04-16 | Ilmenite collecting agent and preparation method thereof |
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| CN108745653A CN108745653A (en) | 2018-11-06 |
| CN108745653B true CN108745653B (en) | 2020-07-14 |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5106489A (en) * | 1991-08-08 | 1992-04-21 | Sierra Rutile Limited | Zircon-rutile-ilmenite froth flotation process |
| CN1371358A (en) * | 1999-08-12 | 2002-09-25 | 科金斯公司 | Method for separating copper from iron |
| CN104069950A (en) * | 2014-07-11 | 2014-10-01 | 汉中天泰商贸有限公司 | Environment-friendly ilmenite collecting agent and preparation method thereof |
| CN105602537A (en) * | 2014-11-18 | 2016-05-25 | 墨西哥石油研究院 | Multifunctional foaming composition |
| CN105880034A (en) * | 2016-04-22 | 2016-08-24 | 北京矿冶研究总院 | Ilmenite chelating collector |
| CN106238219A (en) * | 2016-08-19 | 2016-12-21 | 武汉工程大学 | A kind of ilmenite flotation collector and its preparation method and application |
| CN107617510A (en) * | 2017-09-28 | 2018-01-23 | 攀钢集团矿业有限公司 | A kind of floating agent and its application |
-
2018
- 2018-04-16 CN CN201810339474.7A patent/CN108745653B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5106489A (en) * | 1991-08-08 | 1992-04-21 | Sierra Rutile Limited | Zircon-rutile-ilmenite froth flotation process |
| CN1371358A (en) * | 1999-08-12 | 2002-09-25 | 科金斯公司 | Method for separating copper from iron |
| CN104069950A (en) * | 2014-07-11 | 2014-10-01 | 汉中天泰商贸有限公司 | Environment-friendly ilmenite collecting agent and preparation method thereof |
| CN105602537A (en) * | 2014-11-18 | 2016-05-25 | 墨西哥石油研究院 | Multifunctional foaming composition |
| CN105880034A (en) * | 2016-04-22 | 2016-08-24 | 北京矿冶研究总院 | Ilmenite chelating collector |
| CN106238219A (en) * | 2016-08-19 | 2016-12-21 | 武汉工程大学 | A kind of ilmenite flotation collector and its preparation method and application |
| CN107617510A (en) * | 2017-09-28 | 2018-01-23 | 攀钢集团矿业有限公司 | A kind of floating agent and its application |
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| CN108745653A (en) | 2018-11-06 |
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Effective date of registration: 20200930 Address after: 434400 west side of Jinyin Road, Jinping Industrial Park, Shishou Economic Development Zone, Jingzhou City, Hubei Province Patentee after: Hubei Hongqiang Mining Technology Co.,Ltd. Address before: 434400 Jingzhou City, Hubei province Shishou City Road No. 18 Peach Peach Town Jingjiang Office Patentee before: HUBEI JINGJIANG FLOTATION REAGENTS Co.,Ltd. |
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Effective date of registration: 20210304 Address after: 434400 Jingjiang office, No.18 Taohuashan Road, Taohuashan Town, Shishou City, Jingzhou City, Hubei Province Patentee after: HUBEI JINGJIANG FLOTATION REAGENTS CO.,LTD. Address before: 434400 west of Jinyin Road, Jinping Industrial Park, Shishou Economic Development Zone, Jingzhou City, Hubei Province Patentee before: Hubei Hongqiang Mining Technology Co.,Ltd. |
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Effective date of registration: 20220817 Address after: 434400 west of Jinyin Road, Jinping Industrial Park, Shishou Economic Development Zone, Jingzhou City, Hubei Province Patentee after: Hubei Hongqiang Mining Technology Co.,Ltd. Address before: 434400 Jingjiang office, No.18 Taohuashan Road, Taohuashan Town, Shishou City, Jingzhou City, Hubei Province Patentee before: HUBEI JINGJIANG FLOTATION REAGENTS CO.,LTD. |