CN115283144A - W/O type emulsion collector for electrolytic aluminum and preparation and application thereof - Google Patents
W/O type emulsion collector for electrolytic aluminum and preparation and application thereof Download PDFInfo
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- CN115283144A CN115283144A CN202210899277.7A CN202210899277A CN115283144A CN 115283144 A CN115283144 A CN 115283144A CN 202210899277 A CN202210899277 A CN 202210899277A CN 115283144 A CN115283144 A CN 115283144A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D1/00—Flotation
- B03D1/001—Flotation agents
- B03D1/018—Mixtures of inorganic and organic compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D1/00—Flotation
- B03D1/02—Froth-flotation processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D2201/00—Specified effects produced by the flotation agents
- B03D2201/02—Collectors
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Abstract
The invention belongs to the field of resource utilization of carbon slag, and relates to a W/O type emulsion collector for electrolytic aluminum, and preparation and application thereof. The invention adopts kerosene as an external phase, KCl solution as an internal phase and alkyl glycoside (or polyisobutene ethanolamine) as an emulsifier to prepare the high internal phase W/O type emulsion collector, and the high internal phase W/O type emulsion collector is used in the flotation decarburization and quality improvement process of electrolytic aluminum carbon residue, so that the high-efficiency removal of carbon resources in the carbon residue can be realized under the condition of low oil consumption, the content of carbon impurities in a cosolvent can be reduced, and the cosolvent can be recycled in the electrolytic aluminum process, has great significance for the continuous development of the electrolytic aluminum industry and the resource utilization of the carbon residue, and has good application prospect.
Description
Technical Field
The invention belongs to the field of carbon residue resource utilization, and particularly relates to a W/O type emulsion collecting agent for electrolytic aluminum, and preparation and application thereof.
Background
China has become the first major aluminum consumer nations around the world, the electrolytic aluminum industry is rapidly developed, and the capacity is about 4000 ten thousand tons/year. In the process of electrolyzing aluminum, a cathode and an anode are both carbon-containing materials, and the carbon materials of the cathode and the anode are consumed, peeled, crushed and the like due to electrochemical reaction and electrolyte soaking, so that a large amount of carbon slag is generated. The carbon slag is mixed with the cosolvent necessary for electrolysis, resulting in reduced cosolvent efficiency and ultimately representing carbon-containing solid waste. Meanwhile, the solid wastes are mixed with salts in electrolytes and can only be dumped as dangerous wastes, so that resource waste and treatment cost are increased.
The important step for realizing the resource utilization of the carbon-containing solid waste of the electrolytic aluminum is to separate carbon from a cosolvent, and the main means for separating the carbon from the cosolvent is a flotation method. Diesel oil is used as a collecting agent and No. 2 oil is used as a foaming agent in flotation decarburization, but the flotation efficiency is poor. Patent CN112844852A discloses a method for decarbonizing carbon-containing solid waste of electrolytic aluminum by using a mixed collector of hydrocarbon oil, lipid oil, phthalic acid ester and the like, wherein although the flotation effect is improved, the oil consumption is large, the treatment effect on the fine carbon-containing solid waste is poor, the content of carbon impurities in the obtained cosolvent is still high, and the continuous cyclic utilization is difficult.
Disclosure of Invention
The invention aims to provide a W/O type emulsion collecting agent for electrolytic aluminum and preparation and application thereof, which are mainly characterized by resource utilization of high-carbon waste residues and solve the technical problems of large oil consumption, poor flotation efficiency and difficulty in recycling cosolvent in the existing flotation decarburization process. The carbon separated by the method can be used as a raw material for preparing a high-value carbon material, and the cosolvent can be recycled.
In order to realize the purpose, the invention is realized by the following technical scheme:
the invention provides a preparation method of a W/O type emulsion collector for aluminum electrolysis, which comprises the following steps:
step 1: adding kerosene into alkyl glycoside or polyisobutene ethanolamine, and stirring to obtain a liquid product A;
step 2: and adding the KCl solution into the liquid product A, and continuously stirring to obtain the W/O type emulsion collector.
In the technical scheme, the high internal phase W/O type emulsion collector is prepared by adopting kerosene as an external phase, KCl solution as an internal phase and alkyl glycoside (or polyisobutene ethanolamine) as an emulsifier. The emulsifier is green and degradable, and the obtained emulsion has high volume ratio of the water phase in the emulsion, uniform size distribution of emulsion droplets and strong stability.
Preferably, the mass ratio of the kerosene to the alkyl glycoside or the polyisobutene ethanolamine in the step 1 is 5.
Preferably, in the step 1, the stirring speed is 1000 to 2000r/min, and the stirring time is 5 to 10min.
Preferably, the mass concentration of the KCl solution in the step 2 is 6-7%; the volume ratio of the KCl solution to the liquid product A is 4.
Preferably, the KCl solution in the step 2 is dropwise added into the liquid product A at a constant speed of 2-4 mL/min, and the stirring speed is 1100-2000 r/min along with continuous stirring during the dropwise adding process, so as to prevent the emulsion from phase inversion.
Preferably, in the step 2, the stirring speed is 8000-10000 r/min, and the stirring time is 10-15 min, so that the particle size of the emulsion collector is uniform.
In another aspect, the invention provides a W/O type emulsion collector prepared by the above method.
The invention also provides application of the W/O type emulsion collector in separation of carbon-containing solid wastes of electrolytic aluminum, which specifically comprises the following steps:
step 1: adding the electrolytic aluminum carbon slag into water, and stirring to obtain a mixed solution B;
and 2, step: adding the W/O type emulsion collecting agent into the mixed solution B, and stirring to obtain mixed solution C;
and step 3: and adding a foaming agent into the mixed solution C, introducing air for flotation separation, and scraping bubbles to obtain a carbon substance.
Preferably, the solid-liquid mass ratio of the electrolytic aluminum carbon slag to the water in the step 1 is 1; the mass ratio of the W/O type emulsion collector to the mixed liquor B in the step 2 is 1.
Preferably, in the step 3, the foaming agent is sec-octanol, the addition amount of the sec-octanol is 0.4 to 0.5 times of the addition amount of the W/O type emulsion collector, and the conditions of flotation separation are as follows: stirring is continuously carried out at the speed of 1000-1200 r/min, the gas flow is controlled to be 10-15 mL/min, the flotation time is 5-8 min, and the bubble scraping is carried out at the speed of 10-15 s.
Compared with the prior art, the invention has the following beneficial effects:
the W/O type emulsion collector provided by the invention can realize high-efficiency removal and recovery of carbon resources in the electrolytic aluminum carbon residue (the flotation yield of carbon reaches 80-85%) by a flotation method under the condition of low consumption, and simultaneously greatly reduces the content of carbon impurities in a cosolvent, and has the advantages of simple process, economy, high efficiency and the like. The carbon obtained by flotation separation can be used for preparing high-value carbon materials, and the cosolvent can be recycled in the electrolytic aluminum process, so that the method has very important significance for the sustainable development of the electrolytic aluminum industry and the resource utilization of carbon slag.
Drawings
FIG. 1 is a microscopic view of a W/O type emulsion collector of the present invention.
Detailed Description
In order to facilitate understanding of the present invention, the present invention will be described in more detail with reference to the accompanying drawings and examples. It should be understood that the specific embodiments described herein are merely illustrative of the present application and do not limit the invention.
Example 1
Preparation of W/O type emulsion collector
Step 1: adding 6.25g of kerosene into 1.25g of alkyl glycoside, and stirring at the speed of 1000r/min for 5min to obtain a liquid product A;
step 2: dropwise adding 35g of KCl solution with the mass concentration of 6% into the liquid product A at a constant speed of 2mL/min through a flow meter, and continuously stirring at a speed of 1100r/min in the dropwise adding process until the addition of the KCl solution is finished to obtain a liquid product B;
and step 3: and (4) transferring the liquid product B into a high-speed stirrer, and stirring for 10min at the speed of 8000r/min to obtain the W/O type emulsion collector. The type of the emulsion is judged by a dilution dispersion method and a fluorescent dyeing method, the size of the emulsion is measured by an optical microscope and dynamic light scattering, and the size of the emulsion drops is mainly distributed in 10-40 mu m.
Application of W/O type emulsion collector
Step 1: adding 5g of electrolytic aluminum carbon slag into 100mL of water, stirring and dispersing for 5min to fully wet a carbon slag sample to obtain a mixed solution D;
step 2: adding 3.1mg of the W/O type emulsion collector prepared by the method into the mixed solution D, and continuously stirring for 2min at the stirring speed of 1000r/min to obtain mixed solution E;
and step 3: transferring the mixed solution E into a flotation tube, adding 1.24mg of sec-octanol serving as a foaming agent into the flotation tube, continuously stirring at a stirring speed of 1000r/min, introducing air from the bottom of the flotation tube, controlling the gas flow to be 10mL/min, performing flotation for 5min, scraping out foams floating to the top of the flotation tube at a time interval of 10s, performing suction filtration, washing, drying and recovering to obtain a carbon product, wherein the flotation yield of carbon is 80%;
and 4, step 4: and (3) carrying out suction filtration, washing, drying and recovery on the product remained in the flotation tube to obtain the cosolvent for the electrolytic aluminum, wherein the recovery rate of the cosolvent is 88%.
Example 2
Preparation of W/O type emulsion collector
Step 1: adding 4.5g of kerosene into 1.5g of polyisobutene ethanolamine (PIB), and stirring at the speed of 1100r/min for 6min to obtain a liquid product A;
and 2, step: dropwise adding 40g of KCl solution with the mass concentration of 6% into the liquid product A at a constant speed of 3mL/min through a flowmeter, and continuously stirring at a speed of 1200r/min in the dropwise adding process until the addition of the KCl solution is finished to obtain a liquid product B;
and step 3: and (3) transferring the liquid product B into a high-speed stirrer, stirring for 12min at a speed of 9000r/min to obtain a W/O type emulsion collecting agent, judging the type of the emulsion by a dilution dispersion method and a fluorescent dyeing method, measuring the size of the emulsion by adopting an optical microscope and dynamic light scattering, and mainly distributing the size of emulsion droplets to 20-40 mu m.
Application of W/O type emulsion collector
Step 1: adding 6g of electrolytic aluminum carbon slag into 130mL of water, stirring and dispersing for 6min to fully wet a carbon slag sample to obtain a mixed solution D;
and 2, step: adding 4.1mg of the W/O type emulsion collector prepared by the method into the mixed solution D, and continuously stirring for 2min at the stirring speed of 1100r/min to obtain mixed solution E;
and 3, step 3: transferring the mixed solution E into a flotation tube, adding 1.85mg of sec-octanol serving as a foaming agent into the mixed solution E, continuously stirring at the stirring speed of 1100r/min, introducing air from the bottom of the flotation tube, controlling the gas flow to be 12mL/min, carrying out flotation for 8min, scraping out foams floating to the top of the flotation tube at the speed of 12s time interval, carrying out suction filtration, washing, drying and recovering to obtain a carbon product, wherein the flotation yield of carbon is 82%;
and 4, step 4: and (3) carrying out suction filtration, washing, drying and recovery on the product remained in the flotation tube to obtain the cosolvent for electrolytic aluminum, wherein the recovery rate of the cosolvent is 90%.
Example 3
Preparation of W/O type emulsion collector
Step 1: adding 8g of kerosene into 2g of alkyl glycoside, and stirring at the rotating speed of 1500r/min for 8min to obtain a liquid product A;
step 2: dropwise adding 70g of KCl solution with the mass concentration of 7% into the liquid product A at a constant speed of 4mL/min through a flowmeter, and stirring at a speed of 1800r/min in the dropwise adding process until the addition of the KCl solution is finished to obtain a liquid product B;
and 3, step 3: and (3) transferring the liquid product B into a high-speed stirrer, stirring for 14min at a speed of 9000r/min to obtain a W/O type emulsion collecting agent, judging the type of the emulsion by a dilution dispersion method and a fluorescent dyeing method, measuring the size of the emulsion by adopting an optical microscope and dynamic light scattering, and mainly distributing the size of emulsion droplets to 10-40 mu m.
Application of W/O type emulsion collector
Step 1: adding 8g of electrolytic aluminum carbon slag into 185mL of ultrapure water, stirring and dispersing for 8min to fully wet a carbon slag sample to obtain a mixed solution D;
step 2: adding 5.8mg of the W/O type emulsion collector prepared by the method into the mixed solution D, and continuously stirring for 3min at the stirring speed of 1200r/min to obtain mixed solution E;
and 3, step 3: transferring the mixed solution E into a flotation tube, adding 2.9mg of sec-octanol serving as a foaming agent into the mixed solution E, continuously stirring at the stirring speed of 1200r/min, introducing air from the bottom of the flotation tube, controlling the gas flow to be 14mL/min, performing flotation for 6min, scraping out foams floating to the top of the flotation tube at the speed of 14s, performing suction filtration, washing, drying and recovering to obtain a carbon product, wherein the flotation yield of carbon is 85%;
and 4, step 4: and (3) carrying out suction filtration, washing, drying and recovery on the product remained in the flotation tube to obtain the cosolvent for electrolytic aluminum, wherein the recovery rate of the cosolvent is 93%.
Example 4
Preparation of W/O type emulsion collector
Step 1: adding 10g of kerosene into 2.5g of polyisobutene ethanolamine, and stirring at the speed of 2000r/min for 10min to obtain a liquid product A;
step 2: dropwise adding 100g of KCl solution with the mass concentration of 6% into the liquid product A at a constant speed of 4mL/min through a flow meter, and continuously stirring at a speed of 2000r/min in the dropwise adding process until the addition of the KCl solution is finished to obtain a liquid product B;
and step 3: and (3) transferring the liquid product B into a high-speed stirrer, stirring for 15min at the speed of 10000r/min to obtain a W/O type emulsion collecting agent, judging the type of the emulsion by a dilution dispersion method and a fluorescent dyeing method, measuring the size of the emulsion by adopting an optical microscope and dynamic light scattering, and mainly distributing the size of emulsion droplets to 10-30 mu m.
Application of W/O type emulsion collector
Step 1: adding 10g of electrolytic aluminum carbon slag into 250mL of ultrapure water, stirring and dispersing for 10min to fully wet a carbon slag sample to obtain a mixed solution D;
step 2: adding 7.9mg of the W/O type emulsion collector prepared by the method into the mixed solution D, and continuously stirring for 3min at the stirring speed of 1200r/min to obtain mixed solution E;
and 3, step 3: transferring the mixed solution E into a flotation tube, adding 3.95mg of sec-octanol serving as a foaming agent into the mixed solution E, continuously stirring at the stirring speed of 1200r/min, introducing air from the bottom of the flotation tube, controlling the gas flow to be 15mL/min, carrying out flotation for 5min, scraping out foams floating to the top of the flotation tube at the speed of 15s time interval, carrying out suction filtration, washing, drying and recovering to obtain a carbon product, wherein the flotation yield of carbon is 83%;
and 4, step 4: and (3) carrying out suction filtration, washing, drying and recovery on the product remained in the flotation tube to obtain the cosolvent for the electrolytic aluminum, wherein the recovery rate of the cosolvent is 89%.
All possible combinations of the technical features of the above embodiments may not be described for the sake of brevity, but should be considered as within the scope of the present disclosure as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. A preparation method of a W/O type emulsion collector for electrolyzing aluminum is characterized in that: the method comprises the following steps:
step 1: adding kerosene into alkyl glycoside or polyisobutene ethanolamine, and stirring to obtain a liquid product A;
step 2: and adding the KCl solution into the liquid product A, and continuously stirring to obtain the W/O type emulsion collector.
2. A method of preparing a W/O type emulsion collector for electrolytic aluminum according to claim 1, characterized in that: the mass ratio of the kerosene to the alkyl glycoside or the polyisobutene ethanolamine in the step 1 is 5-3.
3. A method of preparing a W/O type emulsion collector for electrolytic aluminum according to claim 1, characterized in that: in the step 1, the stirring speed is 1000-2000 r/min, and the stirring time is 5-10 min.
4. A method of preparing a W/O type emulsion collector for electrolytic aluminum according to claim 1, characterized in that: the mass concentration of the KCl solution in the step 2 is 6-7%; the volume ratio of the KCl solution to the liquid product A is 4.
5. A method of preparing a W/O type emulsion collector for electrolytic aluminum according to claim 1, characterized in that: and (3) dropwise adding the KCl solution into the liquid product A at a constant speed of 2-4 mL/min in the step (2), and continuously stirring in the dropwise adding process, wherein the stirring speed is 1100-2000 r/min.
6. A method of preparing a W/O type emulsion collector for electrolytic aluminum according to claim 1, characterized in that: in the step 2, the stirring speed is 8000-10000 r/min, and the stirring time is 10-15 min.
7. A W/O type emulsion collector prepared by the method of any one of claims 1 to 6.
8. The application of the W/O type emulsion collector prepared by the method of any one of claims 1 to 6 or the W/O type emulsion collector of claim 7 in the separation of solid waste containing carbon in electrolytic aluminum is characterized in that: the method comprises the following steps:
step 1: adding the electrolytic aluminum carbon slag into water, and stirring to obtain a mixed solution B;
step 2: adding the W/O type emulsion collecting agent into the mixed solution B, and stirring to obtain a mixed solution C;
and 3, step 3: and then adding a foaming agent into the mixed solution C, introducing air to perform flotation separation, and performing foam scraping to obtain a carbon substance.
9. Use of a W/O type emulsion collector according to claim 8, characterized in that: the solid-liquid mass ratio of the electrolytic aluminum carbon slag to the water in the step 1 is 1-20; the mass ratio of the W/O type emulsion collector to the mixed liquor B in the step 2 is 1.
10. Use of a W/O type emulsion collector according to claim 9, characterized in that: the conditions of flotation separation are as follows: in the step 3, the foaming agent is sec-octanol, the addition amount of the sec-octanol is 0.4 to 0.5 times of the addition amount of the W/O type emulsion collecting agent, and the conditions of flotation separation are as follows: stirring is continuously carried out at the speed of 1000-1200 r/min, the gas flow is controlled to be 10-15 mL/min, the flotation time is 5-8 min, and foam scraping is carried out at the speed of 10-15 s.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115846056A (en) * | 2022-11-10 | 2023-03-28 | 山西大学 | W/O type microemulsion collecting agent for low-rank coal flotation, and preparation and application thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115846056A (en) * | 2022-11-10 | 2023-03-28 | 山西大学 | W/O type microemulsion collecting agent for low-rank coal flotation, and preparation and application thereof |
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