CN113351376B - Gasified slag flotation collector and preparation method thereof - Google Patents

Gasified slag flotation collector and preparation method thereof Download PDF

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CN113351376B
CN113351376B CN202110589370.3A CN202110589370A CN113351376B CN 113351376 B CN113351376 B CN 113351376B CN 202110589370 A CN202110589370 A CN 202110589370A CN 113351376 B CN113351376 B CN 113351376B
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flotation
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gasified slag
flotation collector
sodium dodecyl
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张海军
王海楠
李文峰
田全志
闫小康
梁艳男
杨文清
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China University of Mining and Technology CUMT
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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
    • B03D1/018Mixtures of inorganic and organic compounds

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Abstract

The invention relates to the technical field of gasified slag flotation, in particular to a gasified slag flotation collecting agent and a preparation method thereof. The collector comprises 1-3 parts of sodium dodecyl sulfate, 1-5 parts of deionized water, 15-60 parts of nonpolar hydrocarbon oil, 1/10-1/2 parts of hydrophobic particles and 1-3 parts of an emulsifier, wherein the hydrophobic particles are graphite particles with the diameter of 1-2 mu m, and all the components are calculated by weight. According to the gasification slag collecting agent prepared by the invention, the lauryl sodium sulfate and the nonpolar hydrocarbon oil are mixed and compounded, so that the adsorption effect of the agent on the surface of the carbon residue of the gasification slag can be improved, and meanwhile, the hydrophobic particles are added to enable the agent to enter pores on the surface of the gasification slag to be filled in the flotation process, so that the agent is prevented from entering the pores, the utilization rate of the agent is improved, the flotation cost is reduced, and the flotation efficiency is improved.

Description

Gasified slag flotation collector and preparation method thereof
Technical Field
The invention relates to the technical field of gasified slag flotation, in particular to a gasified slag flotation collecting agent and a preparation method thereof.
Background
In the field of clean coal technology, coal gasification technology plays an important role. However, a large amount of ash is generated in the coal gasification process, the amount of the gasification ash in China per year reaches thousands of tons, a large part of the gasification ash is accumulated in an ash storage field, a large land area is occupied, and the gasification ash contains a plurality of metal elements with complex components, so that the environment is greatly polluted.
Because a large amount of mineral melt exists in the gasified slag, the carbon and ash are wrapped and included seriously, the embedded granularity is fine, and the flotation is a main method for realizing the separation of the carbon and the ash. In the process of forming the gasified slag, the coal is reacted in a high-temperature gasification furnace, the physicochemical properties of the surfaces of unburned carbon particles in the gasified slag are greatly changed due to incomplete combustion, pores are developed, the structure of organic aliphatic hydrocarbon is lost, the surface oxidation degree is high, the number of oxygen-containing functional groups is increased, the hydrophilicity is obviously increased, and the floatability of the carbon residue particles in the gasified slag is reduced compared with that of common coal, and the flotation efficiency is low. The conventional diesel oil or kerosene is used as a collecting agent, so that the collecting agent and a foaming agent enter gaps of gasified slag in the flotation process, the utilization rate of the agent is low, and the flotation effect is influenced; on the other hand, these nonpolar hydrocarbon oils have poor adsorption effects on the surface of carbon residue particles containing hydrophilic functional groups, resulting in poor surface modification of the carbon residue particles. Therefore, there is a need to develop a collector suitable for flotation of the gasified slag.
Disclosure of Invention
In order to solve the problems, the invention provides a flotation collector for gasified slag.
The invention adopts the following technical scheme:
the flotation collector for gasified slag comprises 1-3 parts of sodium dodecyl sulfate, 1-5 parts of deionized water, 15-60 parts of nonpolar hydrocarbon oil, 1/10-1/2 parts of hydrophobic particles and 1-3 parts of an emulsifier, wherein the hydrophobic particles are graphite particles with the diameter of 1-2 mu m, and all the components are calculated by weight.
Preferably, the collector comprises 1 part of sodium lauryl sulfate, 1 part of deionized water, 18 parts of non-polar hydrocarbon oil, 1/6 part of hydrophobic particles and 121/120 part of emulsifier.
Preferably, the emulsifier is polyethylene glycol.
Preferably, the nonpolar hydrocarbon oil is any one or more of diesel oil, kerosene or gasoline.
The second purpose of the invention is to provide a preparation method of the gasified slag flotation collector, which comprises the following steps:
s1, adding deionized water into sodium dodecyl sulfate, heating to 50 ℃ by using a magnetic stirrer, and stirring for 10min to prepare a sodium dodecyl sulfate solution;
s2, adding nonpolar hydrocarbon oil into the sodium dodecyl sulfate solution, continuously heating to 70 ℃ by using a magnetic stirrer, and stirring for 10min to obtain a mixed solution;
s3, adding hydrophobic particles into the mixed solution of the S2, and oscillating and mixing for 3min by using an ultrasonic oscillator to obtain a graphite mixed solution;
and S4, adding an emulsifier into the graphite mixed solution obtained in the S3, heating to 70 ℃ by using a magnetic stirrer, and stirring for 1min to obtain the gasified slag flotation collector.
Preferably, in S1, the addition ratio of the sodium dodecyl sulfate to the deionized water is 1:1 by mass.
Preferably, in S2, the addition ratio of the sodium dodecyl sulfate solution to the nonpolar hydrocarbon oil is 1:9 by mass.
Preferably, in S3, the addition ratio of the mixed solution to the hydrophobic particles is 120.
Preferably, in S4, the addition ratio of the graphite mixed solution to the emulsifier is 20.
Preferably, the emulsifier is polyethylene glycol.
Preferably, the nonpolar hydrocarbon oil is any one or more of diesel oil, kerosene or gasoline.
The invention has the beneficial effects that:
1) In the invention, sodium dodecyl sulfate and nonpolar hydrocarbon oil are mixed and compounded, during the flotation process, sodium dodecyl sulfate molecules are adsorbed on carboxyl, hydroxyl and other oxygen-containing functional groups on the surface of the gasification slag carbon residue in an inclined or lying manner and are mainly adsorbed in the form of Van der Waals force and electrostatic force, the sodium dodecyl sulfate and the nonpolar hydrocarbon oil form good synergistic adsorption on the surface of the gasification slag carbon residue, and compared with the nonpolar hydrocarbon oil, the adsorption effect of mixing the sodium dodecyl sulfate and the nonpolar hydrocarbon oil on the surface of the carbon residue is stronger.
2) According to the invention, hydrophobic particles are added into the sodium dodecyl sulfate and nonpolar hydrocarbon oil compound solution, and the mixed solution is fully emulsified through oscillation, so that graphite particles are uniformly dispersed and suspended in the prepared collecting agent. Hydrophobic particles are contacted with gasified slag in the flotation process and enter pores on the surface of the gasified slag for filling, so that a medicament for flotation can be prevented from entering the pores, and the utilization rate of the medicament is improved. The graphite particles of 1 to 2 μm are used mainly because the voids of the slag after grinding are 2 to 3 μm, and if the particle size of the graphite particles is too large, the graphite particles are difficult to enter the voids, and if the particle size is too small, the graphite particles are easily discharged from the voids. Only when the graphite particles are 1-2 μm, the graphite particles are easily embedded into the gaps of the gasified slag, which is beneficial to the maximum effect.
3) The reason why the ultrafine graphite particles are used is that the flotation concentrate of the gasified slag is generally residual carbon, the purity of the flotation concentrate cannot be influenced by adding the graphite particles with the main component of carbon, and the graphite particles are low in price and are suitable for production and use; on the other hand, in the tailings subjected to the flotation of the gasified slag in the prior art, the ash content generally reaches more than 90%, the added graphite particles are mostly filled in gaps of the gasified slag, and the graphite particles which are not filled can be floated to form concentrate, so that the concentrate can not enter the tailings due to the fact that the concentrate cannot be floated, the ash content of the tailings is reduced, and the tailings are polluted.
Drawings
Fig. 1 is a schematic flow diagram of the preparation of a gasified residue flotation collector according to the present invention.
Detailed Description
The technical solution of the present invention is described in more detail with reference to the following embodiments.
Example 1
The preparation method of the gasified slag flotation collector comprises the following steps:
s1, adding deionized water into sodium dodecyl sulfate according to a mass ratio of 1:1, heating to 50 ℃ by using a magnetic stirrer, and stirring for 10min to prepare a sodium dodecyl sulfate solution;
s2, adding nonpolar hydrocarbon oil into a sodium dodecyl sulfate solution according to a mass ratio of 1:9, heating to 70 ℃ by using a magnetic stirrer, and stirring for 10min to obtain a mixed solution;
s3, adding superfine graphite particles into the S2 mixed solution according to a mass ratio of 120; the diameter of the ultrafine graphite particles is 1-2 mu m;
and S4, adding an emulsifier into the graphite mixed solution obtained in the S3 according to the mass ratio of 20.
The emulsifier is polyethylene glycol, and the nonpolar hydrocarbon oil is any one of diesel oil, kerosene or gasoline.
Example 2
Gasified slag flotation test by utilizing gasified slag flotation collecting agent provided by the invention
1. The collecting agent is prepared by the following process:
s1, adding 1g of sodium dodecyl sulfate into 1g of deionized water, and heating the sodium dodecyl sulfate and the deionized water to 50 ℃ by using a magnetic stirrer and stirring for 10min at the same time to obtain a sodium dodecyl sulfate solution;
s2, adding 18g of diesel oil into the product of the S1, heating to 70 ℃ by using a magnetic stirrer, and stirring for 10min to obtain a mixed solution;
s3, adding 0.17g of ultrafine graphite into the product of the S2, and oscillating and mixing for 3min by using an ultrasonic oscillator to obtain a graphite mixed solution;
and S4, adding 1g of polyethylene glycol into the product of the S3, heating to 70 ℃ by using a magnetic stirrer, and stirring for 1min to obtain the gasified slag flotation collector.
2. Flotation of test group
Grinding the gasified slag for 15min before flotation, then adding 50g of the ground gasified slag and 1L of water into a laboratory 1L of mechanical stirring type flotation machine, stirring for 2min, adding 0.15g of the prepared collecting agent, and stirring for 3min again. Adding 0.2g foaming agent (MIBC) into mechanical stirring type flotation machine, stirring for 1min, and performing aeration flotation with aeration amount of 0.1m 3 And h, the flotation time is 9min, and concentrate and tailings are collected.
3. Comparative flotation
The same gasified slag and flotation machine are used in the comparative example, diesel oil is directly used as a collecting agent to carry out a gasified slag flotation test, and concentrate and tailings are collected.
4. Analysis of results
The flotation results for the test groups and the comparative example are shown in table 1 below:
TABLE 1 comparative flotation test results
Figure SMS_1
Data comparison shows that compared with diesel oil, the flotation yield of the concentrate can be improved by 13.92%, and the using effect is good.
Example 3
Using the same materials and procedure as in example 2, the diesel in the collector was adjusted to kerosene and the results of the flotation comparative tests were measured as shown in table 2 below:
TABLE 2 flotation comparative test results
Figure SMS_2
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Data comparison shows that compared with the method of directly using kerosene to prepare the collecting agent, the method has the advantages that the flotation yield of the concentrate is greatly improved, the proportion is improved by 11.40%, and the effect of the collecting agent prepared by the method is better.
Example 4
Using the same materials and methods as in example 2, only the added ultra fine graphite particles were removed from the collectors prepared in the test group, and the results of the flotation comparative tests were measured as shown in table 3 below:
TABLE 3 comparative flotation test results
Figure SMS_3
Data comparison shows that after the ultrafine graphite particles are removed, although the collecting agent prepared by the method can still improve the flotation yield of the ore to a certain extent, compared with the collecting agent added with the ultrafine graphite particles, the improvement proportion is only 5.09%, and is far lower than 13.92% after the ultrafine graphite particles are added, and the addition of the hydrophobic particles has a good effect on the collecting agent in the enhanced gasification slag flotation.
The above embodiments are only used to illustrate the technical solutions of the present invention, and do not limit the present invention; although the present invention has been described in detail with reference to the foregoing embodiments, it should be understood by those skilled in the art that any changes, substitutions, and alterations can be made herein without departing from the spirit and scope of the invention.

Claims (10)

1. The gasified slag flotation collector is characterized by comprising 1-3 parts of sodium dodecyl sulfate, 1-5 parts of deionized water, 15-60 parts of nonpolar hydrocarbon oil, 1/10-1/2 parts of hydrophobic particles and 1-3 parts of an emulsifier, wherein the hydrophobic particles are graphite particles with the diameter of 1-2 mu m, and all the components are calculated by weight.
2. The collector of claim 1, wherein the collector comprises 1 part of sodium dodecyl sulfate, 1 part of deionized water, 18 parts of non-polar hydrocarbon oil, 1/6 part of hydrophobic particles and 121/120 part of emulsifier.
3. The flotation collector for the gasification slag according to claim 1 or 2, wherein the emulsifier is polyethylene glycol.
4. A flotation collector for gasified slag according to claim 1 or claim 2, wherein the non-polar hydrocarbon oil is any one or more of diesel oil, kerosene or gasoline.
5. A method of preparing a gasification slag flotation collector according to claim 1, comprising the steps of:
s1, adding deionized water into sodium dodecyl sulfate, heating to 50 ℃ by using a magnetic stirrer, and stirring for 10min to prepare a sodium dodecyl sulfate solution;
s2, adding nonpolar hydrocarbon oil into the sodium dodecyl sulfate solution, continuously heating to 70 ℃ by using a magnetic stirrer, and stirring for 10min to obtain a mixed solution;
s3, adding hydrophobic particles into the mixed solution in the S2, and oscillating and mixing for 3min by using an ultrasonic oscillator to obtain a graphite mixed solution;
and S4, adding an emulsifier into the graphite mixed solution obtained in the S3, heating to 70 ℃ by using a magnetic stirrer, and stirring for 1min to obtain the gasified slag flotation collector.
6. The method of preparing a gasified slag flotation collector of claim 5, wherein the addition ratio of sodium lauryl sulfate to deionized water in S1 is 1:1 by mass.
7. The method of preparing a gasified slag flotation collector of claim 6, wherein the mass ratio of sodium dodecyl sulfate solution to non-polar hydrocarbon oil added in S2 is 1:9.
8. The method of preparing a gasified slag flotation collector of claim 6, wherein the addition ratio of the mixed solution to the hydrophobic particles in S3 is 120.
9. The method for preparing the gasified slag flotation collector, according to claim 6, wherein the ratio of the graphite mixed solution to the emulsifier added in S4 is 20.
10. The method for preparing the flotation collector for the gasified slag according to any one of claims 5-9, wherein the emulsifier is polyethylene glycol, and the nonpolar hydrocarbon oil is any one or more of diesel oil, kerosene or gasoline.
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