CN113289767A - Micro-fine particle rutile efficient combined collector and preparation method and application thereof - Google Patents

Micro-fine particle rutile efficient combined collector and preparation method and application thereof Download PDF

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Publication number
CN113289767A
CN113289767A CN202110570245.8A CN202110570245A CN113289767A CN 113289767 A CN113289767 A CN 113289767A CN 202110570245 A CN202110570245 A CN 202110570245A CN 113289767 A CN113289767 A CN 113289767A
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rutile
collector
flotation
combined collector
micro
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黄红军
刘芳芳
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Central South University
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Central South University
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Priority to ZA2021/08417A priority patent/ZA202108417B/en
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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
    • B03D1/004—Organic compounds
    • B03D1/008—Organic compounds containing oxygen
    • 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
    • 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
    • B03D2201/04—Frothers
    • 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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  • Manufacture And Refinement Of Metals (AREA)

Abstract

The invention belongs to the technical field of rutile flotation, and particularly relates to a micro-fine particle rutile efficient combined collector and a preparation method and application thereof. The invention takes the lauryl citrate with better rutile selectivity as a main collector, and takes linolenic acid, dodecylamine bis-methylphosphonic acid and butyl ether oil as auxiliary collectors. Dodecyl citrate in the high-efficiency combined collector: linolenic acid: dodecylamine bis (methylphosphonic acid): the proportion of the butyl ether oil is 5:2:2:1, the efficient combined collector can improve the grade of the rutile concentrate obtained by separation and ensure the recovery rate, and has important significance for improving the recovery and utilization of titanium resources.

Description

Micro-fine particle rutile efficient combined collector and preparation method and application thereof
Technical Field
The invention belongs to the technical field of rutile flotation, and particularly relates to a micro-fine particle rutile efficient combined collector and a preparation method and application thereof.
Background
Rutile is one of the raw materials for extracting titanium metal and producing high-grade welding rod and rutile type titanium dioxide. However, most of rutile ores in China are low-grade primary ores, the reserves of the rutile ores account for 86% of rutile resources in China, the rutile ores are fine in granularity and extremely complex in embedding arrangement, and associated silico-calcic gangue minerals are difficult to remove and sort. Flotation is the most common process for rutile separation and is mostly used for treating low-grade and embedded fine rutile, so that a flotation process is inevitably used for obtaining high-grade and high-recovery rutile concentrate from primary rutile ores.
Collectors commonly used for rutile flotation mainly contain fatty acids, arsonic acids, phosphonic acids, hydroximic acids. The fatty acid collector is widely applied to flotation of oxidized ores such as rutile and the like, and has the outstanding advantages of good collecting performance but poor selectivity. The arsinic acid collector has high toxicity and thus cannot be widely used in practical production. Phosphonic acid collectors have better selectivity in the process of flotation of rutile, but the cost of the collectors is higher. The hydroximic acid collecting agent is mainly salicylhydroxamic acid and hydroximic acid containing 7-9 carbon atoms, has better collecting capability to rutile, but is expensive.
Therefore, the conventional rutile flotation agent has poor rutile flotation effect, is harmful to the environment and cannot realize efficient utilization of titanium resources.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to solve the defects of poor flotation effect and unfriendliness to the environment of the rutile flotation agent; according to the invention, the lauryl citrate with high rutile collecting capability is adopted, the combination of linolenic acid and dodecylamine diphosphonic acid with selectivity and collecting capability is selected, and the butyl ether oil is matched, so that the flotation effect is better in the flotation process.
In order to realize the aim, the invention provides a micro-fine particle rutile efficient combined collector which is composed of a main collector, namely lauryl citrate, an auxiliary collector, namely linolenic acid, dodecylamine dimethyl phosphonic acid and butyl ether oil.
Further, the mass ratio of the lauryl citrate to the linolenic acid to the dodecylamine dimethyl phosphonate to the butyl ether oil is 5:1-3:1-3: 1-2; the mass ratio of the lauryl citrate to the linolenic acid to the dodecylamine bis-methylphosphonic acid to the butyl ether oil is preferably 5:2:2: 1.
Based on the same inventive concept, the embodiment of the invention also provides a preparation method of the micro-fine particle rutile efficient combined collector, which is obtained by uniformly mixing lauryl citrate, linolenic acid, dodecylamine bis-methylphosphonic acid, butyl ether oil and water to obtain a mixture, and then fully stirring and dispersing the mixture in a stirrer.
Further, the conditions for stirring and dispersing the high-efficiency combined collector are as follows: the rotating speed is 1000-.
Based on the same inventive concept, the embodiment of the invention also provides an application of the micro-fine particle rutile efficient combined collector in the flotation of rutile, and the application method specifically comprises the following steps:
adding the micro-fine rutile into a pH regulator, an inhibitor, an activator and a high-efficiency combined collector for roughing to obtain rough concentrate and rough tailings;
scavenging the coarse tailings to obtain coarse middlings, and returning the coarse middlings to the roughing process;
and (3) carrying out concentration on the rough concentrate for at least 5 times to obtain rutile concentrate, wherein the concentration process comprises at least two times of concentration by adding a pH regulator, an inhibitor, an activator and a high-efficiency combined collector, and concentration without adding any flotation agent.
Further, the application method further comprises: the fine middlings obtained in the concentration process are returned to the last stage of flotation as feed.
Further, the pH regulator is sulfuric acid; the inhibitor is one or more selected from sodium fluosilicate, water glass and sodium hexametaphosphate; the activating agent is lead nitrate.
Has the advantages that:
according to the invention, lauryl citrate with strong collecting capacity is taken as a main collector, linolenic acid with selectivity and collecting capacity and dodecylamine bis-methylphosphonic acid are added as auxiliary collectors, and an ether foaming agent butyl ether oil and linolenic acid are interacted, so that the critical concentration and surface activity generated by colloidal particles are further improved.
Drawings
FIG. 1 is a flow chart of the flotation process for fine rutile ore provided in example 3 of the present invention.
Detailed Description
In order to make the technical problems, technical solutions and advantages of the present invention more apparent, the following detailed description is given with reference to specific embodiments, but the scope of the present invention is not limited to the following specific embodiments.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
Example 1
The ore blend used in this example was prepared from rutile and quartz in a ratio of 1: 1, the dosage of each time is 2g, wherein the mineral powder of rutile and quartz has a particle size of not more than 0.074mm and accounts for more than 90%.
Preparing a high-efficiency combined collecting agent: the preparation method comprises the steps of mixing lauryl citrate, linolenic acid, dodecylamine dimethyl phosphonate and butyl ether oil according to the mass ratio of 5:2:2:1, adding water, uniformly mixing to obtain a mixture, and stirring and dispersing the mixture in a stirrer at the rotating speed of 1000r/min for 15min to obtain the product.
Artificial mixed ore flotation experiment: adding sulfuric acid to adjust the pH value of the ore pulp to 5, then respectively adding 1000g/t of inhibitor (sodium fluosilicate: water glass: sodium hexametaphosphate is 7: 2: 1), 1000g/t of lead nitrate and 800g/t of efficient combined collector, and after 3min of flotation, calculating the recovery rate of rutile. The recovery rate of rutile in the concentrate is more than 90%, and the recovery rate of quartz is less than 10%, which indicates that the efficient combined collector can selectively collect and float rutile.
Comparative example 1
In the preparation process of the high-efficiency combined collector in example 1, the ratio of lauryl citrate: linolenic acid: dodecylamine bis (methylphosphonic acid): the mass ratio of the butyl ether oil is 2: 5:2: the other preparation process is exactly the same as that of example 1, and combined collector 1 is obtained and floated according to the artificial mixed ore flotation experiment of example 1. The flotation result is as follows: the recovery rate of the rutile in the concentrate is lower than 70 percent, and the recovery rate of the quartz is higher than 15 percent.
Comparative example 2
In the preparation process of the high-efficiency combined collector in example 1, the ratio of lauryl citrate: linolenic acid: dodecylamine bis (methylphosphonic acid): the mass ratio of the butyl ether oil is 2:2: 5: the other preparation process is completely the same as that of the example 1, the combined collector 2 is obtained, and the artificial mixed ore flotation experiment of the example 1 is carried out for flotation. The flotation result is as follows: the recovery rate of the rutile in the concentrate is lower than 65%, and the recovery rate of the quartz is higher than 19%.
From the above example 1 and comparative examples 1 and 2, it can be seen that the ratio of each substance of the high-efficiency combined collector in the present application has a great influence on the collecting effect of rutile, and when the ratio of each raw material in the collector is out of the range of the present invention, the collecting effect of rutile is greatly reduced, and the selectivity is also reduced.
Example 2
The ore sample used in this example was taken from a rutile ore from Sichuan, the average titanium grade was 4.12%, and the ore powder particle size after crushing and grinding was not more than 0.074mm accounted for more than 90%.
In the flotation of the high-efficiency combined collector obtained in example 1, sulfuric acid is firstly added to adjust the pH value of ore pulp to 5, then 1000g/t of inhibitor (sodium fluosilicate: water glass: sodium hexametaphosphate: 7: 2: 1), 1000g/t of lead nitrate and 800g/t of high-efficiency combined collector are respectively added, and the recovery rate of rutile is calculated after 3min of flotation. The grade of the rutile in the concentrate is 19.45 percent, and the recovery rate is 71.02 percent.
Comparative example 3
The same ore sample as in example 2 was subjected to flotation, and the combined collector 1 obtained in comparative example 1 was used as a flotation agent to perform a flotation experiment, and the flotation process was completely the same as in example 2. The results show that the grade of rutile in the concentrate is 13.70%, and the recovery rate is 65.96%.
Comparative example 4
The same ore sample as in example 2 was subjected to flotation, and the combined collector 2 obtained in comparative example 2 was used as a flotation agent to perform a flotation experiment, and the flotation process was completely the same as in example 2. The results show that the grade of rutile in the concentrate is 11.40%, and the recovery rate is 66.82%.
Comparative example 5
In the preparation process of the high-efficiency combined collector in the example 1, the composition of the collector is modified into that of linolenic acid: dodecylamine bis (methylphosphonic acid): the mass ratio of the butyl ether oil is 4: 4: the other preparation process was exactly the same as example 1 to obtain a combined collector 3. The combined collector 3 was subjected to flotation on the same sample as in example 2, the flotation process was completely the same as in example 2, and the result showed that the grade of rutile in the concentrate was 12.57% and the recovery rate was 60.15%.
Comparative example 6
In the preparation process of the high-efficiency combined collector in example 1, the composition of the collector is modified to be dodecyl citrate: dodecylamine bis (methylphosphonic acid): the proportion of the butyl ether oil is 6.25: 2.5: 1.25, the other preparation process was exactly the same as example 1 to obtain the combined collector 4. The combined collector 4 was subjected to flotation on the same ore sample as in example 2, the flotation process was completely the same as in example 2, and the result showed that the grade of rutile in the concentrate was 10.44% and the recovery rate was 63.36%.
Comparative example 7
In the preparation process of the high-efficiency combined collector in example 1, the composition of the collector is modified to be dodecyl citrate: linolenic acid: the proportion of the butyl ether oil is 6.25: 2.5: 1.25, the other preparation process was exactly the same as example 1 to obtain the combined collector 5. The combined collector 5 was subjected to flotation on the same ore sample as in example 2, the flotation process was completely the same as in example 2, and the result showed that the grade of rutile in the concentrate was 13.18% and the recovery rate was 63.29%.
Comparative example 8
The same ore sample as in example 2 was subjected to flotation, and a flotation experiment was performed using benzohydroxamic acid as the flotation agent, and the flotation process was completely the same as in example 2. The results show that the grade of rutile in the concentrate is 11.56% and the recovery is 65.27%.
From the example 2 and the comparative examples 3 to 8, it can be seen that the lack of the raw materials of the efficient combined collector or the change of the proportion of the raw materials has a great influence on the collecting effect of the rutile, and when the efficient combined collector of the invention lacks any raw materials, the collecting effect is greatly reduced, which indicates that the raw materials of the collector have a synergistic effect on a rutile collecting system and is an organic whole. Compared with the embodiment 2 and the comparative example 8, the efficient combined collector has a better collecting effect than a benzohydroxamic acid collector, the grade of the obtained rutile ore is improved, and the recovery rate is greatly increased.
Example 3
The ore sample used in this example was the same as that used in example 2, and a flotation process flow experiment was performed on this fine particle rutile real ore.
The total dosage of the flotation reagent is as follows:
inhibitor (B): roughing at 1000g/t, scavenging at 500g/t, concentrating at 300g/t +100g/t +30 g/t;
activating agent: roughing at 1000g/t, scavenging at 500g/t, concentrating at 300g/t +100g/t +30 g/t;
high-efficiency combined collecting agent: roughing at 800g/t, scavenging at 400g/t, concentrating at 250g/t +100g/t +30 g/t;
the operation steps and technical conditions are as follows:
the fine rutile ore used in this example had a particle size of not more than 0.074mm accounting for 90% or more.
Sodium fluosilicate in the inhibitor: water glass: sodium hexametaphosphate ═ 7: 2: 1. the preparation method of the efficient combined collector comprises the steps of uniformly mixing a certain amount of lauryl citrate, linolenic acid, dodecylamine bis-methylphosphonic acid, butyl ether oil and water to obtain a mixture, and then stirring and dispersing the mixture in a stirrer at the rotating speed of 1000r/min for 15min to obtain the efficient combined collector. Dodecyl citrate in the efficient combined collector in any sorting process: linolenic acid: dodecylamine bis (methylphosphonic acid): butyl ether oil 5:2:2: 1. the method comprises the steps of sequentially adding a pH regulator, an inhibitor, an activating agent and a high-efficiency combined collecting agent in the roughing and scavenging processes, sequentially adding the pH regulator, the inhibitor and a novel high-efficiency combined medicament in the first three-time concentration in the concentration process, and not adding any flotation medicament in the 4 th and 5 th concentration processes. The pH value of the ore pulp is 5 during flotation, and each flotation is carried out for 3 min. Any middlings produced during the sorting process are returned in sequence.
According to the process parameters, a rough-five-fine-one-sweep flotation closed circuit test is carried out, and TiO2 grade is 4.12 percent under the condition of ore feeding TiO2 grade2The grade is 47.83 percent, and the recovery rate is 58.75 percent of rutile concentrate.
Therefore, according to the application method of the high-efficiency combined collecting agent in the rutile ore flotation, the TiO in the ore can be greatly improved2The grade of the titanium is ensured, the recovery rate is ensured, and the recovery and utilization of the titanium resource are improved.
The above-mentioned embodiments are only preferred embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered as the technical scope of the present invention, and equivalents and modifications of the technical solutions and concepts of the present invention should be covered by the scope of the present invention.

Claims (8)

1. The efficient combined collector is characterized by consisting of a main collector lauryl citrate, an auxiliary collector linolenic acid, dodecylamine bis-methylphosphonic acid and butyl ether oil.
2. The micro-fine particle rutile high-efficiency combined collector of claim 1, wherein the mass ratio of lauryl citrate, linolenic acid, dodecylamine bis-methylphosphonic acid and butyl ether oil is 5:1-3:1-3: 1-2.
3. The micro-fine particle rutile high-efficiency combined collector of claim 1, wherein the mass ratio of lauryl citrate, linolenic acid, dodecylamine bis-methylphosphonic acid and butyl ether oil is 5:2:2: 1.
4. A preparation method of a micro-fine particle rutile efficient combined collector is characterized by uniformly mixing lauryl citrate, linolenic acid, dodecylamine bis-methylphosphonic acid, butyl ether oil and water to obtain a mixture, and then fully stirring and dispersing the mixture in a stirrer to obtain the micro-fine particle rutile efficient combined collector.
5. The preparation method of the micro-fine particle rutile high-efficiency combined collector according to claim 4, wherein the conditions for stirring and dispersing the high-efficiency combined collector are as follows: the rotating speed is 1000-.
6. The application of the micro-fine particle rutile efficient combined collector in the flotation of rutile is characterized by specifically comprising the following steps:
adding the micro-fine rutile into a pH regulator, an inhibitor, an activator and a high-efficiency combined collector for roughing to obtain rough concentrate and rough tailings;
scavenging the coarse tailings to obtain coarse middlings, and returning the coarse middlings to the roughing process;
and (3) carrying out concentration on the rough concentrate for at least 5 times to obtain rutile concentrate, wherein the concentration process comprises at least two times of concentration by adding a pH regulator, an inhibitor, an activator and a high-efficiency combined collector, and concentration without adding any flotation agent.
7. The use of a finely particulate rutile high efficiency combination collector according to claim 6 in flotation of rutile, wherein the method of use further comprises:
the fine middlings obtained in the concentration process are returned to the last stage of flotation as feed.
8. The use of a microfine particle rutile high efficiency combination collector of claim 6 in flotation of rutile, wherein the pH modifier is sulfuric acid; the inhibitor is one or more selected from sodium fluosilicate, water glass and sodium hexametaphosphate; the activating agent is lead nitrate.
CN202110570245.8A 2021-05-25 2021-05-25 Micro-fine particle rutile efficient combined collector and preparation method and application thereof Pending CN113289767A (en)

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CN202110570245.8A CN113289767A (en) 2021-05-25 2021-05-25 Micro-fine particle rutile efficient combined collector and preparation method and application thereof
ZA2021/08417A ZA202108417B (en) 2021-05-25 2021-10-29 Efficient combined collector for micro-fine rutile, and preparation method and use thereof

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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AU2009267003A1 (en) * 2008-07-02 2010-01-07 Georgia-Pacific Chemicals Llc Collectors
CN105665146A (en) * 2016-03-04 2016-06-15 中南大学 Method for improving rate of recovery of floatation of rutile
CN106925435A (en) * 2017-04-07 2017-07-07 武汉理工大学 A kind of method for reclaiming rutile
CN107694762A (en) * 2017-11-10 2018-02-16 中南大学 A kind of composition and method for floating of the flotation collecting rutile from ore

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5173176A (en) * 1990-02-23 1992-12-22 The Dow Chemical Company Dialkylated aryl monosulfonate collectors useful in the flotation of minerals
AU2009267003A1 (en) * 2008-07-02 2010-01-07 Georgia-Pacific Chemicals Llc Collectors
CN105665146A (en) * 2016-03-04 2016-06-15 中南大学 Method for improving rate of recovery of floatation of rutile
CN106925435A (en) * 2017-04-07 2017-07-07 武汉理工大学 A kind of method for reclaiming rutile
CN107694762A (en) * 2017-11-10 2018-02-16 中南大学 A kind of composition and method for floating of the flotation collecting rutile from ore

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
尹伟: "黑钨、金红石和锡石的新型捕收剂的分子设计合成及其捕收性能的研究", 《广东教育学院学报》 *
朱建光: "浮选金红石用的捕收剂和调整剂", 《国外金属矿选矿》 *
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