CN111530637B - Collecting agent for mineral flotation and preparation method and application thereof - Google Patents
Collecting agent for mineral flotation and preparation method and application thereof Download PDFInfo
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- CN111530637B CN111530637B CN202010388383.XA CN202010388383A CN111530637B CN 111530637 B CN111530637 B CN 111530637B CN 202010388383 A CN202010388383 A CN 202010388383A CN 111530637 B CN111530637 B CN 111530637B
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- alcohol
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- fatty acid
- collector
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D1/00—Flotation
- B03D1/001—Flotation agents
- B03D1/018—Mixtures of inorganic and organic compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D2201/00—Specified effects produced by the flotation agents
- B03D2201/02—Collectors
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D2203/00—Specified materials treated by the flotation agents; specified applications
- B03D2203/02—Ores
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- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Removal Of Floating Material (AREA)
Abstract
The invention discloses a collector for mineral flotation, which comprises the following components in percentage by mass: 1-35% of nonpolar oil, 1-35% of an activating agent and 64-95% of a supplementary liquid; the activating agent is a reactant obtained after esterification reaction of fatty acid and alcohol, and the supplementary liquid is a salt solution. The invention also discloses a preparation method and application of the collector, and when the collector is used for mineral flotation, the nonpolar oil acts on the change of the physical properties of the mineral surface; the activating agent and the supplementary liquid are used for bridging different mineral particle interfaces and mineral particle and bubble interfaces, so that the traditional collecting agent with the same effect is directionally replaced, the effect of greatly reducing the consumption of the nonpolar oil is integrally realized, and the cost of the activating agent and the supplementary liquid is far lower than that of the nonpolar oil, so that the cost of the collecting agent can be greatly reduced.
Description
Technical Field
The invention belongs to the field of chemical assistants, and particularly relates to a mineral foam flotation collector and a preparation method thereof
Background
The flotation selectively separates the solid particle mixture in a gas-liquid-solid three-phase system by utilizing the surface property difference of different mineral particles. Bubbles are blown into the system, mineral particles with stronger surface hydrophobicity (hydrophily) are preferentially adsorbed on the surfaces of the bubbles and float to the liquid surface along with the bubbles to form a foam layer enriched with specific types of mineral particles, while the mineral particles with stronger hydrophilicity and the bubbles have weaker adsorption degree, and most of the mineral particles are settled to the bottom of the liquid. Through the process, the purpose of separating solid particles with different properties is achieved.
The collecting agent is usually added in the flotation process, the collecting agent can be dispersed into countless small drops in a liquid medium under the action of mechanical stirring, the small drops can be combined with specific types of mineral particles and spread on the surface of the mineral particles to form a film, the surface hydrophobicity of the mineral particles is enhanced, and the adsorption of the mineral particles and bubbles is selectively promoted, so that the separation efficiency of flotation is improved.
Collectors commonly used in the prior art are non-polar oils such as: the essential effect of the collector on the surface of the mineral particles is mainly determined by the surface interface property of a layer of oil film formed by spreading the collector on the surface of the mineral particles, such as kerosene, diesel oil or paraffin oil. However, in the froth flotation process, the collecting agent has only a small proportion of oil film with a plurality of molecular layer thicknesses formed by spreading on the surface of mineral particles, and the rest most of collecting agent is filled in the cavity surrounded by the surfaces of the mineral particles adhered to each other and the cavity between the mineral particles and bubbles adhered to the mineral particles, so that the collecting agent plays a role in connecting different mineral particle interfaces and mineral particle and bubble interfaces, but simultaneously, a large amount of collecting agent is required for bridging action rather than surface modification energy supply, and the using amount of the collecting agent is increased. Chinese patent CN101982241B discloses an emulsified diesel oil collecting agent and a preparation method thereof, and the emulsified diesel oil collecting agent with high stability, good selectivity and high yield is prepared for coal slime flotation. However, the collecting agent needs a large amount of diesel oil, and the mass fraction of the diesel oil in the emulsified diesel oil collecting agent is as high as 21.5-26.5%, so that the emulsified diesel oil collecting agent is high in cost and difficult to be applied in a large scale. Therefore, factors such as selectivity of flotation collector to specific mineral, the amount of collector used, etc. are problems that limit the large scale application of collector in practical industrial processes. The research on the flotation collecting agent with low cost and excellent performance is a difficult point in the field of chemical auxiliary agents.
The present invention has been made to solve the above problems.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a flotation collector and a using method thereof. The flotation collector prepared by the method has the characteristics of strong selectivity and high yield, and can realize the same mineral foam flotation effect with extremely low medicament cost compared with the traditional collector.
The invention provides in a first aspect a collector for mineral flotation, comprising, on a mass percent basis:
1-35% of nonpolar oil, 1-35% of an activating agent and 64-95% of a supplementary liquid;
the activating agent is a reactant obtained after esterification reaction of fatty acid and alcohol, and the supplementary liquid is a salt solution.
Preferably, the non-polar oil comprises one or more of kerosene, diesel oil, light cycle oil, paraffin oil, decant oil, coal-based mineral oil, coal tar.
Preferably, the salt solution is an inorganic salt solution, an organic salt solution or a salt solution prepared by mixing an inorganic salt and an organic salt; the inorganic salt is selected from one or more of sodium chloride, potassium chloride, sodium sulfate, potassium sulfate, sodium nitrate or potassium nitrate; the organic salt is selected from one or more of sodium alkyl phenol ether sulfosuccinate, triethanolamine oleate soap, potassium phenol ether phosphate, potassium isotridecanol ether phosphate or potassium lauryl phosphate.
Preferably, the fatty acid comprises one or more of stearic acid, palmitic acid, oleic acid and dodecanoic acid, and the alcohol comprises a polyol selected from one or more of a diol, a triol, a diol polymer or a triol polymer, i.e. the alcohol before esterification of the fatty acid with the alcohol is a polyol.
Among them, when the alcohol before the esterification reaction of the fatty acid with the alcohol is a polyhydric alcohol, it is preferable that the reactant obtained after the esterification reaction of the fatty acid with the alcohol contains at least one monoester compound of a fatty acid polyhydric alcohol.
More preferably, the alcohols further include monohydric alcohols selected from one or more of allyl alcohol, 4-methyl-1-cyclohexanol, cyclohexylmethanol, 2-decanol, α -terpineol, or 2-ethylhexanol, i.e., the alcohols before esterification of the fatty acids with the alcohols are a mixture of polyhydric and monohydric alcohols.
Wherein, when the alcohol before the esterification reaction of fatty acid and alcohol is the mixture of polyhydric alcohol and monohydric alcohol, both the polyhydric alcohol and monohydric alcohol have esterification reaction with fatty acid, the obtained reactant at least contains a monoester compound of fatty acid polyhydric alcohol and a monohydric alcohol, the monohydric alcohol in the reaction product is incompletely reacted monohydric alcohol, and the reaction product may also include polyester compound of fatty acid polyhydric alcohol and esterified compound of fatty acid monohydric alcohol.
In a second aspect, the invention provides a method for preparing the collector, which comprises the following steps:
(1) carrying out esterification reaction on fatty acid and alcohol to obtain a reaction product, filtering the reaction product and collecting supernatant to obtain the activating agent;
(2) and (2) adding the nonpolar oil and the activating agent obtained in the step (1) into a reactor, stirring and mixing, adding a supplementary liquid, and stirring and mixing to obtain the collecting agent.
Preferably, in the step (1), the reaction temperature is 60-120 ℃, preferably 60-96 ℃, the reaction temperature is controlled to control the reaction product after the fatty acid and the alcohol are subjected to esterification reaction, and the reaction product mainly comprises a monoester compound of fatty acid polyol and incompletely reacted monohydric alcohol. The purpose of controlling the temperature is to control the reaction product, and besides, the method commonly used in the prior art for controlling the reaction product of the esterification reaction of fatty acid and alcohol, or the method for judging the type of the reaction product can be used in the patent. In addition, whether the esterification reaction is ended or not can be judged according to common means such as 'no water is separated out from the water separator' or 'no change of reaction temperature', and the like in the reaction process, so that whether the incompletely reacted raw materials exist or not can be judged.
Preferably, the nonpolar oil and the activator with the mass of 60-80% of the mass of the nonpolar oil are added into the reactor in the step (2); filtering with 0.15-0.45 mm thick oil filter paper if precipitate is generated after mixing, wherein the filtering process can not be stirred or heated, the filtrate can be used after standing for 10 minutes without precipitating, if precipitate is generated again, repeating the above filtering operation. Adding supplementary liquid, controlling the mass fraction of the supplementary liquid to be not less than 64% of the total mass of the mixed solution, and stirring to form stable milky white or slightly yellow milky white viscous paste to obtain the collecting agent.
In the third aspect, the invention provides the use of the collector for mineral flotation, the using amount of the nonpolar oil in the collector is 0.05-1 wt% of the amount of the mineral, in the use, the nonpolar oil is used for changing the physical properties of the surface of the mineral, and the main functions of the activating agent and the replenishing liquid are to bridge different mineral particle interfaces and mineral particle and air bubble interfaces, so that the nonpolar oil with the same effect is directionally replaced.
Preferably, a foaming agent is also added in the flotation process, and the foaming agent is selected from the group consisting of pinitol oil, butyl ether oil, sec-octanol, GF oil, MIBC, isooctanol, ketones of C4-C5, and microorganism synthetic active molecules; the amount of the foaming agent used is 0.05-0.5 per mill of the amount of the mineral substance.
Compared with the prior art, the invention has the following beneficial effects:
1. the collector comprises 1-35% of nonpolar oil, 1-35% of an activating agent and 64-95% of a replenishing liquid (based on mass percentage), wherein the nonpolar oil plays a role equivalent to a common collector (nonpolar oil) in the traditional flotation process, namely the physical property of the surface of a mineral is changed; the main functions of the activating agent and the supplementary liquid are to bridge different mineral particle interfaces and mineral particle and bubble interfaces, so that the traditional collecting agent (nonpolar oil) with the same function is directionally replaced, the effect of greatly reducing the consumption of the nonpolar oil is integrally realized, and the cost of the activating agent and the supplementary liquid is far lower than that of the nonpolar oil, so that the cost of the collecting agent can be greatly reduced.
2. The flotation collector prepared by the invention has the characteristics of strong selectivity and high yield, and can realize the same mineral foam flotation effect with extremely low medicament cost compared with the traditional collector (nonpolar oil). The dosage of the nonpolar oil can be greatly reduced on the premise of achieving the same effect, so that the application cost is reduced.
3. In a preferred embodiment of the present invention, the alcohol before the esterification reaction between the fatty acid and the alcohol is a polyol, and the reactant obtained after the esterification reaction contains at least one monoester compound of a fatty acid polyol, and the monoester compound of a fatty acid polyol obtained by the esterification reaction is used as an activator, and the mineral froth flotation effect is better than that obtained by using the compound of a diester, a triester, or the like of a fatty acid polyol obtained by the esterification reaction as an activator.
4. In a more preferred embodiment of the present invention, the alcohol before the esterification reaction of the fatty acid and the alcohol is a mixture of a polyol and a monohydric alcohol, and the reactant obtained after the esterification reaction contains at least one monoester compound of a fatty acid polyol and an incompletely reacted monohydric alcohol, and the mineral froth flotation effect is better than when the monoester compound of a fatty acid polyol obtained by the esterification reaction is used as an activator and the monoester compound of a fatty acid polyol obtained by the esterification reaction and the incompletely reacted monohydric alcohol are used as activators.
5. The collecting agent is low in cost, and raw materials are easy to obtain; the collecting agent has excellent performance, the raw materials used in the formula are non-toxic and harmless, the environment is not damaged, the collecting agent can be applied in a large scale in the actual industrial process, and the low-cost collecting agent has extremely high economic and commercial values.
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Detailed Description
For the convenience of understanding, the technical scheme of the invention is further illustrated by the specific embodiments. Other persons will appreciate that the illustrated embodiments are only to assist understanding of the invention and therefore should not be seen as a specific limitation of the invention.
The following examples prepare collectors by the following method:
(1) carrying out esterification reaction on fatty acid and alcohol to obtain a reaction product, filtering the reaction product and collecting supernatant to obtain the activating agent;
(2) and (2) adding the nonpolar oil and the activating agent obtained in the step (1) into a reactor, stirring and mixing, adding a supplementary liquid, and stirring and mixing to obtain the collecting agent.
In the step (1), the reaction temperature is 60-120 ℃, further, the reaction temperature is 60-96 ℃, the reaction product after the esterification reaction of the fatty acid and the alcohol is controlled by regulating and controlling the reaction temperature, and the reaction product mainly comprises a monoester compound of the fatty acid polyhydric alcohol and the monohydric alcohol which is not completely reacted. The purpose of controlling the temperature is to control the reaction product, and besides, the method commonly used in the prior art for controlling the reaction product of the esterification reaction of fatty acid and alcohol, or the method for judging the type of the reaction product can be used in the patent. In addition, whether the esterification reaction is terminated or not can be judged according to common means such as 'no water is separated out from the water separator' or 'the reaction temperature is not changed' in the reaction process, so that whether the raw materials for which the reaction is not played exist or not can be judged.
Adding nonpolar oil and an activating agent with the mass of 60-80% of the mass of the nonpolar oil into a reactor in the step (2); filtering with 0.15-0.45 mm thick oil filter paper if precipitate is generated after mixing, wherein the filtering process can not be stirred or heated, the filtrate can be used after standing for 10 minutes without precipitating, if precipitate is generated again, repeating the above filtering operation. Adding supplementary liquid, controlling the mass fraction of the supplementary liquid to be not less than 64% of the total mass of the mixed solution, and stirring to form stable milky white or slightly yellow milky white viscous paste to obtain the collecting agent.
Specific ratios of the collecting agents, types of the foaming agents, weight ratios of nonpolar oil to mineral in the collecting agents, and performance indexes such as yield of clean coal, ash content of clean coal, recovery rate of combustible bodies and the like after flotation of coal particles by using the collecting agents in examples 1 to 14 are shown in the following table.
Examples 1 to 14
Comparing example 1 with example 4, it can be known that, in order to achieve similar flotation effect, the use amount of the nonpolar oil (diesel oil and paraffin oil mixture) in the collecting agent can be effectively reduced by more than 60%, so that the application cost of the agent can be greatly reduced. Similarly, comparative examples 5 and 8, examples 9 and 11, and comparative examples 12 and 14 can be concluded similarly.
It can be seen from a comparison of examples 2 and 4 that higher yields of clean coal and combustible recovery can be achieved with the collectors of the invention using the same amount of non-polar oil. Similarly, comparative examples 6 and 8, examples 10 and 11, and comparative examples 13 and 14 can be concluded similarly.
Comparing example 1 and example 3, it is known that the mineral froth flotation effect is better, the yield of clean coal and the recovery rate of combustible are improved, and the ash content of clean coal is reduced, compared with the case of using a mixture of ethylene glycol dihexadecanoate and ethylene glycol as an activator and a mixture of ethylene glycol monopalmitate and ethylene glycol as an activator.
Comparing example 5 with example 7, it is known that the mineral froth flotation effect is better, the yield of clean coal and the recovery rate of combustible material can be improved, and the ash content of clean coal can be reduced, compared with the case of using polyethylene glycol monooleate as an activator and using a mixture of polyethylene glycol monooleate and allyl alcohol which is not completely reacted as an activator.
Claims (1)
1. Use of a collector for mineral flotation, the collector comprising, on a mass percent basis:
1-35% of nonpolar oil, 1-35% of an activating agent and 64-95% of a supplementary liquid;
the activating agent is a reactant obtained after esterification reaction of fatty acid and alcohol, and the supplementary liquid is a salt solution;
the nonpolar oil comprises one or more of kerosene, diesel oil, light cycle oil, paraffin oil, clarified oil, coal-based mineral oil and coal tar;
the salt solution is an inorganic salt solution, an organic salt solution or a salt solution prepared by mixing inorganic salt and organic salt; the inorganic salt is selected from one or more of sodium chloride, potassium chloride, sodium sulfate, potassium sulfate, sodium nitrate or potassium nitrate; the organic salt is selected from one or more of sodium alkyl phenol ether sulfosuccinate, triethanolamine oleate soap, potassium phenol ether phosphate, potassium isotridecanol ether phosphate or potassium lauryl phosphate;
the fatty acid comprises one or more of stearic acid, palmitic acid, oleic acid and dodecanoic acid, the alcohol comprises a polyol, and the polyol is selected from one or more of dihydric alcohol, trihydric alcohol, dihydric alcohol polymer or trihydric alcohol polymer;
the alcohols further include monohydric alcohols, the monohydric alcohols being allyl alcohol;
the method is characterized in that a reactant obtained by esterification reaction of fatty acid and alcohol at least contains a monoester compound of fatty acid polyol and allyl alcohol; the usage amount of the nonpolar oil in the collecting agent is 0.05-1 wt% of the amount of the mineral substance.
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| CN202010294597 | 2020-04-15 | ||
| CN2020102945970 | 2020-04-15 |
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| CN111530637B true CN111530637B (en) | 2022-03-15 |
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| CN115155822A (en) * | 2022-06-24 | 2022-10-11 | 湖南三林新材料有限公司 | Efficient foaming agent for copper ore flotation and preparation method thereof |
| CN115178119B (en) * | 2022-07-21 | 2023-11-03 | 中国矿业大学 | Flotation reagent emulsifying equipment and method for coal |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CA1211870A (en) * | 1982-10-14 | 1986-09-23 | Robert O. Keys | Promotors for froth flotation of coal |
| CN85106071A (en) * | 1985-08-14 | 1986-01-10 | 轻工业部日用化学工业科学研究所 | Oil-in-water emulsion used in flotation of coal slurry |
| CN1129611A (en) * | 1995-02-23 | 1996-08-28 | 北京市华能新资源开发高技术公司 | Powdered coal flotation agent and preparation thereof |
| CN105880031B (en) * | 2016-04-06 | 2018-08-07 | 武汉理工大学 | A kind of method of hydrophilic coal slime flotation |
| CN109759239B (en) * | 2019-03-28 | 2020-01-17 | 中国矿业大学 | Flotation process for treating coal slime by using salt-containing wastewater |
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