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 PDF

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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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type emulsion
electrolytic aluminum
stirring
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carbon
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程芳琴
李恩泽
薛芳斌
成怀刚
樊彪
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Shanxi University
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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
    • 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

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Abstract

本发明属于碳渣资源化利用领域,一种用于电解铝的W/O型乳液捕收剂及其制备与应用。本发明采用煤油为外相、KCl溶液为内相、烷基糖苷(或聚异丁烯乙醇胺)为乳化剂,制备出一种高内相W/O型乳液捕收剂,并将其用于电解铝碳渣的浮选脱碳提质过程中,在耗油量较低的情况下能够实现碳渣中碳资源的高效脱除、降低助溶剂中碳杂质的含量,助溶剂可循环再利用于电解铝过程中,对于电解铝产业的可续发展以及碳渣的资源化利用意义重大,有着良好的应用前景。

Figure 202210899277

The invention belongs to the field of carbon residue resource utilization, and relates to a W/O type emulsion collector for electrolytic aluminum and its preparation and application. The present invention adopts kerosene as the outer phase, KCl solution as the inner phase, and alkyl glycoside (or polyisobutylene ethanolamine) as the emulsifier to prepare a high inner phase W/O type emulsion collector, which is used for electrolysis of aluminum carbon In the process of flotation, decarburization and upgrading of slag, it can achieve efficient removal of carbon resources in carbon slag and reduce the content of carbon impurities in co-solvent under the condition of low oil consumption, and the co-solvent can be recycled for electrolytic aluminum. In the process, it is of great significance to the sustainable development of the electrolytic aluminum industry and the resource utilization of carbon slag, and has a good application prospect.

Figure 202210899277

Description

一种用于电解铝的W/O型乳液捕收剂及其制备与应用A W/O emulsion collector for electrolytic aluminum and its preparation and application

技术领域technical field

本发明属于碳渣资源化利用领域,具体涉及一种用于电解铝的W/O型乳液捕收剂及其制备与应用。The invention belongs to the field of resource utilization of carbon slag, and in particular relates to a W/O emulsion collector for electrolytic aluminum and its preparation and application.

背景技术Background technique

我国已成为全球第一大铝消费国,电解铝工业也随之迅速发展,产能已接近4000万吨/年。电解铝过程中,阴极和阳极均为含碳材料,阴阳极碳材料因电化学反应和电解质浸泡发生消耗、剥落、破碎等,会产生大量碳渣。碳渣与电解必需的助溶剂混合,导致助溶剂效率降低,最终表现为含碳固废。同时该固废也会混有电解质中的盐,只能以危废堆弃,造成资源浪费和处理费用增加。my country has become the world's largest aluminum consumer, and the electrolytic aluminum industry has also developed rapidly, with a production capacity of nearly 40 million tons per year. In the process of electrolytic aluminum, both the cathode and the anode are carbon-containing materials, and the carbon materials of the cathode and anode are consumed, peeled off, broken, etc. due to electrochemical reactions and electrolyte immersion, and a large amount of carbon slag will be generated. The carbon residue is mixed with the necessary co-solvent for electrolysis, resulting in a decrease in the efficiency of the co-solvent, which eventually appears as carbon-containing solid waste. At the same time, the solid waste will also be mixed with salt in the electrolyte, so it can only be dumped as hazardous waste, resulting in waste of resources and increased treatment costs.

实现电解铝含碳固废资源化利用的重要步骤是将碳与助溶剂分离,二者分离主要手段为浮选法。浮选脱碳常用柴油为捕收剂、2号油为起泡剂,但浮选效率差。专利CN112844852A公布了一种由烃类油、脂类油、邻苯二甲酸酯等混合捕收剂用于电解铝含碳固废脱碳,尽管浮选效果有所提升,但油用量大,且对于细粒含碳固废处理效果差,所得助溶剂碳杂质含量仍较高,难以继续循环利用。The important step to realize the resource utilization of electrolytic aluminum carbon-containing solid waste is to separate the carbon from the co-solvent, and the main means of separation is the flotation method. In flotation decarbonization, diesel oil is commonly used as collector and No. 2 oil is used as foaming agent, but the flotation efficiency is poor. Patent CN112844852A discloses a mixed collector made of hydrocarbon oil, lipid oil, phthalate, etc. for the decarbonization of carbon-containing solid waste in electrolytic aluminum. Although the flotation effect has been improved, the oil consumption is large. Moreover, the treatment effect on fine-grained carbon-containing solid waste is poor, and the carbon impurity content of the obtained co-solvent is still high, making it difficult to continue recycling.

发明内容Contents of the invention

本发明的目的在于提供一种用于电解铝的W/O型乳液捕收剂及其制备与应用,以高碳废渣资源化利用为重点,解决现有浮选脱碳工艺中油用量大、浮选效率差、助溶剂难以回收利用的技术问题。本发明分离出的碳可作为原料用于制备高值碳材料,助溶剂可以循环利用。The purpose of the present invention is to provide a W/O type emulsion collector for electrolytic aluminum and its preparation and application, focusing on the resource utilization of high-carbon waste residue, to solve the problem of large oil consumption and flotation in the existing flotation decarbonization process. The technical problems of poor selection efficiency and difficult recovery of co-solvent. The carbon separated by the invention can be used as a raw material to prepare high-value carbon materials, and the auxiliary solvent can be recycled.

为实现上述目的,本发明是通过以下技术方案来实现:To achieve the above object, the present invention is achieved through the following technical solutions:

本发明一方面提供了一种用于电解铝的W/O型乳液捕收剂的制备方法,包括以下步骤:One aspect of the present invention provides a method for preparing a W/O emulsion collector for electrolytic aluminum, comprising the following steps:

步骤1:将煤油加入至烷基糖苷或聚异丁烯乙醇胺中,搅拌,得到液体产物A;Step 1: adding kerosene to alkyl glucoside or polyisobutene ethanolamine, stirring to obtain liquid product A;

步骤2:将KCl溶液加入至液体产物A中,继续搅拌,即得所述W/O型乳液捕收剂。Step 2: Add the KCl solution into the liquid product A and continue stirring to obtain the W/O emulsion collector.

上述技术方案中,采用煤油为外相、KCl溶液为内相、烷基糖苷(或聚异丁烯乙醇胺)为乳化剂,制备出一种高内相W/O型乳液捕收剂。其中,所用乳化剂为绿色可降解,所得乳液内水相体积比例高、乳滴尺寸分布均匀、稳定性强。In the above technical solution, kerosene is used as the external phase, KCl solution is used as the internal phase, and alkyl glycoside (or polyisobutene ethanolamine) is used as an emulsifier to prepare a high internal phase W/O emulsion collector. Among them, the emulsifier used is green and degradable, and the obtained emulsion has a high volume ratio of the water phase, uniform emulsion droplet size distribution, and strong stability.

作为优选,所述步骤1中煤油与烷基糖苷或聚异丁烯乙醇胺的质量比为5:1~3:1。Preferably, the mass ratio of kerosene to alkyl glycoside or polyisobutene ethanolamine in step 1 is 5:1-3:1.

作为优选,所述步骤1中搅拌速度为1000~2000r/min,搅拌时间为5~10min。Preferably, in the step 1, the stirring speed is 1000-2000 r/min, and the stirring time is 5-10 min.

作为优选,所述步骤2中KCl溶液质量浓度为6~7%;KCl溶液与液体产物A的体积比为4:1~6:1。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 4:1-6:1.

作为优选,所述步骤2中KCl溶液以2~4mL/min的速度匀速滴加至液体产物A中,且滴加过程中伴随持续搅拌,搅拌速度为1100~2000r/min,以防止乳液转相。As a preference, in the step 2, the KCl solution is added dropwise to the liquid product A at a constant speed of 2 to 4 mL/min, and the dropping process is accompanied by continuous stirring at a stirring speed of 1100 to 2000 r/min to prevent phase inversion of the emulsion .

作为优选,所述步骤2中搅拌速度为8000~10000r/min,搅拌时间为10~15min,以使乳液捕收剂粒径均匀。Preferably, in the step 2, the stirring speed is 8000-10000 r/min, and the stirring time is 10-15 minutes, so that the particle size of the emulsion collector is uniform.

本发明另一方面提供了上述方法制备的W/O型乳液捕收剂。Another aspect of the present invention provides the W/O emulsion collector prepared by the above method.

本发明另一方面还提供了上述W/O型乳液捕收剂在电解铝含碳固废分离中的应用,具体包括以下步骤:Another aspect of the present invention also provides the application of the above-mentioned W/O emulsion collector in the separation of electrolytic aluminum carbon-containing solid waste, which specifically includes the following steps:

步骤1:将电解铝碳渣加入至水中,搅拌,得到混合液B;Step 1: Add electrolytic aluminum carbon slag into water, stir to obtain mixed solution B;

步骤2:向混合液B中加入所述W/O型乳液捕收剂,搅拌,得到混合液C;Step 2: Add the W/O type emulsion collector to the mixed solution B and stir to obtain the mixed solution C;

步骤3:然后向混合液C中加入起泡剂,通入空气进行浮选分离,进行刮泡,得到碳物质。Step 3: Then add a foaming agent to the mixed solution C, pass in air for flotation separation, and scrape to obtain carbon substances.

作为优选,所述步骤1中电解铝碳渣与水的固液质量比为1:20~1:25;所述步骤2中W/O型乳液捕收剂与混合液B的质量比为1:33000~1:34000,搅拌速度为1000~1200r/min,搅拌时间为2~3min。As a preference, the solid-to-liquid mass ratio of electrolytic aluminum carbon slag to water in step 1 is 1:20 to 1:25; the mass ratio of W/O emulsion collector to mixed solution B in step 2 is 1 :33000~1:34000, the stirring speed is 1000~1200r/min, and the stirring time is 2~3min.

作为优选,所述步骤3中起泡剂为仲辛醇,仲辛醇的添加量为W/O型乳液捕收剂添加量的0.4~0.5倍,浮选分离的条件为:以1000~1200r/min的速度持续搅拌,气体流量控制为10~15mL/min,浮选时间为5~8min,以时间间隔为10~15s的速度进行刮泡。As preferably, in the step 3, the foaming agent is secondary octanol, and the amount of secondary octanol added is 0.4 to 0.5 times that of the W/O emulsion collector, and the conditions for flotation separation are: 1000 to 1200r Stir continuously at a speed of 1/min, the gas flow rate is controlled at 10-15mL/min, the flotation time is 5-8min, and the time interval is 10-15s for scraping.

与现有技术相比,本发明的有益效果如下:Compared with the prior art, the beneficial effects of the present invention are as follows:

本发明提供的W/O型乳液捕收剂在用量较低的情况下可通过浮选法实现电解铝碳渣中碳资源的高效脱除与回收(碳的浮选收率达80%~85%),同时大大降低了助溶剂中碳杂质的含量,具有工艺简单、经济高效等优点。本发明浮选分离所得碳可用于高值碳材料的制备,助溶剂可循环再利用于电解铝过程中,对于电解铝产业的可续发展以及碳渣的资源化利用具有十分重要的意义。The W/O type emulsion collector provided by the present invention can realize the efficient removal and recovery of carbon resources in electrolytic aluminum carbon slag by the flotation method when the dosage is relatively low (the flotation yield of carbon reaches 80%-85%) %), while greatly reducing the content of carbon impurities in the co-solvent, and has the advantages of simple process, cost-effective and high-efficiency. The carbon obtained by flotation separation in the present invention can be used for the preparation of high-value carbon materials, and the cosolvent can be recycled and reused in the electrolytic aluminum process, which is of great significance to the sustainable development of the electrolytic aluminum industry and the resource utilization of carbon slag.

附图说明Description of drawings

图1为本发明W/O型乳液捕收剂的显微镜图。Fig. 1 is a micrograph of the W/O emulsion collector of the present invention.

具体实施方式Detailed ways

为了便于理解本发明,下面将结合附图及实施例对本发明进行更详细地记载。应当理解,此处描述的具体实施例仅仅用以解释本申请,并不用于限定发明。In order to facilitate understanding of the present invention, the present invention will be described in more detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described here are only used to explain the present application, and are not intended to limit the invention.

实施例1Example 1

W/O型乳液捕收剂的制备Preparation of W/O Type Emulsion Collector

步骤1:将6.25g煤油加入到1.25g烷基糖苷中,以1000r/min速度搅拌5min,得到液体产物A;Step 1: Add 6.25g of kerosene to 1.25g of alkyl glucoside, and stir at a speed of 1000r/min for 5min to obtain liquid product A;

步骤2:将35g质量浓度为6%的KCl溶液通过流量计以2mL/min的速度匀速滴加至液体产物A中,在滴加过程以1100r/min的速度继续搅拌至KCl溶液添加结束,得到液体产物B;Step 2: 35g of KCl solution with a mass concentration of 6% is added dropwise to the liquid product A at a constant speed of 2mL/min through a flowmeter, and the stirring is continued at a speed of 1100r/min during the dropping process until the addition of the KCl solution is completed to obtain liquid product B;

步骤3:将液体产物B移至高速搅拌机中,在8000r/min速度下搅拌10min,得到W/O型乳液捕收剂。乳液类型通过稀释分散法和荧光染色法进行判定,乳液尺寸大小采用光学显微镜和动态光散射进行测定,乳滴尺寸大小主要分布于10~40μm。Step 3: Move the liquid product B to a high-speed mixer, and stir for 10 minutes at a speed of 8000 r/min to obtain a W/O emulsion collector. The type of emulsion was judged by dilution dispersion method and fluorescent dyeing method. The size of emulsion was measured by optical microscope and dynamic light scattering. The size of emulsion droplet was mainly distributed in the range of 10-40 μm.

W/O型乳液捕收剂的应用Application of W/O Type Emulsion Collector

步骤1:将5g电解铝碳渣加入到100mL水中搅拌分散5min,使碳渣样品充分润湿,得到混合液D;Step 1: Add 5g of electrolytic aluminum carbon slag to 100mL of water and stir for 5 minutes to make the carbon slag sample fully wet to obtain the mixed solution D;

步骤2:将3.1mg上述方法制得的W/O型乳液捕收剂加入到混合液D中,以1000r/min搅拌速度继续搅拌2min,得到混合液E;Step 2: Add 3.1 mg of the W/O emulsion collector prepared by the above method into the mixed solution D, and continue stirring at a stirring speed of 1000 r/min for 2 minutes to obtain the mixed solution E;

步骤3:将混合液E转移至浮选管中,向其中加入1.24mg仲辛醇作为起泡剂,以1000r/min搅拌速度持续搅拌,从浮选管底部通入空气,气体流量控制为10mL/min,浮选5min,以时间间隔为10s的速度将上浮至浮选管顶部的泡沫刮出,进行抽滤,洗涤,干燥,回收,即得碳产品,碳的浮选收率为80%;Step 3: Transfer the mixed liquid E to the flotation tube, add 1.24mg of 2-octanol as a foaming agent, keep stirring at a stirring speed of 1000r/min, pass air from the bottom of the flotation tube, and control the gas flow rate to 10mL /min, flotation for 5 minutes, scrape off the foam floating to the top of the flotation tube at a time interval of 10s, perform suction filtration, wash, dry, and recycle to obtain carbon products, and the flotation yield of carbon is 80% ;

步骤4:残留在浮选管中的产品进行抽滤,洗涤,干燥,回收,即得电解铝用助溶剂,助溶剂回收率为88%。Step 4: The product remaining in the flotation tube is subjected to suction filtration, washed, dried, and recovered to obtain a co-solvent for electrolytic aluminum, and the recovery rate of the co-solvent is 88%.

实施例2Example 2

W/O型乳液捕收剂的制备Preparation of W/O Type Emulsion Collector

步骤1:将4.5g煤油加入到1.5g聚异丁烯乙醇胺(PIB)中,以1100r/min速度搅拌6min,得到液体产物A;Step 1: Add 4.5g of kerosene to 1.5g of polyisobutene ethanolamine (PIB), and stir at a speed of 1100r/min for 6min to obtain a liquid product A;

步骤2:将40g质量浓度为6%的KCl溶液通过流量计以3mL/min的速度匀速滴加至液体产物A中,在滴加过程以1200r/min的速度继续搅拌至KCl溶液添加结束,得到液体产物B;Step 2: 40g of KCl solution with a mass concentration of 6% is added dropwise to the liquid product A at a constant speed of 3mL/min through a flowmeter, and the stirring is continued at a speed of 1200r/min during the dropping process until the addition of the KCl solution is completed to obtain liquid product B;

步骤3:将液体产物B移至高速搅拌机中,在9000r/min速度下搅拌12min,得到W/O型乳液捕收剂,乳液类型通过稀释分散法和荧光染色法进行判定,乳液尺寸大小采用光学显微镜和动态光散射进行测定,乳滴尺寸大小主要分布于20~40μm。Step 3: Move the liquid product B to a high-speed mixer, and stir at a speed of 9000r/min for 12 minutes to obtain a W/O emulsion collector. The emulsion type is determined by dilution dispersion and fluorescent dyeing. The size of the emulsion is determined by optical Microscope and dynamic light scattering are used to measure, and the size of emulsion droplets is mainly distributed in the range of 20-40 μm.

W/O型乳液捕收剂的应用Application of W/O Type Emulsion Collector

步骤1:将6g电解铝碳渣加入到130mL水中搅拌分散6min,使碳渣样品充分润湿,得到混合液D;Step 1: Add 6g of electrolytic aluminum carbon slag into 130mL water and stir and disperse for 6 minutes to fully wet the carbon slag sample to obtain a mixed solution D;

步骤2:将4.1mg上述方法制得的W/O型乳液捕收剂加入到混合液D中,以1100r/min搅拌速度继续搅拌2min,得到混合液E;Step 2: Add 4.1 mg of the W/O emulsion collector prepared by the above method into the mixed solution D, and continue stirring at a stirring speed of 1100 r/min for 2 minutes to obtain the mixed solution E;

步骤3:将混合液E转移至浮选管中,向其中加入1.85mg仲辛醇作为起泡剂,以1100r/min搅拌速度持续搅拌,从浮选管底部通入空气,气体流量控制为12mL/min,浮选8min,以时间间隔为12s的速度将上浮至浮选管顶部的泡沫刮出,进行抽滤,洗涤,干燥,回收,即得碳产品,碳的浮选收率为82%;Step 3: Transfer the mixed solution E to the flotation tube, add 1.85 mg of 2-octanol as a foaming agent, keep stirring at a stirring speed of 1100 r/min, and feed air from the bottom of the flotation tube, and control the gas flow rate to 12 mL /min, flotation for 8min, scraping off the foam floating to the top of the flotation tube at a time interval of 12s, performing suction filtration, washing, drying, and recycling to obtain carbon products, and the flotation yield of carbon is 82% ;

步骤4:将残留在浮选管中的产品进行抽滤,洗涤,干燥,回收,即得电解铝用助溶剂,助溶剂的回收率为90%。Step 4: The product remaining in the flotation tube is suction-filtered, washed, dried, and recovered to obtain a co-solvent for electrolytic aluminum, and the recovery rate of the co-solvent is 90%.

实施例3Example 3

W/O型乳液捕收剂的制备Preparation of W/O Type Emulsion Collector

步骤1:将8g煤油加入到2g烷基糖苷中,以1500r/min转速搅拌8min,得到液体产物A;Step 1: Add 8g of kerosene to 2g of alkyl glucoside, and stir at 1500r/min for 8min to obtain liquid product A;

步骤2:将70g质量浓度为7%的KCl溶液通过流量计以4mL/min的速度匀速滴加至液体产物A中,在滴加过程以1800r/min的速度搅拌至KCl溶液添加结束,得到液体产物B;Step 2: 70g of KCl solution with a mass concentration of 7% is added dropwise at a constant speed of 4mL/min to the liquid product A through a flowmeter, and stirred at a speed of 1800r/min during the dropping process until the addition of the KCl solution is completed to obtain a liquid product B;

步骤3:将液体产物B移至高速搅拌机中,在9000r/min速度下搅拌14min,得到W/O型乳液捕收剂,乳液类型通过稀释分散法和荧光染色法进行判定,乳液尺寸大小采用光学显微镜和动态光散射进行测定,乳滴尺寸大小主要分布于10~40μm。Step 3: Move the liquid product B to a high-speed mixer, and stir at a speed of 9000r/min for 14 minutes to obtain a W/O emulsion collector. The emulsion type is determined by dilution dispersion and fluorescent dyeing. The size of the emulsion is determined by optical Microscope and dynamic light scattering were used to measure, and the size of emulsion droplets was mainly distributed in the range of 10-40 μm.

W/O型乳液捕收剂的应用Application of W/O Type Emulsion Collector

步骤1:将8g电解铝碳渣加入到185mL超纯水中搅拌分散8min,使碳渣样品充分润湿,得到混合液D;Step 1: Add 8g of electrolytic aluminum carbon slag to 185mL ultrapure water and stir for 8 minutes to make the carbon slag sample fully wet to obtain the mixed solution D;

步骤2:将5.8mg上述方法制得的W/O型乳液捕收剂加入到混合液D中,以1200r/min搅拌速度继续搅拌3min,得到混合液E;Step 2: Add 5.8 mg of the W/O emulsion collector prepared by the above method into the mixed solution D, and continue stirring at a stirring speed of 1200 r/min for 3 minutes to obtain the mixed solution E;

步骤3:将混合液E转移至浮选管中,向其中加入2.9mg仲辛醇作为起泡剂,以1200r/min搅拌速度持续搅拌,从浮选管底部通入空气,气体流量控制为14mL/min,浮选6min,以时间间隔为14s的速度将上浮至浮选管顶部的泡沫刮出,进行抽滤,洗涤,干燥,回收,即得碳产品,碳的浮选收率为85%;Step 3: Transfer the mixed solution E to the flotation tube, add 2.9mg of 2-octanol as a foaming agent, keep stirring at a stirring speed of 1200r/min, feed air from the bottom of the flotation tube, and control the gas flow rate to 14mL /min, flotation for 6 minutes, scrape off the foam floating to the top of the flotation tube at a time interval of 14s, perform suction filtration, wash, dry, and recycle to obtain carbon products, and the flotation yield of carbon is 85% ;

步骤4:残留在浮选管中的产品进行抽滤,洗涤,干燥,回收,即得电解铝用助溶剂,助溶剂的回收率为93%。Step 4: The product remaining in the flotation tube is suction filtered, washed, dried, and recovered to obtain a cosolvent for electrolytic aluminum, and the recovery rate of the cosolvent is 93%.

实施例4Example 4

W/O型乳液捕收剂的制备Preparation of W/O Type Emulsion Collector

步骤1:将10g煤油加入到2.5g聚异丁烯乙醇胺中,以2000r/min速度搅拌10min,得到液体产物A;Step 1: Add 10 g of kerosene to 2.5 g of polyisobutene ethanolamine, and stir at a speed of 2000 r/min for 10 min to obtain a liquid product A;

步骤2:将100g质量浓度为6%的KCl溶液通过流量计以4mL/min的速度匀速滴加至液体产物A中,在滴加过程以2000r/min的速度继续搅拌至KCl溶液添加结束,得到液体产物B;Step 2: 100g of KCl solution with a mass concentration of 6% is added dropwise at a constant speed of 4mL/min to the liquid product A through a flowmeter, and the stirring is continued at a speed of 2000r/min during the dropping process until the addition of the KCl solution is completed to obtain liquid product B;

步骤3:将液体产物B移至高速搅拌机中,在10000r/min速度下搅拌15min,得到W/O型乳液捕收剂,乳液类型通过稀释分散法和荧光染色法进行判定,乳液尺寸大小采用光学显微镜和动态光散射进行测定,乳滴尺寸大小主要分布于10~30μm。Step 3: Move the liquid product B to a high-speed mixer and stir for 15 minutes at a speed of 10,000r/min to obtain a W/O emulsion collector. The type of emulsion is determined by dilution dispersion and fluorescent dyeing. The size of the emulsion is determined by optical Microscope and dynamic light scattering were used to measure, and the size of emulsion droplets was mainly distributed in the range of 10-30 μm.

W/O型乳液捕收剂的应用Application of W/O Type Emulsion Collector

步骤1:将10g电解铝碳渣加入到250mL超纯水中搅拌分散10min,使碳渣样品充分润湿,得到混合液D;Step 1: Add 10g of electrolytic aluminum carbon slag into 250mL ultrapure water and stir and disperse for 10 minutes to fully wet the carbon slag sample to obtain a mixed solution D;

步骤2:将7.9mg上述方法制得的W/O型乳液捕收剂加入到混合液D中,以1200r/min搅拌速度继续搅拌3min,得到混合液E;Step 2: Add 7.9 mg of the W/O emulsion collector prepared by the above method into the mixed solution D, and continue stirring at a stirring speed of 1200 r/min for 3 minutes to obtain the mixed solution E;

步骤3:将混合液E转移至浮选管中,向其中加入3.95mg仲辛醇作为起泡剂,以1200r/min搅拌速度持续搅拌,从浮选管底部通入空气,气体流量控制为15mL/min,浮选5min,以时间间隔为15s的速度将上浮至浮选管顶部的泡沫刮出,进行抽滤,洗涤,干燥,回收,即得碳产品,碳的浮选收率为83%;Step 3: Transfer the mixed solution E to the flotation tube, add 3.95 mg of 2-octanol as a foaming agent, keep stirring at a stirring speed of 1200 r/min, and feed air from the bottom of the flotation tube, and control the gas flow rate to 15 mL /min, flotation for 5 minutes, scrape off the foam floating to the top of the flotation tube at a time interval of 15s, perform suction filtration, wash, dry, and recover to obtain carbon products, and the flotation yield of carbon is 83% ;

步骤4:残留在浮选管中的产品进行抽滤,洗涤,干燥,回收,即得电解铝用助溶剂,助溶剂的回收率为89%。Step 4: The product remaining in the flotation tube is subjected to suction filtration, washed, dried, and recovered to obtain a co-solvent for electrolytic aluminum, and the recovery rate of the co-solvent is 89%.

以上所述实施例的各技术特征可以进行任意的组合,为使描述简洁,未对上述实施例中的各个技术特征所有可能的组合都进行描述,然而,只要这些技术特征的组合不存在矛盾,都应当认为是本说明书记载的范围。The technical features of the above-mentioned embodiments can be combined arbitrarily. To make the description concise, all possible combinations of the technical features in the above-mentioned embodiments are not described. However, as long as there is no contradiction in the combination of these technical features, should be considered as within the scope of this specification.

以上所述实施例仅表达了本发明的几种实施方式,其描述较为具体和详细,但并不能因此而理解为对发明专利范围的限制。应当指出的是,对于本领域的普通技术人员来说,在不脱离本发明构思的前提下,还可以做出若干变形和改进,这些都属于本发明的保护范围。因此,本发明专利的保护范围应以所附权利要求为准。The above-mentioned embodiments only express several implementation modes of the present invention, and the descriptions thereof are relatively specific and detailed, but should not be construed as limiting the patent scope of the invention. It should be noted that those skilled in the art can make several modifications and improvements without departing from the concept of the present invention, and these all belong to the protection scope of the present invention. Therefore, the protection scope of the patent for the present invention should be based on 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.
CN202210899277.7A 2022-07-28 2022-07-28 W/O type emulsion collector for electrolytic aluminum and preparation and application thereof Pending CN115283144A (en)

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