CN109894281B - Fluorite flotation collector and preparation method and application thereof - Google Patents

Fluorite flotation collector and preparation method and application thereof Download PDF

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CN109894281B
CN109894281B CN201910110371.8A CN201910110371A CN109894281B CN 109894281 B CN109894281 B CN 109894281B CN 201910110371 A CN201910110371 A CN 201910110371A CN 109894281 B CN109894281 B CN 109894281B
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flotation
collector
fluorite
flotation collector
ethanol
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CN109894281A (en
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宋英
王福良
金火荣
陈建建
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China Kings Resources Group Co ltd
Zhejiang University of Technology ZJUT
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Zhejiang University of Technology ZJUT
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Abstract

The invention belongs to the technical field of mineral flotation, and particularly relates to a fluorite flotation collector and a preparation method and application thereof. The flotation collector comprises dioctyl sodium sulfosuccinate, oleic acid and ethanol. The flotation collector has the advantages of strong collecting capacity, good water-soluble dispersibility and flotation selectivity, stable flotation index, capability of improving the recovery rate of fluorite flotation, and good repeated effect in large-scale industrial application. The concentrate obtained by flotation with the collector has high recovery rate, low content of silicon dioxide and lower grade of tailings. In addition, the flotation collector can also perform flotation on minerals at a low temperature, can effectively avoid the problems of ore pulp heating and the like, and is beneficial to energy conservation and emission reduction.

Description

Fluorite flotation collector and preparation method and application thereof
Technical Field
The invention belongs to the technical field of mineral flotation, and particularly relates to a fluorite flotation collector and a preparation method and application thereof.
Background
The floatation method is a mineral separation method which can selectively separate according to the difference of surface physicochemical properties between minerals, and is characterized by that its collector can be selectively adsorbed on the surface of useful mineral, so that it can be selectively attached to air bubbles in the ore pulp, and can be floated on the surface of the ore pulp, so that the separation of useful mineral from gangue can be implemented. Taking fluorite as an example, along with the lower and lower grade of fluorite raw ore and the mutual embedding of fluorite and gangue mineral, the fluorite mineral monomer dissociation can be achieved only through fine grinding, and the most effective method is flotation for the separation of fine ore after fine grinding.
Chinese patent document CN108160342A discloses a process for beneficiation of fluorite ore, which comprises subjecting ground ore to roughing i, scavenging, refining i, refining ii, refining iii, and refining iv to obtain rough concentrate; grading the rough concentrate obtained by the fine concentration IV to obtain a reground product; combining the reground product and the fine fraction obtained by grading together to carry out concentration V, concentration VI and concentration VII, wherein the concentrate of the concentration VII is the final concentrate; in the beneficiation process, coarse concentrate obtained by fine concentration IV is classified to obtain a fine fraction and a coarse fraction, the coarse fraction needs to be reground, the production cost is high, tailings 1 and tailings 2 are generated in the beneficiation process, and the tailings grade is high in practical industrial production application; in addition, pure sodium oleate is used as a collecting agent and is applied to the fluorite flotation process, and the flotation selectivity is basically consistent with that of oleic acid.
Disclosure of Invention
Therefore, the invention aims to overcome the defects that the recovery rate of fluorite flotation is low, the repeatability is poor, the content of silicon dioxide in the flotation concentrate is higher, the flotation collector is not suitable for the flotation of various minerals, the selectivity of a carboxylic acid collector is poor and the like in the prior art, and provides the fluorite flotation collector and the preparation method and application thereof.
Therefore, the invention provides the following technical scheme:
the invention provides a fluorite flotation collector which comprises dioctyl sodium sulfosuccinate, oleic acid and ethanol.
The sodium dioctyl sulfosuccinate salt is at least one of sodium dioctyl sulfosuccinate and disodium dioctyl sulfosuccinate.
The mass ratio of the dioctyl sodium sulfosuccinate to the oleic acid to the ethanol is (135-155): (760-790): (65-85).
The invention also provides a preparation method of the flotation collector, which comprises the steps of mixing the oleic acid, the dioctyl sodium sulfosuccinate and the ethanol in sequence, and stirring and reacting for 0.5-1h to obtain the flotation collector.
In addition, the invention provides application of the flotation collector in fluorite flotation.
The fluorite flotation step is that the raw ore is crushed, the raw ore is ground, then a regulator is added for size mixing, an inhibitor and a collecting agent are added for full stirring, and a concentrate product and tailings are obtained through one-time rough concentration, seven-time fine concentration and two-time scavenging.
In the roughing process: the using amount of the collecting agent is 800-1500g in terms of 1000kg of raw ore; the dosage of the regulator is 800-1200 g; the dosage of the inhibitor is 400-800 g;
in the selection process: the using amount of the collecting agent is 50-200g calculated by 1000kg of raw ore; the dosage of the inhibitor is 1000-1500 g;
in the scavenging process: the using amount of the collecting agent is 50-200g calculated by 1000kg of raw ore.
The inhibitor in the roughing stage is water glass, and the regulator is sodium carbonate.
The inhibitor of the concentration stage is acidified water glass; the acidified water glass comprises water glass (10 wt%) and sulfuric acid (10 wt%) in a mass ratio of (0.8-1.2): 1.
The technical scheme of the invention has the following advantages:
1. the fluorite flotation collector provided by the invention comprises dioctyl sodium sulfosuccinate, oleic acid and ethanol. The flotation collector has the advantages of strong collecting capacity, good water-soluble dispersibility and flotation selectivity, stable flotation index, capability of improving the recovery rate of ore flotation, and good repeatability in large-scale industrial application. The concentrate obtained by flotation with the collector has high recovery rate, low content of silicon dioxide and lower grade of tailings. In addition, the flotation collector can also perform flotation on minerals at a low temperature, can effectively avoid the problems of ore pulp heating and the like, and is beneficial to energy conservation and emission reduction.
2. According to the flotation collector provided by the invention, the dioctyl sodium sulfosuccinate is beneficial to separation of a target mineral and gangue, so that the target mineral is easy to float out in flotation; the ethanol can improve the stability of the flotation collector, has a defoaming effect in flotation, and improves the secondary enrichment effect of foams.
3. The collecting agent provided by the invention is applied to fluorite flotation, and specifically comprises the steps of crushing raw ore, adding a regulator for size mixing after ore grinding is performed to achieve sufficient monomer dissociation, adding an inhibitor and the collecting agent for fully stirring, and performing one-time rough concentration, seven-time fine concentration and two-time scavenging to obtain a concentrate product and tailings. The collecting agent provided by the invention is applied to the ore flotation process, the recovery rate of ore flotation can be improved, the repeatability is better in actual production, the production cost can be reduced, and the collecting agent has an actual production application value in industry. In addition, the acidified water glass helps to inhibit quartz and calcite during the beneficiation process, improving product quality and purity.
The flotation collector can also be applied to flotation of minerals such as phosphorite, ilmenite, scheelite, wolframite, rutile, cassiterite, rare earth ore, bauxite and the like.
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In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art 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 can be obtained by those skilled in the art without creative efforts.
Figure 1 is a process flow diagram of the use of collectors in fluorite flotation in example 1 of the invention.
Detailed Description
The following examples are provided to further understand the present invention, not to limit the scope of the present invention, but to provide the best mode, not to limit the content and the protection scope of the present invention, and any product similar or similar to the present invention, which is obtained by combining the present invention with other prior art features, falls within the protection scope of the present invention.
The examples do not show the specific experimental steps or conditions, and can be performed according to the conventional experimental steps described in the literature in the field. The reagents or instruments used are not indicated by manufacturers, and are all conventional reagent products which can be obtained commercially.
Example 1
The embodiment provides a flotation collector, a preparation method and application thereof, and particularly provides a flotation collector,
the flotation collector comprises dioctyl disodium sulfosuccinate with the mass of 143kg, 778kg and 79kg, oleic acid and ethanol;
the preparation method of the flotation collector comprises the following steps:
sequentially adding oleic acid, dioctyl disodium sulfosuccinate and ethanol into a reaction kettle, and fully stirring for 1h to obtain the collecting agent;
referring to fig. 1, which is a process flow chart of the application of the collector in fluorite flotation provided by the invention, the specific steps are as follows:
roughing: grinding 1000kg of raw ore to obtain a ground ore product, wherein the content of-200 meshes in the ground ore product is 58%; adding 800g of sodium carbonate as a regulator, 800g of inhibitor water glass and 1000g of collecting agent into the ground ore product for roughing to obtain rough concentrate and rough tailings;
selecting: carrying out concentration for 7 times, adding a collecting agent and acidified water glass in the concentration process, obtaining concentrate and tailings in each concentration, wherein the concentrate enters the next concentration treatment step, and the tailings enter the previous concentration step for circular treatment; wherein the collecting agent is added for 1 time, the using amount is 100g, the acidified water glass is added for 7 times, the total using amount is 1000g, the acidified water glass consists of water glass and sulfuric acid in a mass ratio of 1:1, and the concentrate obtained after the concentration VII is a concentrate product;
sweeping: scavenging for 2 times, adding 100g of collecting agent into the rough tailings, and scavenging for two times to obtain flotation tailings; and (3) adding the collecting agent at one time, scavenging to obtain scavenging concentrate and scavenging tailings, circularly treating the scavenging concentrate in the last step, and performing scavenging to obtain the scavenging tailings in the next scavenging step, wherein the scavenging tailings obtained after the scavenging II are tailings.
Example 2
The embodiment provides a flotation collector, a preparation method and application thereof, and particularly provides a flotation collector,
the flotation collector comprises 135kg, 760kg and 85kg of dioctyl disodium sulfosuccinate, oleic acid and ethanol;
the preparation method of the flotation collector comprises the following steps:
sequentially adding oleic acid, dioctyl disodium sulfosuccinate and ethanol into a reaction kettle, and fully stirring for 1h to obtain the collecting agent;
the flotation collector is applied to fluorite flotation:
roughing: grinding 1000kg of raw ore to obtain a ground ore product, wherein the content of-200 meshes in the ground ore product is 58%; adding 1200g of sodium carbonate serving as a regulator, 400g of inhibitor water glass and 800g of collecting agent into the ore grinding product for roughing to obtain rough concentrate and rough tailings;
selecting: carrying out concentration for 7 times, adding a collecting agent and acidified water glass in the concentration process, obtaining concentrate and tailings in each concentration, wherein the concentrate enters the next concentration treatment step, and the tailings enter the previous concentration step for circular treatment; wherein the collecting agent is added for 1 time, the using amount is 150g, the acidified water glass is added for 7 times, the total using amount is 1000g, the acidified water glass consists of water glass and sulfuric acid in a mass ratio of 0.8:1, and the concentrate obtained after the concentration VII is a concentrate product;
sweeping: scavenging for 2 times, adding 200g of collecting agent into the coarse tailings, and scavenging for two times to obtain flotation tailings; and (3) adding the collecting agent at one time, scavenging to obtain scavenging concentrate and scavenging tailings, circularly treating the scavenging concentrate in the last step, and performing scavenging to obtain the scavenging tailings in the next scavenging step, wherein the scavenging tailings obtained after the scavenging II are tailings.
Example 3
The embodiment provides a flotation collector, a preparation method and application thereof, and particularly provides a flotation collector,
the flotation collector comprises dioctyl sodium sulfosuccinate with the mass of 155kg, 790kg and 65kg, oleic acid and ethanol;
the preparation method of the flotation collector comprises the following steps:
sequentially adding oleic acid, dioctyl sodium sulfosuccinate and ethanol into a reaction kettle, and fully stirring for 1h to obtain the collecting agent;
the flotation collector is applied to fluorite flotation:
roughing: grinding 1000kg of raw ore to obtain a ground ore product, wherein the content of-200 meshes in the ground ore product is 58%; adding 1000g of sodium carbonate as a regulator, 600g of inhibitor water glass and 1500g of collecting agent into the ground ore product for roughing to obtain rough concentrate and rough tailings;
selecting: carrying out concentration for 7 times, adding a collecting agent and acidified water glass in the concentration process, obtaining concentrate and tailings in each concentration, wherein the concentrate enters the next concentration treatment step, and the tailings enter the previous concentration step for circular treatment; wherein the collecting agent is added for 1 time, the using amount is 50g, the acidified water glass is added for 7 times, the total using amount is 1500g, the acidified water glass consists of water glass and sulfuric acid in a mass ratio of 1.2:1, and the concentrate obtained after the concentration VII is a concentrate product;
sweeping: scavenging for 2 times, adding 50g of collecting agent into the rough tailings, and scavenging for two times to obtain flotation tailings; and (3) adding the collecting agent at one time, scavenging to obtain scavenging concentrate and scavenging tailings, circularly treating the scavenging concentrate in the last step, and performing scavenging to obtain the scavenging tailings in the next scavenging step, wherein the scavenging tailings obtained after the scavenging II are tailings.
Comparative example 1
The present comparative example provides a flotation collector and a method of preparation and use, differing from example 1 in that the collector in the rougher, cleaner and scavenger process is replaced by oleic acid.
Comparative example 2
The present comparative example provides a flotation collector and a method of preparation and use, differing from example 1 in that the collector in the rougher, cleaner and scavenger process is replaced by sodium oleate.
Test examples
The raw ores and the concentrates in the examples 1-3 and the comparative examples 1-2 are subjected to component analysis, the test method is shown in national standard GB/T5195, and the specific results are shown in Table 1;
table 1 table of analysis results of components of raw ore and concentrate in examples 1 to 3 and comparative examples 1 to 2
Figure BDA0001967874850000071
Figure BDA0001967874850000081
From table 1, it can be seen that the flotation collector provided by the invention has the advantages of strong collecting capability, good flotation selectivity, stable flotation index and capability of improving the recovery rate of fluorite flotation.
Compared with the comparative examples 1 and 2, the collector in the example 1 can lower the content of silicon dioxide in fluorite concentrate, improve the recovery rate of the concentrate by at least 2 percent and lower the grade of tailings; the dioctyl sodium sulfosuccinate can improve the hydrophobicity of the surface of calcium fluoride, so that the calcium fluoride is easy to separate from silicon dioxide, fluorite is easy to float in flotation, and the flotation recovery rate of the fluorite is improved; the ethanol can improve the stability of the collecting agent and has a defoaming effect in the flotation; the collector in example 1 helps to suppress calcium carbonate impurities during fluorite flotation, in which fluorite and calcium carbonate are easily separated.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications of the invention may be made without departing from the spirit or scope of the invention.

Claims (10)

1. A fluorite flotation collector is characterized by comprising dioctyl sodium sulfosuccinate, oleic acid and ethanol;
the preparation method of the fluorite flotation collector comprises the steps of mixing oleic acid, dioctyl sodium sulfosuccinate and ethanol in sequence, and stirring for reaction to obtain the flotation collector.
2. A fluorite flotation collector according to claim 1 including dioctyl sodium sulfosuccinate, oleic acid and ethanol;
the preparation method of the fluorite flotation collector comprises the steps of mixing oleic acid, dioctyl sodium sulfosuccinate and ethanol in sequence, and stirring for reaction for 0.5-1h to obtain the flotation collector.
3. A collector according to claim 1 or 2 wherein the dioctyl sodium sulfosuccinate is at least one of dioctyl sodium sulfosuccinate and dioctyl disodium sulfosuccinate.
4. A flotation collector according to claim 1 or 2, characterized in that the mass ratio of dioctyl sodium sulfosuccinate, oleic acid and ethanol is (135-155): (760-790): (65-85).
5. A preparation method of a flotation collector according to any one of claims 1 to 4, characterized in that oleic acid, dioctyl sodium sulfosuccinate and ethanol are mixed in sequence and stirred to react for 0.5 to 1 hour to obtain the flotation collector.
6. The use of the flotation collector according to any one of claims 1 to 4 or the flotation collector prepared by the preparation method according to claim 5 in fluorite flotation.
7. The application of the flotation collector in fluorite flotation according to claim 6, wherein the fluorite flotation step comprises the steps of crushing raw ore, grinding the raw ore, adding a regulator for size mixing, adding the inhibitor and the collector, fully stirring, and performing rough concentration once, fine concentration seven times and scavenging twice to obtain a concentrate product and tailings.
8. Use of a flotation collector according to claim 7 in fluorite flotation, wherein during the rougher flotation: the using amount of the collecting agent is 800-1500g in terms of 1000kg of raw ore; the dosage of the regulator is 800-1200 g; the dosage of the inhibitor is 400-800 g;
in the selection process: the using amount of the collecting agent is 50-200g calculated by 1000kg of raw ore; the dosage of the inhibitor is 1000-1500 g;
in the scavenging process: the using amount of the collecting agent is 50-200g calculated by 1000kg of raw ore.
9. The use of a flotation collector in fluorite flotation according to claim 8, wherein the depressor in the roughing stage is water glass and the modifier is sodium carbonate.
10. Use of a collector according to claim 8 or claim 9 in fluorite flotation, wherein the depressants in the concentration stage are acidified waterglass; the mass ratio of water glass to sulfuric acid in the acidified water glass is (0.8-1.2): 1.
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CN110560257A (en) * 2019-09-17 2019-12-13 长沙三博矿业科技有限公司 Beneficiation method for recovering associated fluorite from multi-metal tailings
CN113522517B (en) * 2021-07-15 2023-03-24 中化地质矿山总局地质研究院 Fluorite ore beneficiation method
CN114713364B (en) * 2022-03-17 2023-11-24 江西领辉科技有限公司 Method for recovering lepidolite concentrate from lepidolite beneficiation tail mud

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CN103447158A (en) * 2013-09-05 2013-12-18 鞍钢集团矿业公司 Anionic collector for normal temperature flotation of hematite and preparation method thereof
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