CN114887773B - Flotation collector and preparation method and application thereof - Google Patents

Flotation collector and preparation method and application thereof Download PDF

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Publication number
CN114887773B
CN114887773B CN202210671191.9A CN202210671191A CN114887773B CN 114887773 B CN114887773 B CN 114887773B CN 202210671191 A CN202210671191 A CN 202210671191A CN 114887773 B CN114887773 B CN 114887773B
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parts
flotation collector
flotation
cocoamine
collector
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CN114887773A (en
Inventor
凌石生
尚衍波
王中明
肖巧斌
刘方
刘书杰
谭欣
赵晨
贺壮志
吴世鹏
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Beikuang Chemical Technology Cangzhou Co ltd
BGRIMM Technology Group Co Ltd
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Beikuang Chemical Technology Cangzhou Co ltd
BGRIMM Technology Group Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03DFLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D1/00Flotation
    • B03D1/001Flotation agents
    • B03D1/004Organic compounds
    • B03D1/01Organic compounds containing nitrogen
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03DFLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D1/00Flotation
    • B03D1/02Froth-flotation processes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03DFLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D2201/00Specified effects produced by the flotation agents
    • B03D2201/02Collectors
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03DFLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D2203/00Specified materials treated by the flotation agents; specified applications
    • B03D2203/02Ores
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00Technologies for solid waste management
    • Y02W30/50Reuse, recycling or recovery technologies
    • Y02W30/52Mechanical processing of waste for the recovery of materials, e.g. crushing, shredding, separation or disassembly

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Abstract

The invention provides a flotation collector, a preparation method and application thereof, wherein the flotation collector comprises cocoamine, glacial acetic acid, octanol and m-diazacyclopentene; the method has the characteristics of easy water dissolution, good dispersibility, good foam friability and the like, can be directly added in flotation operation during use, does not need to add hydrochloric acid for configuration, and has good operation environment; the flotation collector fully plays the synergistic effect of cocoamine, glacial acetic acid, octyl alcohol and meta-diazacyclopentene, so that the collecting capability of the amine collector is maintained, the solubility and the dispersibility of the flotation collector are improved, the dispersion of the flotation collector in ore pulp and the adsorption of the flotation collector on the lepidolite surface are facilitated, and a better sorting effect can be achieved by using a smaller amount of the flotation collector.

Description

Flotation collector and preparation method and application thereof
Technical Field
The invention relates to the technical field of mineral processing, in particular to a flotation collector and a preparation method and application thereof.
Background
Lepidolite is one of the most important resources for extracting lithium elements. The lepidolite ore dressing mainly adopts a floatation method, and the most widely applied and most stable index is an amine cationic collector floatation method.
CN111229470a discloses a mineral separation activator for lepidolite flotation process, which comprises the following raw materials in parts by weight: 60% of mineral dressing activating agent, 30% of collecting agent and 10% of foaming agent. The mineral separation activating agent for the lepidolite flotation process is prepared by adding dodecylamine or cocoamine into a heated reaction kettle, adding alcohol after dodecylamine or cocoamine is heated and dissolved, stirring uniformly, adding hydrochloric acid for reaction, and finally adding hot water for dilution for standby after the reaction is completed.
CN114247559a is a tailing-free beneficiation method for lithium ore recovery; the method comprises the following steps: sequentially carrying out crushing grinding and pulp mixing treatment on the raw ore of the lepidolite, and then carrying out lepidolite pre-enrichment by adopting a preferential flotation process and using dodecyl amine as a collector to obtain lepidolite rough concentrate; blank concentration is carried out on the lepidolite rough concentrate, so that flotation concentrate is lepidolite concentrate, and flotation tailings are feldspar and quartz separated ore feeding; grinding tailings subjected to preferential flotation, pulping, and performing flotation separation to obtain spodumene rough concentrate and feldspar quartz separated ore feeding; performing low-intensity magnetic separation on the spodumene rough concentrate to remove iron, and performing high-intensity magnetic separation and spiral chute reselection to obtain spodumene concentrate and niobium tantalum iron minerals; and separating feldspar and quartz by adopting floatation to obtain feldspar concentrate and quartz concentrate. The lepidolite is subjected to preferential flotation, spodumene rough concentrate is subjected to iron removal, niobium-tantalum mineral is selectively enriched, quartz feldspar is separated, and the comprehensive utilization rate of the lepidolite is greatly improved.
CN110369146B discloses a spodumene ore floatation collector, a preparation method thereof and a spodumene ore floatation method. The collector comprises the following components: 10-30 parts of dodecyl dimethyl tertiary amine, 150-450 parts of vegetable oleic acid and 25-75 parts of sodium hydroxide, and the preparation method comprises the following steps: and uniformly mixing the vegetable oleic acid and the dodecyl dimethyl tertiary amine to obtain a mixed material, mixing the mixed material with sodium hydroxide, heating and stirring until the reaction is complete, and obtaining the spodumene ore flotation collector.
CN106040437B discloses a flotation collector for lithium-containing minerals and a preparation method thereof, which solves the problems of large consumption, high cost, large influence by low temperature, more foam, poor selectivity and Li in concentrate of the existing flotation collector 2 The problems of non-ideal O content and recovery rate index are solved, wherein the lithium-containing mineral flotation collector comprises the following components: 1 part by weight of naphthenic acid, 2-4 parts by weight of oxidized paraffin soap, 4-8 parts by weight of oleic acid, 0.1-0.3 part by weight of sodium isooctyl arsenate and 0.1-0.3 part by weight of octadecylamine.
However, the amine cationic collector has obvious defects that firstly, a large amount of hydrochloric acid is required to be added in the process of configuration and use of amines, the volatility and corrosiveness are strong, the harm to human bodies is large, and potential safety hazards exist; secondly, the amine collector has higher solidifying point, and can be added by adopting fire baking and melting when the air temperature is low, and even if a large amount of hydrochloric acid is added for configuration, the problems of poor solubility and selectivity, large dosage of the agent, low flotation recovery rate and the like still exist.
Therefore, there is a need for a high-efficiency collector with good operating environment, which improves recovery rate and solves the problems of large addition of hydrochloric acid, poor solubility, poor selectivity, and the like in the configuration of amine collectors.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention aims to provide a flotation collector, a preparation method and application thereof, wherein the flotation collector comprises cocoamine, glacial acetic acid, octanol and m-diazacyclopentene; the method has the characteristics of easy water dissolution, good dispersibility, good foam friability and the like, can be directly added in flotation operation during use, does not need to add hydrochloric acid for configuration, and has good operation environment; the flotation collector fully plays the synergistic effect of cocoamine, glacial acetic acid, octyl alcohol and meta-diazacyclopentene, so that the collecting capability of the amine-transfer collector is maintained, the solubility and the dispersibility of the flotation collector are improved, the flotation collector is favorably dispersed in ore pulp and adsorbed on the surface of lepidolite, and a better sorting effect can be achieved by using a smaller amount of the flotation collector.
To achieve the purpose, the invention adopts the following technical scheme:
it is an object of the present invention to provide a flotation collector comprising cocoamine, glacial acetic acid, octanol and meta-diazacyclopentene.
It is worth to say that the flotation collector fully exerts the synergistic effect of cocoamine, glacial acetic acid, octanol and metadiazepine, not only maintains the collecting capacity of amine-transfer collectors, but also improves the solubility and dispersibility of the flotation collector, and is beneficial to dispersing the flotation collector in ore pulp and adsorbing on the surface of lepidolite; the method has the characteristics of easy water dissolution, good dispersibility, good foam friability and the like, can be directly added in flotation operation during use, does not need to add hydrochloric acid for configuration, and has good operation environment; the better sorting effect can be achieved with a small dosage (200-500 g/t).
As a preferred technical scheme of the invention, the flotation collector comprises the following components in parts by weight: 20-40 parts of cocoamine, for example, 20 parts, 21 parts, 22 parts, 23 parts, 24 parts, 25 parts, 26 parts, 27 parts, 28 parts, 29 parts, 30 parts, 31 parts, 32 parts, 33 parts, 34 parts, 35 parts, 36 parts, 37 parts, 38 parts, 39 parts, 40 parts and the like; 30-60 parts of glacial acetic acid, for example, 30 parts, 33 parts, 35 parts, 38 parts, 40 parts, 42 parts, 45 parts, 48 parts, 50 parts, 52 parts, 56 parts, 59 parts, 60 parts and the like; 3-15 parts of octanol, for example, 3 parts, 4 parts, 5 parts, 6 parts, 7 parts, 8 parts, 9 parts, 10 parts, 11 parts, 12 parts, 13 parts, 14 parts, 15 parts, etc.; 3 to 15 parts of m-diazacyclopentene may be, for example, 3 parts, 4 parts, 5 parts, 6 parts, 7 parts, 8 parts, 9 parts, 10 parts, 11 parts, 12 parts, 13 parts, 14 parts, 15 parts, etc., but are not limited to the recited values, and other non-recited values within this range are equally applicable.
It is worth noting that 20-40 parts of cocoamine in the flotation collector, if less than 20 parts, the amine content in the collector decreases, resulting in a decrease in the collecting capacity; if the content exceeds 40 parts, the content of amine is high, the solubility and dispersibility of the collector are poor, and the flotation index is lowered; 30-60 parts of glacial acetic acid in the flotation collector, if the amount of glacial acetic acid in the flotation collector is less than 30 parts, the solubility of amine in the collector is reduced, so that flotation is not facilitated; if the content exceeds 60 parts, the glacial acetic acid is excessive and is easy to volatilize; 3-15 parts of octanol in the flotation collector, if the octanol is less than 3 parts, a foam layer is thin during flotation, so that the flotation recovery rate is affected; if the concentration of the concentrate exceeds 15 parts, the thickness of the flotation froth layer influences the concentrate grade; 3-15 parts of diazacyclopentene in the middle of the flotation collector, if less than 3 parts, the synergistic effect of the diazacyclopentene and cocoamine is weakened, and the flotation recovery rate is influenced; if the content exceeds 15 parts, the content of other components in the collector is reduced, which is unfavorable for the synergistic effect between the components of the collector.
As a preferred technical scheme of the invention, the flotation collector comprises the following components in parts by weight: 25 to 35 parts of cocoamine can be, for example, 25 parts, 25.5 parts, 26 parts, 26.5 parts, 27 parts, 27.5 parts, 28 parts, 28.5 parts, 29 parts, 29.5 parts, 30 parts, 30.5 parts, 31 parts, 31.5 parts, 32 parts, 32.5 parts, 33 parts, 33.5 parts, 34 parts, 34.5 parts, 35 parts, etc.; 40 to 50 parts of glacial acetic acid may be, for example, 40 parts, 40.5 parts, 41 parts, 41.5 parts, 42 parts, 42.5 parts, 43 parts, 43.5 parts, 44 parts, 44.5 parts, 45 parts, 45.5 parts, 46 parts, 46.5 parts, 47 parts, 47.5 parts, 48 parts, 48.5 parts, 49 parts, 49.5 parts, 50 parts, etc.; octanol 5-10 parts, for example, 5 parts, 5.5 parts, 6 parts, 6.5 parts, 7 parts, 7.5 parts, 8 parts, 8.5 parts, 9 parts, 9.5 parts, 10 parts, etc.; 5 to 10 parts of m-diazacyclopentene may be, for example, 5 parts, 5.5 parts, 6 parts, 6.5 parts, 7 parts, 7.5 parts, 8 parts, 8.5 parts, 9 parts, 9.5 parts, 10 parts, etc., but are not limited to the recited values, and other non-recited values within this range are equally applicable.
The adoption of proper glacial acetic acid can ensure the complete dissolution of cocoamine, enhance the solubility and the dispersibility of cocoamine in ore pulp, be more beneficial to the selective adsorption of cocoamine on the surface of lepidolite, and improve the collection capacity and the selectivity; the meta-diazacyclopentene has the advantages of good collection performance, good water solubility and dispersibility, contribution to selective adsorption on the surface of lepidolite, and octanol can promote the dissolution and dispersion of cocoanut amine, is also a good foaming agent, can adjust the foam state, and is more beneficial to floatation of lepidolite.
As a preferred embodiment of the present invention, the octanol comprises n-octanol and/or isooctanol.
The second object of the invention is to provide a method for preparing the flotation collector, which comprises the following steps:
(1) Heating cocoamine until the cocoamine is melted, and performing first mixing with glacial acetic acid to obtain a mixed solution A;
(2) Carrying out second mixing on octanol and m-diazacyclopentene to obtain a mixed solution B;
(3) And (3) adding the mixed solution B in the step (2) into the mixed solution A in the step (1) to perform third mixing to obtain the flotation collector.
In a preferred embodiment of the present invention, the temperature of the first mixture in the step (1) is 25 to 30. DegreeC, for example, 25. DegreeC, 26. DegreeC, 27. DegreeC, 28. DegreeC, 29. DegreeC, 30. DegreeC, etc., but the present invention is not limited to the above-mentioned values, and other values not shown in the above-mentioned range are equally applicable.
Preferably, the time of the first mixing in the step (1) is 0.5-1h, for example, 0.5h, 0.6h, 0.7h, 0.8h, 0.9h, 1h, etc., but not limited to the recited values, and other non-recited values in the range are equally applicable.
In a preferred embodiment of the present invention, the temperature of the second mixture in the step (2) is 25 to 30. DegreeC, for example, 25. DegreeC, 26. DegreeC, 27. DegreeC, 28. DegreeC, 29. DegreeC, 30. DegreeC, etc., but the present invention is not limited to the values recited, and other values not recited in the range are equally applicable.
Preferably, the second mixing time in step (2) is 0.5-1h, for example, 0.5h, 0.6h, 0.7h, 0.8h, 0.9h, 1h, etc., but not limited to the recited values, and other non-recited values within this range are equally applicable.
In a preferred embodiment of the present invention, the temperature of the third mixture in the step (3) is 25 to 30. DegreeC, for example, 25. DegreeC, 26. DegreeC, 27. DegreeC, 28. DegreeC, 29. DegreeC, 30. DegreeC, etc., but the present invention is not limited to the above-mentioned values, and other values not shown in the above-mentioned range are equally applicable.
Preferably, the third mixing time in step (3) is 0.5-1h, for example, 0.5h, 0.6h, 0.7h, 0.8h, 0.9h, 1h, etc., but not limited to the recited values, and other non-recited values within this range are equally applicable.
As a preferable technical scheme of the invention, the preparation method comprises the following steps:
(1) Heating 20-40 parts of cocoamine until the cocoamine is melted, and carrying out first mixing with 30-60 parts of glacial acetic acid at 25-30 ℃ for 0.5-1h to obtain a mixed solution A;
(2) Mixing 3-15 parts of octanol and 3-15 parts of m-diazacyclopentene for 0.5-1h at 25-30 ℃ to obtain a mixed solution B;
(3) And (3) adding the mixed solution B obtained in the step (2) into the mixed solution A obtained in the step (1), and carrying out third mixing for 0.5-1h at 25-30 ℃ to obtain the flotation collector.
It is a further object of the present invention to provide the use of a flotation collector as described in one of the objects for flotation of lepidolite from lepidolite ores.
The numerical ranges recited herein include not only the above-listed point values, but also any point values between the above-listed numerical ranges that are not listed, and are limited in space and for the sake of brevity, the present invention is not intended to be exhaustive of the specific point values that the stated ranges include.
Compared with the prior art, the invention has the beneficial effects that:
(1) The flotation collector has the characteristics of easy water dissolution, good dispersibility, good foam friability and the like, can be directly added in flotation operation when in use, does not need to be added with hydrochloric acid for configuration, and has good operation environment;
(2) The flotation collector fully plays the synergistic effect of cocoamine, glacial acetic acid, octyl alcohol and metadiazene, maintains the collecting capability of the amine collector, improves the solubility and the dispersibility of the flotation collector, is beneficial to dispersing the flotation collector in ore pulp and adsorbing the flotation collector on the surface of lepidolite, and ensures that Li in the lepidolite concentrate 2 High O content, li 2 The recovery rate of O is high;
(3) The flotation collector disclosed by the invention can obviously reduce the dosage of the flotation collector, is low in medicament cost, and can achieve a better sorting effect with a smaller dosage.
Detailed Description
The technical scheme of the invention is further described by the following specific embodiments. It will be apparent to those skilled in the art that the examples are merely to aid in understanding the invention and are not to be construed as a specific limitation thereof.
Example 1
The embodiment provides a flotation collector and a preparation method thereof, wherein the flotation collector comprises the following components in parts by weight: 30 parts of cocoamine, 45 parts of glacial acetic acid, 8 parts of n-octanol and 8 parts of m-diazacyclopentene;
the preparation method comprises the following steps:
(1) Heating cocoamine until the cocoamine is melted, and carrying out first mixing with glacial acetic acid at 25 ℃ for 1h to obtain a mixed solution A;
(2) Carrying out second mixing on n-octanol and m-diazacyclopentene for 1h at 25 ℃ to obtain a mixed solution B;
(3) And (3) adding the mixed solution B in the step (2) into the mixed solution A in the step (1), and carrying out third mixing for 1h at 25 ℃ to obtain the flotation collector.
Example 2
The embodiment provides a flotation collector and a preparation method thereof, wherein the flotation collector comprises the following components in parts by weight: 35 parts of cocoamine, 50 parts of glacial acetic acid, 5 parts of n-octanol and 5 parts of m-diazacyclopentene;
the preparation method comprises the following steps:
(1) Heating cocoamine until the cocoamine is melted, and carrying out first mixing with glacial acetic acid at 30 ℃ for 1h to obtain a mixed solution A;
(2) Carrying out second mixing on isooctanol and m-diazacyclopentene for 1h at the temperature of 30 ℃ to obtain a mixed solution B;
(3) And (3) adding the mixed solution B in the step (2) into the mixed solution A in the step (1), and carrying out third mixing for 1h at 30 ℃ to obtain the flotation collector.
Example 3
The embodiment provides a flotation collector and a preparation method thereof, wherein the flotation collector comprises the following components in parts by weight: 25 parts of cocoamine, 40 parts of glacial acetic acid, 10 parts of n-octanol and 10 parts of m-diazacyclopentene;
the preparation method comprises the following steps:
(1) Heating cocoamine until the cocoamine is melted, and carrying out first mixing with glacial acetic acid at 28 ℃ for 0.5h to obtain a mixed solution A;
(2) Carrying out second mixing on n-octanol and m-diazacyclopentene for 0.5h at the temperature of 28 ℃ to obtain a mixed solution B;
(3) And (3) adding the mixed solution B in the step (2) into the mixed solution A in the step (1), and carrying out third mixing for 0.5h at 28 ℃ to obtain the flotation collector.
Example 4
The embodiment provides a flotation collector and a preparation method thereof, and the flotation collector comprises the following components in parts by weight with reference to the flotation collector in embodiment 1: 20 parts of cocoamine, 30 parts of glacial acetic acid, 3 parts of n-octanol and 15 parts of m-diazacyclopentene; the preparation method refers to the preparation method of example 1.
Example 5
The embodiment provides a flotation collector and a preparation method thereof, and the flotation collector comprises the following components in parts by weight with reference to the flotation collector in embodiment 1: 40 parts of cocoamine, 60 parts of glacial acetic acid, 15 parts of n-octanol and 3 parts of m-diazacyclopentene; the preparation method refers to the preparation method of example 1.
Example 6
This example provides a flotation collector and a method for preparing the same, and the flotation collector described with reference to example 1 differs only in that: keeping the total amount of coco amine, glacial acetic acid, n-octanol and m-diazacyclopentene unchanged, wherein the coco amine is 15 parts, and other components are adjusted according to the original proportion; the preparation method refers to the preparation method of example 1.
Example 7
This example provides a flotation collector and a method for preparing the same, and the flotation collector described with reference to example 1 differs only in that: keeping the total amount of coco amine, glacial acetic acid, n-octanol and m-diazacyclopentene unchanged, wherein the coco amine is 45 parts, and other components are adjusted according to the original proportion; the preparation method refers to the preparation method of example 1.
Example 8
This example provides a flotation collector and a method for preparing the same, and the flotation collector described with reference to example 1 differs only in that: keeping the total amount of cocoamine, glacial acetic acid, n-octanol and m-diazacyclopentene unchanged, wherein the total amount of the glacial acetic acid is 25 parts, and other components are adjusted according to the original proportion; the preparation method refers to the preparation method of example 1.
Example 9
This example provides a flotation collector and a method for preparing the same, and the flotation collector described with reference to example 1 differs only in that: keeping the total amount of cocoamine, glacial acetic acid, n-octanol and m-diazacyclopentene unchanged, wherein the glacial acetic acid is 65 parts, and other components are adjusted according to the original proportion; the preparation method refers to the preparation method of example 1.
Example 10
This example provides a flotation collector and a method for preparing the same, and the flotation collector described with reference to example 1 differs only in that: keeping the total amount of cocoamine, glacial acetic acid, n-octanol and m-diazacyclopentene unchanged, wherein the n-octanol is 1 part, and other components are adjusted according to the original proportion; the preparation method refers to the preparation method of example 1.
Example 11
This example provides a flotation collector and a method for preparing the same, and the flotation collector described with reference to example 1 differs only in that: keeping the total amount of cocoamine, glacial acetic acid, n-octanol and m-diazacyclopentene unchanged, wherein the n-octanol is 20 parts, and other components are adjusted according to the original proportion; the preparation method refers to the preparation method of example 1.
Example 12
This example provides a flotation collector and a method for preparing the same, and the flotation collector described with reference to example 1 differs only in that: keeping the total amount of cocoamine, glacial acetic acid, n-octanol and m-diazacyclopentene unchanged, wherein 1 part of m-diazacyclopentene is used, and other components are adjusted according to the original proportion; the preparation method refers to the preparation method of example 1.
Example 13
This example provides a flotation collector and a method for preparing the same, and the flotation collector described with reference to example 1 differs only in that: keeping the total amount of cocoamine, glacial acetic acid, n-octanol and m-diazacyclopentene unchanged, wherein the amount of the m-diazacyclopentene is 20 parts, and other components are adjusted according to the original proportion; the preparation method refers to the preparation method of example 1.
Comparative example 1
This comparative example provides a flotation collector and a method of making the same, with reference to the flotation collector described in example 1, differing only in: the coco amine is replaced by glacial acetic acid, n-octanol and m-diazacyclopentene in an equivalent way according to the original proportion; the preparation method refers to the preparation method of example 1.
Comparative example 2
This comparative example provides a flotation collector and a method of making the same, with reference to the flotation collector described in example 1, differing only in: the glacial acetic acid is replaced by cocoamine, n-octanol and m-diazacyclopentene in an equivalent way according to the original proportion; the preparation method refers to the preparation method of example 1.
Comparative example 3
This comparative example provides a flotation collector and a method of making the same, with reference to the flotation collector described in example 1, differing only in: n-octanol is replaced by cocoamine, glacial acetic acid and m-diazacyclopentene in an equivalent way according to the original proportion; the preparation method refers to the preparation method of example 1.
Comparative example 4
This comparative example provides a flotation collector and a method of making the same, with reference to the flotation collector described in example 1, differing only in: the meta-diazacyclopentene is replaced by cocoamine, glacial acetic acid and n-octanol in equal quantity according to the original proportion; the preparation method refers to the preparation method of example 1.
Comparative example 5
This comparative example provides a flotation collector and a method of making the same, with reference to the flotation collector described in example 1, differing only in: the glacial acetic acid is replaced by hydrochloric acid in equal quantity; the preparation method refers to the preparation method of example 1.
Comparative example 6
This comparative example provides a flotation collector and a method of making the same, with reference to the flotation collector described in example 1, differing only in: equivalent replacement of cocoamine with dodecylamine; the preparation method refers to the preparation method of example 1.
Comparative example 7
This comparative example provides a flotation collector and a method of making the same, with reference to the flotation collector described in example 1, differing only in: octanol equivalent replacement with 2# oil; the preparation method refers to the preparation method of example 1.
The # 2 oil used in this comparative example was purchased from north mineralization discipline, inc.
The flotation performance of the flotation collectors obtained in the examples and the comparative examples is tested, and the specific steps include the following steps:
1) Lepidolite ore feeding (Li 2 O content 1.02%) and water to prepare pulp with solid content of 30-35%, and adding hydrochloric acid to adjust pulp pH=3; adding a flotation collector to perform flotation to obtain concentrate, and controlling the addition amount of the flotation collector to be 300g/t based on lepidolite ore feeding;
2) For Li in concentrate 2 O content and Li 2 The O recovery rate is detected and calculated by the following method:
li in lepidolite concentrate 2 O content: detecting by adopting a method in a line mark YS/T509.1-2008;
Li 2 o recovery = (Li in lepidolite concentrate 2 O content x lepidolite concentrate yield)/(Li in lepidolite feed 2 O content x lepidolite ore feeding yield) x 100%;
the results are shown in Table 1.
TABLE 1
Project Li in concentrate 2 O content/% Li 2 O recovery/%
Example 1 4.31 94.19
Example 2 4.19 94.51
Example 3 4.24 94.02
Example 4 4.06 91.12
Example 5 3.89 93.55
Example 6 3.91 88.05
Example 7 3.96 90.61
Example 8 3.88 88.55
Example 9 3.99 88.90
Example 10 4.16 87.01
Example 11 3.73 91.23
Example 12 4.07 88.31
Example 13 3.98 89.01
Comparative example 1 3.23 70.14
Comparative example 2 3.28 67.36
Comparative example 3 3.68 87.22
Comparative example 4 3.32 86.86
Comparative example 5 3.33 86.53
Comparative example 6 4.09 90.84
Comparative example 7 3.83 90.69
From table 1, the following points can be found:
(1) From examples 1 to 5, it can be seen that the flotation collector of the invention fully exerts the synergistic effect of cocoamine, glacial acetic acid, octyl alcohol and meta-diaza-pentene, and is beneficial to dispersing the flotation collector in ore pulp and adsorbing on the lepidolite surface, and Li in concentrate 2 High O content, li 2 The recovery rate of O is high;
(2) Comparing example 1 with examples 6-13, it can be seen that 15 parts cocoamine in example 6, below the preferred 20-40 parts of the invention, li in concentrate 2 Reduced O content, li 2 The recovery rate of O is reduced; 45 parts of cocoamine in example 7, 20-40 parts beyond the preferred one of the invention, li in concentrate 2 Reduced O content, li 2 The recovery rate of O is reduced; in example 8, the glacial acetic acid was 25 parts, less than the preferred 30-60 parts of the invention, the solubility of the collector was reduced, and the Li in the concentrate 2 Reduced O content, li 2 The recovery rate of O is reduced; in example 9, the glacial acetic acid was 65 parts, and beyond the preferred 30-60 parts of the invention, the other components were reduced, resulting in Li in the concentrate 2 Reduced O content, li 2 The recovery rate of O is reduced; in example 10, n-octanol was 1 part, less than 3-15 parts preferred in the present invention, the flotation froth layer was thin, li in concentrate 2 Reduced O content, li 2 The recovery rate of O is reduced; in example 11, n-octanol was 20 parts, 3-15 parts beyond the preferred one of the present invention, the content of other components was reduced, and foam viscosity was caused, leading to Li in concentrate 2 Reduced O content, li 2 The recovery rate of O is reduced; EXAMPLE 12 intermediate twoThe content of the nitrogen cyclopentene is 1 part, is lower than 3-15 parts which are preferable in the invention, is difficult to have synergistic effect with other components, and Li in concentrate 2 Reduced O content, li 2 The recovery rate of O is reduced; example 13 the intermediate diazacyclopentene was 20 parts, 3-15 parts beyond the preferred one of the invention, and the other components were reduced in content, resulting in Li in the concentrate 2 Reduced O content, li 2 The recovery rate of O is reduced;
(3) Comparing example 1 with comparative examples 1-4, it can be seen that the absence of cocoamine from comparative example 1 results in reduced performance of the flotation collectors and Li in the concentrate 2 Reduced O content, li 2 The recovery rate of O is reduced; the absence of glacial acetic acid in comparative example 2 resulted in reduced solubility and dispersion of the flotation collectors and Li in the concentrate 2 Reduced O content, li 2 The recovery rate of O is reduced; comparative example 3 does not include n-octanol, resulting in a thin froth layer for flotation, li in concentrate 2 Reduced O content, li 2 The recovery rate of O is reduced; the absence of meta-diazacyclopentene in comparative example 4 resulted in reduced performance of the flotation collectors and Li in the concentrate 2 Reduced O content, li 2 The recovery rate of O is reduced;
(4) Comparing example 1 with comparative examples 5-7, it can be seen that comparative example 5 replaces glacial acetic acid with hydrochloric acid in equal amount, which reacts with cocoamine to easily form complex, and the solubility and dispersion properties are reduced, resulting in reduced performance of the flotation collector, li in concentrate 2 Reduced O content, li 2 The recovery rate of O is reduced; comparative example 6 equivalent replacement of cocoamine with dodecylamine, resulting in reduced performance of the flotation collectors, li in concentrate 2 Reduced O content, li 2 The recovery rate of O is reduced; comparative example 7 equivalent replacement of octanol with 2# oil, resulting in reduced performance of the flotation collectors, li in concentrate 2 Reduced O content, li 2 The O recovery rate is reduced.
While the foregoing is directed to embodiments of the present invention, other and further details of the invention may be had by the present invention, it should be understood that the foregoing description is merely illustrative of the present invention and that no limitations are intended to the scope of the invention, except insofar as modifications, equivalents, improvements or modifications are within the spirit and principles of the invention.

Claims (13)

1. A flotation collector comprising cocoamine, glacial acetic acid, octanol and meta-diazacyclopentene;
the preparation process is as follows:
(1) Heating cocoamine until the cocoamine is melted, and performing first mixing with glacial acetic acid to obtain a mixed solution A;
(2) Carrying out second mixing on octanol and m-diazacyclopentene to obtain a mixed solution B;
(3) And (3) adding the mixed solution B in the step (2) into the mixed solution A in the step (1) to perform third mixing to obtain the flotation collector.
2. The flotation collector of claim 1, wherein the flotation collector comprises in parts by weight: 20-40 parts of cocoamine, 30-60 parts of glacial acetic acid, 3-15 parts of octanol and 3-15 parts of m-diazacyclopentene.
3. The flotation collector of claim 1, wherein the flotation collector comprises in parts by weight: 25-35 parts of cocoamine, 40-50 parts of glacial acetic acid, 5-10 parts of octanol and 5-10 parts of m-diazacyclopentene.
4. The flotation collector of claim 1 wherein the octanol comprises n-octanol and/or iso-octanol.
5. A method of preparing a flotation collector as claimed in any one of claims 1 to 4, comprising the steps of:
(1) Heating cocoamine until the cocoamine is melted, and performing first mixing with glacial acetic acid to obtain a mixed solution A;
(2) Carrying out second mixing on octanol and m-diazacyclopentene to obtain a mixed solution B;
(3) And (3) adding the mixed solution B in the step (2) into the mixed solution A in the step (1) to perform third mixing to obtain the flotation collector.
6. The method of claim 5, wherein the temperature of the first mixing in step (1) is 25-30 ℃.
7. The method of claim 5, wherein the first mixing in step (1) is for a period of 0.5 to 1 hour.
8. The method of claim 5, wherein the second mixing in step (2) is at a temperature of 25-30 ℃.
9. The method of claim 5, wherein the second mixing in step (2) is for a period of 0.5 to 1 hour.
10. The method of claim 5, wherein the temperature of the third mixing in step (3) is 25-30 ℃.
11. The method according to claim 5, wherein the third mixing in step (3) is performed for a time of 0.5 to 1 hour.
12. The preparation method according to any one of claims 5 to 11, characterized in that the preparation method comprises the steps of:
(1) Heating 20-40 parts of cocoamine until the cocoamine is melted, and carrying out first mixing with 30-60 parts of glacial acetic acid at 25-30 ℃ for 0.5-1h to obtain a mixed solution A;
(2) Mixing 3-15 parts of octanol and 3-15 parts of m-diazacyclopentene for 0.5-1h at 25-30 ℃ to obtain a mixed solution B;
(3) And (3) adding the mixed solution B obtained in the step (2) into the mixed solution A obtained in the step (1), and carrying out third mixing for 0.5-1h at 25-30 ℃ to obtain the flotation collector.
13. Use of a flotation collector according to any one of claims 1-4 for flotation of lepidolite from lepidolite ore.
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CN87104013A (en) * 1987-05-30 1988-12-14 广西冶金研究所 The combination medicament of froth flotation zircon
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CN110369146A (en) * 2019-07-19 2019-10-25 中南大学 Spodumene mine flotation collector and preparation method thereof and spodumene mine method for floating
CN114160313A (en) * 2021-12-06 2022-03-11 中南大学 Lepidolite flotation collector and application thereof

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US5106489A (en) * 1991-08-08 1992-04-21 Sierra Rutile Limited Zircon-rutile-ilmenite froth flotation process
CN102407189A (en) * 2011-10-11 2012-04-11 辽宁科技大学 Reverse flotation collector for bauxite and preparation method thereof
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