CN113769896B - Collecting agent and preparation method and application thereof - Google Patents
Collecting agent and preparation method and application thereof Download PDFInfo
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- CN113769896B CN113769896B CN202110893056.4A CN202110893056A CN113769896B CN 113769896 B CN113769896 B CN 113769896B CN 202110893056 A CN202110893056 A CN 202110893056A CN 113769896 B CN113769896 B CN 113769896B
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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
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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
- B03D1/01—Organic compounds containing nitrogen
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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
- B03D1/014—Organic compounds containing phosphorus
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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
- B03D1/02—Froth-flotation processes
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Abstract
The invention particularly relates to a collector, a preparation method and application thereof, belonging to the technical field of bauxite flotation desilication, wherein the collector has the structural formula:
wherein R contains at least one-COOH functional group and/or at least one-H 2 PO 3 A functional group; the function group-C (O) NHOH in the collector has stronger action with Al points on the surface of minerals, the formed chelate is more stable, the collecting performance is improved, the introduction of-COOH increases the dissolving performance of the collector, and the consumption of the collector is reduced, and the content of-H is reduced 2 PO 3 The introduction of the (C) increases the low-temperature performance of the collector, and has excellent low-temperature adaptability and selectivity compared with the traditional fatty acid collector.
Description
Technical Field
The invention belongs to the technical field of bauxite flotation desilication, and particularly relates to a collecting agent, a preparation method and application thereof.
Background
The bauxite in China is rich in resources, but most of the bauxite belongs to bauxite with low aluminum, high silicon and low aluminum-silicon ratio. Bauxite ore is mainly made of diasporite, boehmite, gibbsite and the like, impurity minerals are mainly made of aluminosilicate, and in order to improve the market competitiveness of alumina enterprises in China, high-quality concentrate products are provided for alumina production through economic and effective ore dressing and desilication, and a great amount of experimental researches are carried out on bauxite ore dressing and desilication collectors at present.
The patent documents disclosed at present are: the Chinese patent application CN109465113B is a bauxite flotation collector and a bauxite flotation method, and the bauxite flotation collector is characterized in that: the main collector comprises sodium laurate, sodium C16 fatty acid, sodium C18 fatty acid, oleic acid, linoleic acid, linolenic acid and sodium C22 fatty acid. The use temperature of the bauxite collector is 55-60 ℃, and the reagent flotation temperature is far higher than that of the common bauxite collector, so that the reagent flotation collector is not suitable for a low-temperature operation environment; the Chinese patent application CN108435436A is a bauxite direct flotation collector, which comprises the following components of alkyl alcohol, fatty acid, saturated fatty acid and sulfonate, wherein the components comprise, by mass, 20% -30% of alkyl alcohol, 40% -60% of fatty acid, 10% -30% of saturated fatty acid and 30% -40% of sulfonate, and the collector is fully dissolved and dispersed with a sodium carbonate solution with the total mass of 40% -60% and then uniformly stirred, and is left stand for 2 hours to obtain the bauxite direct flotation collector. The positive flotation collector is mainly composed of fat compounds, and has poor dispersion and solubility and poor selectivity; the Chinese patent application CN103480497B is a combined collector for the forward flotation of diasporic bauxite and a use method thereof, wherein the main components of the combined collector are saponification products of vegetable oleic acid, naphthenic acid and dodecyl ether phosphate, the ratio is 1:1:0.5, and the dosage is 800-1200g/t. The medicament combination has large medicament use amount and high production cost.
The papers currently published are: wei Xiao et al (bauxite with certain low aluminium-silicon ratio)Flotation test study, mining study and development, 2014,34 (2): 50-53), describes a diasporic-kaolinite bauxite in Guizhou, the test uses sodium oleate and C5-9 hydroxamic acid as collecting agents, adopts a test flow of one coarse, three fine and three sweeps, the collecting agent dosage is 1500g/t, and the concentrate Al 2 O 3 Grade 63.43%, al 2 O 3 Recovery rate is 71.02% and Al-Si ratio is 5.72. The flotation test flow is longer, the consumption of the collector is large, the selectivity is poor, and the concentrate yield is low; peng Zhibing et Al (research on bauxite positive flotation test, nonferrous metal beneficiation part, 2013, 1:40-44), describe a certain diasporite-kaolinite type bauxite with high iron and low aluminum-silicon ratio, and use a combined reagent of sodium oleate and heptyl hydroxamic acid as a collector, and use sodium carbonate and sodium hexametaphosphate to disperse ore pulp and inhibit kaolinite, wherein the dosage of the collector is 1200g/t, and finally concentrate Al is obtained 2 O 3 Grade 57.85%, al 2 O 3 An index of recovery 74.36% and Al-Si ratio 8.09; zhang Guofan (influence of temperature on adsorption of sodium oleate on the surface of a hydraulic diasporite mineral, chinese non-ferrous metals journal, 2004 (6): 1042-1046), sodium oleate does not show obvious chemical adsorption on the surface of a hydraulic diasporite at normal or relatively low temperature, and obvious chemical adsorption only occurs under certain medicament concentration and certain temperature conditions. Therefore, the low-temperature performance of the oleic acid collector is weaker.
The existing bauxite collecting agent mainly takes fatty acid, alkyl acid and sodium salt thereof as a flotation collecting agent, and has the problems of poor water solubility, low-temperature solubility, poor selectivity, large dosage of medicament, intolerance to low temperature and the like due to the existence of alkyl chains.
Disclosure of Invention
The invention aims to provide a collecting agent, a preparation method and application thereof, and aims to solve the problems of poor reagent selectivity, large reagent dosage, intolerance to low temperature and the like in the current beneficiation process.
The embodiment of the invention provides a collector, which has the structural formula:
wherein R contains at least one-COOH functional group and/or at least one-H 2 PO 3 Functional groups.
Optionally, the collector has a structural formula in which the number of carbons of R is 4 to 16.
Optionally, the collector comprises at least one of 3, 3-bis-hydroxycarbamoyl heptanoic acid, 3-bis-hydroxycarbamoyl-1-dodecane phosphate, 4-bis-hydroxycarbamoyl heptadecanoic acid, 4-bis-hydroxycarbamoyl decanoic acid, 4-bis-hydroxycarbamoyl pentadecanoic acid, 3-bis-hydroxycarbamoyl-1-hexadecyl phosphate, and 4, 4-bis-hydroxycarbamoyl undecanoic acid.
Based on the same inventive concept, the embodiment of the invention also provides a preparation method of the collecting agent, which comprises the following steps:
obtaining the bishydroxamic acid;
at least one-COOH functional group and/or at least one-H 2 PO 3 The functional group is introduced into the bishydroxamic acid to obtain a collector, and the structural formula of the collector is as follows:
wherein R contains at least one-COOH functional group and/or at least one-H 2 PO 3 Functional groups.
Optionally, the collector has a structural formula in which the number of carbons of R is 4 to 16.
Optionally, the method for obtaining the bishydroxamic acid specifically comprises the following steps:
introducing a-C (O) NHOH functional group into a hydroxamic acid compound to obtain the bishydroxamic acid.
Based on the same inventive concept, the embodiments of the present invention also provide an application of a collector, including application of the collector to flotation desilication of bauxite; the structural formula of the collector is as follows:
wherein R contains at least one-COOH functional group and/or at least one-H 2 PO 3 Functional groups.
Optionally, the collector has a structural formula in which the number of carbons of R is 4 to 16.
Optionally, the flotation desilication method comprises the following steps:
and (3) regulating the pH value of the ore pulp of the bauxite, and then adding the collector to perform flotation desilication to obtain flotation concentrate and flotation tailings.
Optionally, the weight content of the particles with the granularity smaller than 0.074mm in the ore pulp of the bauxite powder is more than or equal to 60.0%.
Optionally, the pH value of the ore pulp subjected to flotation desilication is 4-8; the temperature of the floatation desilication is 3-60 ℃; the addition amount of the collector is 300.0g/t pulp-800.0 g/t pulp.
One or more technical solutions in the embodiments of the present invention at least have the following technical effects or advantages:
the structural formula of the collector provided by the embodiment of the invention is as follows:
wherein R contains at least one-COOH functional group and/or at least one-H 2 PO 3 A functional group; the function group-C (O) NHOH in the collector has stronger action with Al points on the surface of minerals, the formed chelate is more stable, the collecting performance is improved, the introduction of-COOH increases the dissolving performance of the collector, and the consumption of the collector is reduced, and the content of-H is reduced 2 PO 3 The introduction of the (C) increases the low-temperature performance of the collector, and has excellent low-temperature adaptability and selectivity compared with the traditional fatty acid collector.
The foregoing description is only an overview of the present invention, and is intended to be implemented in accordance with the teachings of the present invention in order that the same may be more clearly understood and to make the same and other objects, features and advantages of the present invention more readily apparent.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required for the description of the embodiments will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a flow chart of a positive flotation desilication test of 'one roughing, one refining and one scavenging';
FIG. 2 is a flow chart of a positive flotation desilication test of once roughing, twice refining and once scavenging;
fig. 3 is a flowchart of a preparation method provided in an embodiment of the present invention.
Detailed Description
The advantages and various effects of the present invention will be more clearly apparent from the following detailed description and examples. It will be understood by those skilled in the art that these specific embodiments and examples are intended to illustrate the invention, not to limit the invention.
Throughout the specification, unless specifically indicated otherwise, the terms used herein should be understood as meaning as commonly used in the art. Accordingly, unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. In case of conflict, the present specification will control.
Unless otherwise specifically indicated, the various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or may be prepared by existing methods.
The technical scheme of the embodiment of the application aims to solve the technical problems, and the overall thought is as follows:
aims at solving the problems of poor reagent selectivity, large reagent dosage, intolerance to low temperature and the like in the existing mineral separation processMineral analysis is carried out on bauxite to examine mineral components, charge properties of minerals in ore pulp and cleavage plane characteristics of minerals, and-C (O) NHOH is introduced into hydroxamic acid compounds to obtain bishydroxamic acid, and then-COOH and-H are introduced on the basis 2 PO 3 And (3) obtaining the novel C6-C18 carbonyl (phosphate group) bishydroxamic acid collector by the equal functional groups.
According to an exemplary embodiment of the present invention, there is provided a collector having the structural formula:
wherein R contains at least one-COOH functional group and/or at least one-H 2 PO 3 Functional groups.
The function group-C (O) NHOH in the collector has stronger action with Al points on the surface of minerals, the formed chelate is more stable, the collecting performance is improved, the introduction of-COOH increases the dissolving performance of the collector, and the consumption of the collector is reduced, and the content of-H is reduced 2 PO 3 The introduction of (c) increases the low temperature performance of the collector.
As an alternative embodiment, the collector has a formula wherein R has a carbon number of 4 to 16.
Specifically, the collector may be selected from at least one of 3, 3-dihydroxycarbamoyl heptanoic acid, 3-dihydroxycarbamoyl-1-dodecane phosphate, 4-dihydroxycarbamoyl heptadecanoic acid, 4-dihydroxycarbamoyl decanoic acid, 4-dihydroxycarbamoyl pentadecanoic acid, 3-dihydroxycarbamoyl-1-phosphoric hexadecane, and 4, 4-dihydroxycarbamoyl undecanoic acid, wherein the structural formula of the 3, 3-dihydroxycarbamoyl heptanoic acid is as follows:
3. the structural formula of the 3-bis-hydroxylamine formyl-1-dodecane phosphate is as follows:
4. the structural formula of the 4-bis-hydroxylamine formyl heptadecanoic acid is as follows:
it should be noted that the above list of collectors is only for illustrating that the present application can be implemented, and is not limited to the present invention, and in other embodiments, those skilled in the art may choose to satisfy the structural formula:
wherein R contains at least one-COOH functional group and/or at least one-H 2 PO 3 A collector of functional groups.
According to another exemplary embodiment of the present invention, there is provided a method for preparing a collector, the method including:
s1, introducing a-C (O) NHOH functional group into a hydroxamic acid compound to obtain bishydroxamic acid;
s2, at least one-COOH functional group and/or at least one-H 2 PO 3 The functional group is introduced into the bishydroxamic acid to obtain a collector, and the structural formula of the collector is as follows:
wherein R contains at least one-COOH functional group and/or at least one-H 2 PO 3 Functional groups.
For example, the collector 3, 3-bis-hydroxylamine formyl heptanoic acid can be prepared by: 1. reacting dimethyl 2-pentanyl malonate in hydroxylamine hydrochloride and sodium hydroxide methanol solution to obtain 2-pentanyl bishydroxamic acid; 2. the obtained 2-pentane-based bishydroxamic acid reacts with sodium ethoxide and sodium chloroacetate, and is treated by dilute hydrochloric acid to obtain 3, 3-bishydroxylamine formyl heptanoic acid.
Common oleic acid and other carboxylic acid collectors similar to oleic acid in nature are mainly obtained by extraction and separation from plant seeds, and can be used by combining collectors with different chain lengths and different saturation degrees in the use process.
According to another exemplary embodiment of the present invention, there is provided the use of a collector comprising applying the collector to the flotation desilication of bauxite; the structural formula of the collector is as follows:
wherein R contains at least one-COOH functional group and/or at least one-H 2 PO 3 Functional groups.
Specifically, the method for flotation desilication comprises the following steps: and (3) regulating the pH value of the ore pulp of the bauxite, and then adding the collector to perform flotation desilication to obtain flotation concentrate and flotation tailings.
As an alternative implementation mode, the weight content of the particles with the granularity less than 0.074mm in the ore pulp of the bauxite powder is more than or equal to 60.0 percent. The separation of the monomers of each mineral can be realized through grinding, and the separation is easy during floatation; however, most gangue minerals such as kaolinite, illite and pyrophyllite are closely embedded with the target mineral diasporite, and when the grinding fineness is required to reach a certain degree, the method can realize the dissociation of the monomer. As an alternative embodiment, the slurry of the flotation desilication has a pH of 4 to 8; the temperature of the floatation desilication is 3-60 ℃; the addition amount of the collector is 300.0g/t pulp-800.0 g/t pulp.
The pH regulator has the main functions of improving the surface electrical property of ore and enhancing the combination of the reagent and the target mineral by adding the regulator, thereby promoting the adsorption between the flotation reagent and the target and realizing the effective separation of the target mineral and the non-target mineral.
The collectors of the present application, and methods of making and using the same, will be described in detail below with reference to examples, comparative examples, and experimental data.
Example 1
The aluminum-silicon ratio is 3.81 and Al 2 O 3 Grinding raw bauxite ore with content of 46.56% to fineness of 62.13% (-0.074 mm) by adopting the process flow shown in figure 1, and adding Na at flotation temperature of 6deg.C 2 CO 3 Regulating the pH value of ore pulp to 7.5, adding a novel bauxite flotation desilication collector 3, 3-dihydroxycarbamoyl heptanoic acid with the dosage of 750g/t, and carrying out a positive flotation desilication test research to obtain flotation concentrate with the aluminum-silicon ratio of 7.98, the enrichment ratio of 2.09, the alumina recovery rate of 80.61 percent and the tailing aluminum-silicon ratio of 1.29.
Example 2
The aluminum-silicon ratio is 3.27, al 2 O 3 Certain bauxite raw ore with 51.06 percent of content is ground by adopting the process flow shown in figure 1 until the grinding fineness is 98.92 percent (minus 0.074 mm), and Na is added under the condition that the floatation temperature is 20 DEG C 2 CO 3 And NaOH (1:1) to adjust the pH value of ore pulp to 8, adding a novel bauxite flotation desilication collector 3, 3-bis (hydroxylamine formyl-1-dodecane) as a collector, carrying out positive flotation desilication test research with the dosage of 550g/t, wherein the obtained flotation concentrate has an aluminum-silicon ratio of 6.61, an enrichment ratio of 2.02, an alumina recovery rate of 80.13% and a tailing aluminum-silicon ratio of 1.27.
Example 3
The aluminum-silicon ratio is 3.95 and Al 2 O 3 Raw bauxite ore with the content of 45.29 percent is ground to the fineness of 78.63 percent (minus 0.074 mm) by adopting the process flow shown in figure 1, the pH value of ore pulp is regulated to 4 by adding HCl under the condition that the floatation temperature is 15 ℃, a novel bauxite floatation desilication collector 4 and 4-dihydroxycarbamoyl heptadecanoic acid are added as collectors, the dosage is 350g/t, the research of a positive floatation desilication test is carried out, the aluminum-silicon ratio of the obtained floatation concentrate is 7.98, the enrichment ratio is 2.06, the alumina recovery rate is 81.26 percent, and the aluminum-silicon ratio of tailings is 1.26.
Example 4
The aluminum-silicon ratio is 4.24 and Al 2 O 3 Bauxite raw ore with the content of 50.27 percent is ground into ore with the fineness of 81.24 percent (-0.074 mm) by adopting the process flow shown in figure 1, and the ore is regulated under the condition that the floatation temperature is 40 DEG CAnd (3) adding a novel bauxite flotation desilication collector with the pH value of the slurry of 7, using 4, 4-bis-hydroxylamine formyldecanoic acid and 4, 4-bis-hydroxylamine formylpentadecanoic acid (1:1) as collectors, using 600g/t, and performing a positive flotation desilication test research, wherein the aluminum-silicon ratio of the obtained flotation concentrate is 8.95, the enrichment ratio is 2.11, the alumina recovery rate is 80.96%, and the tailing aluminum-silicon ratio is 1.28.
Example 5
The aluminum-silicon ratio is 4.28, al 2 O 3 Bauxite raw ore with the content of 57.45 percent is ground to the fineness of 85.12 percent (-0.074 mm) by adopting the process flow shown in figure 2, HCL is added to adjust the pH value of ore pulp to 5.5 under the condition that the floatation temperature is 15 ℃, a novel bauxite floatation desilication collector is added, 3-bis-hydroxycarbamoyl-1-phosphate hexadecane and 4, 4-bis-hydroxycarbamoyl undecanoic acid (2:1) are used as collectors, the dosage is 500g/t, the research of a positive floatation desilication test is carried out, the aluminum-silicon ratio of the obtained floatation concentrate is 9.13, the enrichment ratio is 2.13, the alumina recovery rate is 82.36 percent, and the aluminum-silicon ratio of tailings is 1.23.
Comparative example 1
The aluminum-silicon ratio is 3.95 and Al 2 O 3 The raw bauxite ore with the content of 45.29 percent is subjected to flotation desilication by adopting a bauxite flotation collector and a flotation method provided by a bauxite flotation method as disclosed in Chinese patent application No. 109465113B.
Comparative example 2
The aluminum-silicon ratio is 3.95 and Al 2 O 3 The bauxite crude ore with the content of 45.29 percent is subjected to flotation desilication by adopting a combined collector for the positive flotation of diasporic bauxite, as shown in Chinese patent application No. CN103480497B, and a collector and a flotation method provided by the use method of the combined collector.
Test results:
the test results of examples 1-5 and comparative examples 1-2 are shown in the following table.
The collector and the flotation method provided by the embodiment of the invention can realize the indexes that the concentrate enrichment ratio is more than or equal to 2.0, the alumina recovery rate is more than or equal to 80% and the tailing aluminum-silicon ratio is less than or equal to 1.3, and can be obtained by comparing the data of comparative examples 1 and 2 with the data of example 3.
One or more technical solutions in the embodiments of the present invention at least have the following technical effects or advantages:
(1) The collector provided by the embodiment of the invention obtains the bishydroxamic acid by introducing-C (O) NHOH into the hydroxamic acid compound, and then introduces-COOH and-H on the basis 2 PO 3 Obtaining a novel C6-C18 carbonyl (phosphate group) bishydroxamic acid collector by the equal functional groups;
(2) The functional group-C (O) NHOH in the collector provided by the embodiment of the invention has stronger action with the Al point on the surface of the mineral, the formed chelate is more stable, the collecting performance is improved, the introduction of-COOH increases the dissolving performance of the collector, the consumption of the collector is reduced, and the content of-H is reduced 2 PO 3 The introduction of (2) increases the low temperature performance of the collector;
(3) Compared with the traditional fatty acid collector, the collector provided by the embodiment of the invention has excellent low-temperature adaptability and selectivity;
(4) The collector provided by the embodiment of the invention is matched with the optimized flotation process flow, so that the index that the concentrate enrichment ratio is more than or equal to 2.0, the alumina recovery rate is more than or equal to 80% and the tailing aluminum-silicon ratio is less than or equal to 1.3 is realized.
Finally, it is also noted that the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
While preferred embodiments of the present invention have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. It is therefore intended that the following claims be interpreted as including the preferred embodiments and all such alterations and modifications as fall within the scope of the invention.
It will be apparent to those skilled in the art that various modifications and variations can be made to the present invention without departing from the spirit or scope of the invention. Thus, it is intended that the present invention also include such modifications and alterations insofar as they come within the scope of the appended claims or the equivalents thereof.
Claims (3)
1. A method for flotation and desilication of bauxite is characterized in that,
regulating the pH value of the ore pulp of the bauxite, and then adding a collector to carry out flotation desilication to obtain flotation concentrate and flotation tailings; the weight content of particles with the granularity smaller than 0.074mm in the ore pulp of the bauxite powder is more than or equal to 60.0%, and the pH value of the ore pulp subjected to flotation desilication is 4-8; the temperature of the floatation desilication is 3-60 ℃; the addition amount of the collector is 300.0g/t pulp-800.0 g/t pulp;
the structural formula of the collector is as follows:
wherein R contains at least one-H 2 PO 3 Functional groups.
2. The flotation desilication process of claim 1 wherein the collector has a formula wherein the number of carbons of R is 4 to 16.
3. The flotation desilication process of claim 1, wherein the collector comprises at least one of 3, 3-bis-hydroxycarbamoyl-1-phosphate dodecane, 3-bis-hydroxycarbamoyl-1-phosphate hexadecane.
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