阅读说明：本技术 一种微纳米气泡耦合水力旋流分离脱除电石渣中杂质的方法及系统装置 (Method and system device for removing impurities in carbide slag through micro-nano bubble coupling hydrocyclone separation ) 是由 李少鹏 孟子衡 李会泉 朱干宇 李占兵 颜坤 于 2021-09-13 设计创作，主要内容包括：本发明提供一种微纳米气泡耦合水力旋流分离脱除电石渣中杂质的方法及系统装置,所述方法通过加入改性剂产生微纳米气泡,并耦合水力旋流分离,可以有效分离电石渣中的含碳、硅、铝或铁等杂质,具有杂质脱除效率高、处理量大、成本低等优势,有利于实现电石渣进一步的高值化利用；所述系统装置连接简单,操作简便,能够工业化连续运行。(The invention provides a method and a system device for removing impurities in carbide slag by micro-nano bubble coupling hydrocyclone separation, wherein micro-nano bubbles are generated by adding a modifier and are coupled with hydrocyclone separation, so that impurities containing carbon, silicon, aluminum or iron and the like in the carbide slag can be effectively separated, the method has the advantages of high impurity removal efficiency, large treatment capacity, low cost and the like, and is favorable for realizing further high-value utilization of the carbide slag; the system device is simple in connection, simple and convenient to operate and capable of achieving industrial continuous operation.)

1. A method for removing impurities in carbide slag by micro-nano bubble coupling hydrocyclone separation is characterized by comprising the following steps:

(1) mixing the carbide slag slurry with a modifier to serve as a water source, and enabling the water source and a gas source to enter a micro-nano bubble generating device to form carbide slag slurry containing micro-nano bubbles;

(2) and after the carbide slag slurry containing the micro-nano bubbles is subjected to dispersion treatment, removing impurities through hydraulic cyclone separation.

2. The method of claim 1, wherein the modifier of step (1) comprises a mixture of an organic alcohol and an adjuvant;

the auxiliary agent comprises an organic compound containing both carboxyl and phosphonic acid groups.

3. The method according to claim 2, wherein the modifier is added in the step (1) in an amount of 10-1000 g per ton of carbide slag.

4. The method according to any one of claims 1 to 3, wherein the volume flow of the air source entering the micro-nano bubble generating device in the step (1) is 5% to 15% of the volume flow of the water source entering the micro-nano bubble generating device.

5. The method according to any one of claims 1 to 3, wherein the mixing in step (1) and the dispersing in step (2) are carried out in the same vessel.

6. The method according to claim 5, wherein the ratio of the volume of the water source entering the micro-nano bubble generator per hour to the volume of the water source in the dispersion treatment is 1 (0.5-5).

7. The method according to any one of claims 1 to 3, wherein the feed pressure of the hydrocyclone in step (2) is 0.02 to 2 MPa.

8. The method according to any one of claims 1 to 3, further comprising (3): respectively carrying out re-separation treatment on the first slag slurry and the second slag slurry obtained by hydraulic cyclone separation to obtain a carbide slag slurry product and a recyclable solution, and recycling the recyclable solution to the dispersion treatment; the average particle size of the first slurry is smaller than the average particle size of the second slurry.

9. A system device for removing impurities in carbide slag through micro-nano bubble coupling hydrocyclone separation is characterized in that the system device can operate the method for removing impurities in carbide slag through micro-nano bubble coupling hydrocyclone separation according to any one of claims 1-8;

the system device comprises a micro-nano bubble generating device, a dispersion treatment device and a hydraulic cyclone separation device which are connected in sequence; the micro-nano bubble generating device is provided with an air source inlet, a water source inlet and a carbide slag slurry outlet containing micro-nano bubbles; the carbide slag slurry outlet containing micro-nano bubbles in the micro-nano bubble generating device is connected with the carbide slag slurry inlet containing micro-nano bubbles of the dispersion treatment device, and the outlet of the dispersion treatment device is connected with the hydraulic cyclone separation device.

10. The system-assembly of claim 9 wherein said water source inlet is connected to said water source outlet of said dispersion treatment device.

Technical Field

The invention relates to the technical field of resources and environment, in particular to a method and a system device for removing impurities in carbide slag by micro-nano bubble coupling hydrocyclone separation.

Background

The carbide slag is industrial solid waste formed in the acetylene production process, has large discharge amount, is mainly calcium hydroxide, has the content generally higher than 90 percent, and contains a small amount of impurities such as coke particles, ferrosilicon, aluminum-silicon minerals and the like. The carbide slag is an agglomerated particle, the impurity phase in the particle is mixed with calcium hydroxide, and for the carbide slag particle with larger particle size, the impurity phase and the calcium hydroxide are contained at the same time, so the impurity in the carbide slag is difficult to be effectively removed by simple particle size separation.

CN102091525A discloses a preparation device and a process for carbide slag desulfurization slurry from silicon iron recovery, wherein the process adopts multi-step physical screening combined with a magnetic rod group to remove silicon iron in carbide slag slurry.

CN102351232A discloses a technology for removing ferrosilicon particles in carbide slag slurry, the technology utilizes a magnetic field of 0.05-0.5T to separate ferrosilicon through carbide slag slurry melting process, reduces the content of black impurities in carbide slag desulfurized gypsum, and improves the quality of the gypsum.

CN113019714A discloses an impurity desorption system device and an impurity desorption method for carbide slag, the method utilizes the characteristics that the settling rates of coke, ferrosilicon impurity particles and other particles are different and the adhesion forces of micro-nano bubbles to different fine particles are different, combines the quick oxidation effect of the micro-nano bubbles to reducing substances, realizes the oxidation and separation coupling of impurities in the carbide slag, and is beneficial to improving the forced oxidation rate and the quality of desulfurized gypsum in the carbide slag desulfurization process.

CN103803627A discloses a method for separating and removing impurities from desulfurized gypsum slurry by a white mud/carbide slag-gypsum method, which utilizes the characteristic that gypsum particles and black suspended matters have different settling rates, and adopts a two-stage suspension stirring and settling separation device to remove the black suspended matters, thereby improving the quality of the gypsum.

CN102266715A discloses a method for producing a desulfurizer by using carbide slag, which utilizes cyclone separation to remove heavy impurities such as silicon iron and the like in dry carbide slag and utilizes sand washing sedimentation to remove large impurities and silicon iron particles in carbide slag slurry.

Although the above process method separates impurities such as ferrosilicon and black float carbon, the aluminosilicate with higher content in the carbide slag is not considered for separation and removal, which is not beneficial to further high-value utilization of the carbide slag.

Therefore, it is required to develop a process capable of separating aluminosilicate from carbide slag.

Disclosure of Invention

In view of the problems in the prior art, the invention provides a method and a system device for removing impurities in carbide slag by micro-nano bubble coupling hydrocyclone separation.

In order to achieve the purpose, the invention adopts the following technical scheme:

in a first aspect, the invention provides a method for removing impurities in carbide slag by micro-nano bubble coupled hydrocyclone separation, which comprises the following steps:

(1) mixing the carbide slag slurry with a modifier to serve as a water source, and enabling the water source and a gas source to enter a micro-nano bubble generating device to form carbide slag slurry containing micro-nano bubbles;

(2) and after the carbide slag slurry containing the micro-nano bubbles is subjected to dispersion treatment, removing impurities through hydraulic cyclone separation.

According to the method, the calcium carbide slag particles are firstly crushed and refined by a micro-nano bubble method, and meanwhile, the surface characteristics of the calcium hydroxide particles are changed by the interaction of a modifier and the calcium hydroxide particles in the calcium carbide slag, so that micro-nano bubbles can be attached to the surfaces of the calcium hydroxide particles, and then the hydrocyclone is used for cyclone separation, and the calcium hydroxide particles and particle impurities such as aluminum-silicon minerals and silicon iron can be effectively separated in a synergistic manner.

The method comprises the following specific steps: the chemical components of the carbide slag are mainly calcium hydroxide and contain a small amount of impurities such as coke particles, ferrosilicon, aluminum silicon minerals and the like. The carbide slag is an agglomerated particle, the impurity phase and the calcium hydroxide in the particle are mixed together, and for the carbide slag particle with larger particle size, the impurity and the calcium hydroxide are contained at the same time, so that the impurity in the carbide slag is difficult to be effectively removed by simple particle size classification. The micro-nano bubbles rotate and spray gas-liquid mixed fluid at high speed in the generation process to generate strong shearing and high-frequency pressure change, and when the micro-nano bubbles are broken, pressure is released instantly to form ultrahigh-speed micro jet flow and local ultrahigh temperature, so that the breaking and refining of carbide slag particles are facilitated, and the effective dispersion of impurities and calcium hydroxide is realized.

After the carbide slag particles are crushed and refined, impurities such as coke particles, ferrosilicon, aluminum silicon minerals and the like and calcium hydroxide are effectively dispersed. The coke particles in the carbide slag have low density and are easy to float on the water surface; the ferrosilicon particles are generally higher in density, and the ferrosilicon can be separated by simple gravity sedimentation; and the density of the aluminum-silicon mineral particles with higher content in the carbide slag is close to that of calcium hydroxide, so that the separation is difficult through gravity or granularity, and the separation of the aluminum-silicon mineral particles in the carbide slag is more facilitated through the hydrocyclone separation. And the micro-nano bubbles have small size and long retention time, and the surfaces of the micro-nano bubbles are negatively charged and can adsorb substances with positive electricity. The modifier is added to react with calcium hydroxide particles in carbide slag to change the hydrophilic and oleophilic characteristics of the surface of the calcium hydroxide, so that micro-nano bubbles can be attached to the surface of the calcium hydroxide particles, the hydraulic characteristics of the calcium hydroxide particles in a cyclone can be changed, and the calcium hydroxide particles can be effectively separated from aluminum silicon minerals, silicon iron and other particles.

The size of the micro-nano bubbles in the field generally refers to the size of 1 nm-1000 mu m.

Preferably, the micro-nano bubbles have a size of 100nm to 100 μm, and may be, for example, 100nm, 500nm, 1 μm, 5 μm, 10 μm, 50 μm or 100 μm, but not limited to the values listed, and other values not listed in the range are also applicable.

Preferably, the impurities of step (2) comprise an aluminum silicon mineral and/or a silicon iron compound.

Preferably, the modifier of step (1) comprises a mixture of an organic alcohol and an auxiliary. The modifier disclosed by the invention is preferably an organic alcohol-containing modifier, and can be used for modifying the surfaces of calcium hydroxide particles in the carbide slag.

Preferably, the organic alcohol includes any one of aliphatic alcohol, alicyclic alcohol or aromatic alcohol or a combination of at least two of them, wherein typical but non-limiting combinations are a combination of aliphatic alcohol and alicyclic alcohol, a combination of aromatic alcohol and alicyclic alcohol, and a combination of aliphatic alcohol and aromatic alcohol.

Preferably, the number of hydroxyl groups in the aliphatic, alicyclic or aromatic alcohol is 1 to 6, and may be 1,2, 3, 4, 5 or 6, for example.

Preferably, the auxiliary agent comprises an organic compound containing carboxyl and phosphonic acid groups, so that the modification effect is better, and the synergistic effect of later-stage hydrocyclone separation with water conservancy is stronger.

Preferably, the number of carboxyl groups in the auxiliary agent is 1-5, and for example, the number of carboxyl groups in the auxiliary agent can be 1,2, 3, 4 or 5.

Preferably, the number of phosphonic acid groups in the adjuvant is 1 to 6, and may be, for example, 1,2, 3, 4, 5 or 6.

Preferably, the molar ratio of the organic alcohol to the auxiliary in step (1) is (1-50): 1, and may be, for example, 1:1, 2:1, 5:1, 10:1, 15:1, 20:1, 30:1, 40:1, 45:1 or 50:1, but is not limited to the recited values, and other values not recited in this range are also applicable.

Preferably, the modifier is added in an amount of 10-1000 g, such as 10g, 120g, 230g, 340g, 450g, 560g, 670g, 780g, 890g or 1000g, per ton of carbide slag, but not limited to the recited values, and other values not recited in this range are also applicable.

Preferably, the gas source in step (1) comprises any one or a combination of at least two of air, oxygen, argon, helium, neon or ozone, wherein typical but non-limiting combinations are a combination of air and oxygen, a combination of argon and ozone, a combination of air and argon, a combination of helium and neon, a combination of helium and oxygen, and a combination of neon and ozone.

Preferably, the volume flow of the gas source entering the micro-nano bubble generating device accounts for 5% -15% of the volume flow of the water source entering the micro-nano bubble generating device, and may be, for example, 5%, 7%, 8%, 9%, 10%, 11%, 12%, 13%, 14%, or 15%, and the like, but is not limited to the values listed, and other values not listed in the range are also applicable.

Preferably, the mass concentration of the carbide slag slurry in the dispersion treatment in the step (2) is 5% to 25%, for example, 5%, 8%, 10%, 12%, 14%, 17%, 19%, 21%, 23%, or 25%, etc., but not limited to the recited values, and other values not recited in the range are also applicable.

Preferably, the time of the dispersion treatment is 20min to 10 hours, and for example, it may be 20min, 30min, 1h, 2h, 3h, 4h, 5h, 6h, 7h, 8h, 9h or 10h, etc., but is not limited to the values listed, and other values not listed in the range are also applicable.

Preferably, the dispersion treatment is carried out under stirring conditions.

Preferably, the stirring speed of the dispersion treatment is 50 to 300r/min, for example, 50r/min, 70r/min, 100r/min, 130r/min, 160r/min, 180r/min, 200r/min, 240r/min, 270r/min or 300r/min, etc., but is not limited to the values listed, and other values not listed in the range are also applicable.

Preferably, the temperature of the carbide slag slurry in the dispersion treatment is 20 to 70 ℃, and may be, for example, 20 ℃, 25 ℃, 30 ℃, 37 ℃, 43 ℃, 45 ℃, 50 ℃, 55 ℃, 65 ℃ or 70 ℃, but not limited to the recited values, and other values not recited in the range are also applicable.

Preferably, the mixing of step (1) and the dispersing of step (2) are carried out in the same vessel.

Preferably, the ratio of the volume of the water source entering the micro-nano bubble generator per hour to the volume of the water source in the dispersion treatment is 1 (0.5-5), and may be, for example, 1:0.5, 1:1, 1:1.5, 1:2, 1:2.5, 1:3, 1:3.5, 1:4, 1:4.5 or 1:5, but is not limited to the enumerated values, and other unrecited values in the range are also applicable.

Preferably, the feed pressure of the hydrocyclone in step (2) is 0.02 to 2MPa, and may be, for example, 0.02MPa, 0.2MPa, 0.4MPa, 0.6MPa, 0.8MPa, 1MPa, 1.2MPa, 1.4MPa, 1.6MPa, 1.8MPa or 2MPa, but is not limited to the values listed, and other values not listed in this range are equally applicable.

Preferably, the method further comprises (3): and respectively carrying out re-separation treatment on the first slag slurry and the second slag slurry obtained by the hydrocyclone separation to obtain a carbide slag slurry product and a recyclable solution, and recycling the recyclable solution to the dispersion treatment. The average particle size of the first slurry is smaller than the average particle size of the second slurry;

preferably, the re-separation process comprises: and (3) carrying out secondary separation on the first slag slurry to obtain floating slag on the upper part and obtain a carbide slag slurry product on the middle part.

Preferably, the scum is subjected to first stirring dispersion and solid-liquid separation in sequence to obtain first slag and a first solution.

Preferably, the carbide slag slurry product is subjected to solid-liquid separation to obtain refined carbide slag and a second solution.

Preferably, the re-separation process comprises: and the second slag slurry is subjected to second stirring dispersion and solid-liquid separation in sequence to obtain second slag and a third solution.

Preferably, the first solution, the second solution and the third solution are each independently circulated as a recyclable solution into the dispersion treatment.

Preferably, the solid-liquid separation comprises filtration.

As a preferable technical scheme of the invention, the method comprises the following steps:

(1) the method comprises the following steps of mixing 5-25% by mass of carbide slag slurry and a modifier consisting of organic alcohol and an auxiliary agent in a molar ratio of (1-50): 1, adding 10-1000 g of the modifier into each ton of carbide slag to serve as a water source, and enabling the water source and a gas source to enter a micro-nano bubble generating device to form the carbide slag slurry containing micro-nano bubbles; the volume flow of the air source entering the micro-nano bubble generating device accounts for 5% -15% of the volume flow of the water source entering the micro-nano bubble generating device;

(2) after the carbide slag slurry containing the micro-nano bubbles is subjected to dispersion treatment for 20 min-10 h at the stirring speed of 50-300 r/min and the temperature of 20-70 ℃, the carbide slag slurry enters a hydraulic cyclone separation device at the feeding pressure of 0.02-2 MPa for hydraulic cyclone separation, and impurities are removed; the ratio of the volume of the water source entering the micro-nano bubble generator per hour to the volume of the water source in the dispersion treatment is 1 (0.5-5); the mixing of the step (1) and the dispersion treatment of the step (2) are carried out in the same container;

(3) performing secondary separation on the first slag slurry obtained at the upper part of the hydrocyclone separation at 50-200 r/min to obtain floating slag at the upper part and obtain a carbide slag slurry product at the middle part; the scum is subjected to first stirring dispersion and solid-liquid separation in sequence to obtain first slag and a first solution; carrying out solid-liquid separation on the carbide slag slurry product to obtain refined carbide slag and a second solution;

and the second slag slurry obtained at the bottom of the hydrocyclone separation is subjected to second stirring dispersion and solid-liquid separation in sequence to obtain second slag and a third solution, and the first solution, the second solution and the third solution are used as recyclable solutions and are all recycled to the dispersion treatment.

In a second aspect, the invention provides a system device for removing impurities in carbide slag by micro-nano bubble coupled hydrocyclone separation, and the system device can operate the method for removing impurities in carbide slag by micro-nano bubble coupled hydrocyclone separation.

The system device comprises a micro-nano bubble generating device, a dispersion treatment device and a hydraulic cyclone separation device which are connected in sequence; the micro-nano bubble generating device is provided with an air source inlet, a water source inlet and a carbide slag slurry outlet containing micro-nano bubbles; the carbide slag slurry outlet containing micro-nano bubbles in the micro-nano bubble generating device is connected with the carbide slag slurry inlet containing micro-nano bubbles of the dispersion treatment device, and the outlet of the dispersion treatment device is connected with the hydraulic cyclone separation device.

Preferably, the water source inlet is connected to the water source outlet of the dispersion treatment apparatus.

Preferably, the dispersion treatment device is provided with a carbide slag slurry inlet and a modifier inlet.

Preferably, a first stirring component is arranged in the dispersion treatment device.

Preferably, the system apparatus further comprises a material conveying device arranged between the dispersion treatment device and the hydrocyclone separation device.

Preferably, the material conveying means comprises a pump.

Preferably, the system installation further comprises a reprocessing unit disposed after the hydrocyclone plant.

Preferably, the reprocessing unit comprises a first slurry processing unit and a second slurry processing unit, the first slurry processing unit is connected with the upper part of the hydrocyclone separation device, and the second slurry processing unit is connected with the bottom of the hydrocyclone separation device.

Preferably, the first slurry treatment unit comprises a secondary separation device, a first stirring and dispersing device and a first solid-liquid separation device which are connected in sequence.

Preferably, a stirring component is arranged in the secondary separation device.

Preferably, the secondary separation means comprises a secondary separation tank.

Preferably, the first stirring and dispersing device is a scum trough.

Preferably, the first slurry treatment unit further comprises a second solid-liquid separation device connected with the middle part of the secondary separation device.

Preferably, the second solid-liquid separation device separates to obtain refined carbide slag and a second solution.

Preferably, the second slurry treatment unit comprises a second stirring and dispersing device and a third solid-liquid separation device which are connected in sequence.

Preferably, the liquid phase outlets of the first solid-liquid separation device, the second solid-liquid separation device and the third solid-liquid separation device are respectively and independently connected with the dispersion treatment device.

Compared with the prior art, the invention has at least the following beneficial effects:

(1) the method for removing impurities in the carbide slag by micro-nano bubble coupling hydrocyclone separation can effectively separate impurities containing carbon, silicon, aluminum, iron and the like in the carbide slag, has high impurity removal efficiency, wherein the impurity removal rate is over 70wt%, preferably over 80%, and the obtained refined carbide slag contains Ca (OH)₂The content is more than or equal to 97wt%, preferablyMore than or equal to 98wt% under the condition, the silicon content in the refined carbide slag is less than or equal to 1.1wt%, and preferably less than or equal to 0.5wt%, and the method has the advantages of large treatment capacity, low cost and the like, and is favorable for realizing further high-value utilization of the carbide slag;

(2) the system device for separating and removing impurities in carbide slag by micro-nano bubble coupling hydrocyclone can continuously and industrially operate, and process parameters are easy to control.

Drawings

FIG. 1 is a schematic diagram of a system and an apparatus for removing impurities in carbide slag by micro-nano bubble coupled hydrocyclone separation.

In the figure: 1-micro-nano bubble generating device; 11-gas source inlet; 12-water source inlet; 13-carbide slag slurry outlet containing micro-nano bubbles; 2-a dispersion treatment device; 21-carbide slag slurry inlet; 22-modifier inlet; 23-water source outlet; 24-a carbide slag slurry inlet containing micro-nano bubbles; 3-a material conveying device; 4-a hydrocyclone separation device; 51-a secondary separation device; 52-first stirring and dispersing device; 53-a first solid-liquid separation device; 54-a second solid-liquid separation device; 61-a second stirring and dispersing device; 62-a third solid-liquid separation device.

Detailed Description

The technical scheme of the invention is further explained by the specific implementation mode in combination with the attached drawings.

The present invention is described in further detail below. The following examples are merely illustrative of the present invention and do not represent or limit the scope of the claims, which are defined by the claims.

It is to be understood that in the description of the present invention, the terms "center", "longitudinal", "lateral", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", etc., indicate orientations or positional relationships based on those shown in the drawings, and are used only for convenience in describing the present invention and for simplicity in description, and do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be taken as limiting the present invention. Furthermore, the terms "first", "second", etc. are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first," "second," etc. may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless otherwise specified.

It should be noted that, in the description of the present invention, unless otherwise explicitly specified or limited, the terms "disposed," "connected" and "connected" are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meaning of the above terms in the present invention can be understood by those of ordinary skill in the art through specific situations.

It should be understood by those skilled in the art that the present invention necessarily includes necessary piping, conventional valves and general pump equipment for achieving the complete process, but the above contents do not belong to the main inventive points of the present invention, and those skilled in the art can select the layout of the additional equipment based on the process flow and the equipment structure, and the present invention is not particularly limited to this.

As a specific embodiment in the present invention, a system device for removing impurities from carbide slag by micro-nano bubble-coupled hydrocyclone separation is provided, as shown in fig. 1, the system device includes a micro-nano bubble generating device 1, a dispersion processing device 2, and a hydrocyclone separation device 4, which are connected in sequence; the micro-nano bubble generating device 1 is provided with an air source inlet 11, a water source inlet 12 and a carbide slag slurry outlet 13 containing micro-nano bubbles; the carbide slag slurry outlet 13 containing micro-nano bubbles in the micro-nano bubble generating device 1 is connected with the carbide slag slurry inlet 24 containing micro-nano bubbles of the dispersion treatment device, and the outlet of the dispersion treatment device 2 is connected with the hydraulic cyclone separation device 4.

The water source inlet 12 is connected to the water source outlet 23 of the dispersion treatment apparatus. The dispersion treatment device 2 is provided with a carbide slag slurry inlet 21 and a modifier inlet 22. A first stirring component is arranged in the dispersion treatment device 2.

The system arrangement also comprises a material conveying device 3 arranged between the dispersion treatment device 2 and the hydrocyclone separation device 4. The material conveying device 3 comprises a pump.

The system arrangement also comprises a reprocessing unit arranged after the hydrocyclone 4. The reprocessing unit comprises a first slurry processing unit and a second slurry processing unit.

The first slag slurry processing unit is connected with the upper part of the hydrocyclone separation device 4, and the second slag slurry processing unit is connected with the bottom of the hydrocyclone separation device 4. The first slurry treatment unit comprises a secondary separation device 51, a first stirring and dispersing device 52 and a first solid-liquid separation device 53 which are connected in sequence. A stirring member is provided in the secondary separation device 51. The secondary separating device 51 includes a secondary separating tank. The first stirring and dispersing device 52 is a scum trough. The first slurry treatment unit further comprises a second solid-liquid separation device 54 connected to the middle part of the secondary separation device 51.

The second slag slurry treatment unit comprises a second stirring and dispersing device 61 and a third solid-liquid separation device 62 which are connected in sequence. The liquid phase outlets of the first solid-liquid separation device 53, the second solid-liquid separation device 54, and the third solid-liquid separation device 62 are each independently connected to the dispersion treatment apparatus 2.

Specifically, the present invention is not limited to the type of the stirring and dispersing device, and any stirring and dispersing device known to those skilled in the art may be used, for example, a stirring and dispersing tank capable of achieving stirring and suspension separation; the type and structure of the solid-liquid separation apparatus are not particularly limited in the present invention, and any apparatus known to those skilled in the art that can be used for solid-liquid separation may be used, and a filtration apparatus is preferred in this embodiment.

As another specific embodiment in the present invention, a method for removing impurities from carbide slag by micro-nano bubble-coupled hydrocyclone separation is provided, which comprises the following steps:

(1) adding 10-1000 g of modifier into each ton of carbide slag according to the molar ratio of 5-25% of carbide slag slurry to a modifier consisting of organic alcohol and an auxiliary agent in a proportion of 1-50: 1, mixing the modifier in a dispersion treatment device to serve as a water source, and allowing the water source and a gas source to enter a micro-nano bubble generation device to form the carbide slag slurry containing micro-nano bubbles; the air source of the micro-nano bubble generating device is air, and the volume flow of the air source entering the micro-nano bubble generating device accounts for 5% -15% of the volume flow of the water source entering the micro-nano bubble generating device;

(2) the carbide slag slurry containing the micro-nano bubbles returns to the dispersion treatment device, after dispersion treatment is carried out on the carbide slag slurry containing the micro-nano bubbles in the dispersion treatment device for 20min to 10h at a stirring speed of 50 to 300r/min and a temperature of 20 to 70 ℃ through a spray head on the side face of the dispersion treatment device, the carbide slag slurry enters a hydraulic cyclone separation device for hydraulic cyclone separation at a feeding pressure of 0.02 to 2MPa through a carbide slag slurry pump, and impurities are removed; the ratio of the volume of the water source entering the micro-nano bubble generator per hour to the volume of the water source in the dispersion treatment is 1: 3;

(3) introducing the first slag slurry obtained by the overflow of the upper part of the hydrocyclone separation into a secondary separation device, and carrying out secondary separation and impurity removal at 50-200 r/min to obtain floating slag at the upper part and obtain a carbide slag slurry product at the middle part;

the scum enters a scum groove, and enters a first solid-liquid separation device for solid-liquid separation after being subjected to first stirring dispersion to obtain first slag and first solution; the carbide slag slurry product enters a second solid-liquid separation device to be subjected to solid-liquid separation, so that refined carbide slag and a second solution are obtained;

and the second slag slurry obtained at the bottom of the hydrocyclone separation enters a second stirring and dispersing device, is subjected to second stirring and dispersing, and then enters a third solid-liquid separation device for solid-liquid separation to obtain second slag and a third solution, and the first solution, the second solution and the third solution are used as recyclable solutions and are circulated to a dispersion treatment tank for dispersion treatment.

Example 1

The embodiment provides a system device for removing impurities in carbide slag by micro-nano bubble coupling hydrocyclone separation, which comprises a micro-nano bubble generating device, a dispersion treatment device and a hydrocyclone separation device which are sequentially connected; the micro-nano bubble generating device is provided with an air source inlet, a water source inlet and a carbide slag slurry outlet containing micro-nano bubbles; the carbide slag slurry outlet containing micro-nano bubbles in the micro-nano bubble generating device is connected with the carbide slag slurry inlet containing micro-nano bubbles of the dispersion treatment device, and the outlet of the dispersion treatment device is connected with the hydraulic cyclone separation device.

The water source inlet is connected with the water source outlet of the dispersion treatment device. The dispersion treatment device is provided with a carbide slag slurry inlet and a modifier inlet. A first stirring component is arranged in the dispersion treatment device. The dispersion treatment device is a dispersion treatment tank.

The system device also comprises a material conveying device arranged between the dispersion treatment device and the hydrocyclone separation device. The material conveying device comprises a carbide slurry pump.

The system arrangement further comprises a reprocessing unit arranged after the hydrocyclone unit. The reprocessing unit comprises a first slurry processing unit and a second slurry processing unit.

The first slag slurry processing unit is connected with the upper part of the hydrocyclone separation device, and the second slag slurry processing unit is connected with the bottom of the hydrocyclone separation device. The first slurry treatment unit comprises a secondary separation device, a first stirring and dispersing device and a first solid-liquid separation device which are sequentially connected. And a stirring component is arranged in the secondary separation device. The secondary separation device comprises a secondary separation tank. The first stirring and dispersing device is a scum tank. The first solid-liquid separation device is a first filtering device. The first slurry treatment unit also comprises a second solid-liquid separation device connected with the middle part of the secondary separation device. The second solid-liquid separation device is a second filtering device.

The second slag slurry treatment unit comprises a second stirring and dispersing device and a third solid-liquid separation device which are sequentially connected. The second stirring and dispersing device is a coarse slag groove, a stirring component is arranged in the second stirring and dispersing device, and the third solid-liquid separation device is a third solid-liquid separation device.

And liquid phase outlets of the first solid-liquid separation device, the second solid-liquid separation device and the third solid-liquid separation device are respectively and independently connected with the dispersion treatment device.

Application example 1

The application example provides a method for removing impurities in carbide slag by micro-nano bubble coupling hydrocyclone separation, which is carried out by adopting the device provided by the embodiment 1, and specifically comprises the following steps:

(1) adding 600g of modifier into each ton of carbide slag according to a molar ratio of 1, 2-butanediol to 1:1 and a modifier consisting of an auxiliary agent (an organic compound containing 1 carboxyl group, 1 phosphonic acid group and 6 carbon alkyl groups, diethyl phosphoacetic acid and produced from alatin) in a dispersion treatment tank, mixing the modifier and the carbide slag to form a water source, and allowing the water source and a gas source to enter a micro-nano bubble generating device to form carbide slag slurry containing micro-nano bubbles of 100 nm-100 mu m; the air source of the micro-nano bubble generating device is air, and the volume flow of the air source entering the micro-nano bubble generating device accounts for 8% of the volume flow of the water source entering the micro-nano bubble generating device;

(2) the carbide slag slurry containing the micro-nano bubbles returns to the dispersion treatment tank, after the carbide slag slurry containing the micro-nano bubbles in the dispersion treatment tank is subjected to dispersion treatment for 6 hours at a stirring speed of 200r/min and a temperature of 50 ℃ by a spray head on the side surface of the dispersion treatment tank, the carbide slag slurry enters a hydraulic cyclone separation device at a feeding pressure of 1.5MPa for hydraulic cyclone separation, and impurities are removed; the ratio of the volume of the water source entering the micro-nano bubble generator per hour to the volume of the water source in the dispersion treatment is 1: 3;

(3) introducing the first slag slurry obtained by the overflow of the upper part of the hydrocyclone separation into a secondary separation tank, and carrying out secondary separation and impurity removal at 150r/min to obtain floating slag at the upper part and obtain a carbide slag slurry product at the middle part;

the scum enters a scum groove, and enters a first filtering device for filtering after being subjected to first stirring and dispersing to obtain first slag and first solution; the carbide slag slurry product enters a second filtering device and is filtered to obtain refined carbide slag and a second solution;

and the second slag slurry obtained at the bottom of the hydrocyclone separation enters a coarse slag tank, is subjected to second stirring and dispersion, and then enters a third filtering device for filtering to obtain second slag and a third solution, and the first solution, the second solution and the third solution are used as recyclable solutions and are circulated to a dispersion treatment tank for dispersion treatment.

Application example 2

The application example provides a method for removing impurities in carbide slag by micro-nano bubble coupling hydrocyclone separation, which is carried out by adopting the device provided by the embodiment 1, and specifically comprises the following steps:

(1) adding 1000g of modifier into each ton of carbide slag according to a molar ratio of 1:1, and mixing the modifier with 1:1 of 1,3, 5-trihydroxycyclohexane and an additive (an organic compound containing 1 carboxyl group, 1 phosphonic acid group and 4 carbon alkyl groups, 4-phosphobutyric acid and produced from alatin) in a dispersion treatment tank to serve as a water source, wherein the water source and a gas source enter a micro-nano bubble generation device to form carbide slag slurry containing micro-nano bubbles of 100 nm-80 mu m; the air source of the micro-nano bubble generating device is oxygen with volume fraction of 80%, 20% of nitrogen is balance gas, and the volume flow of the air source entering the micro-nano bubble generating device accounts for 15% of the volume flow of the water source entering the micro-nano bubble generating device;

(2) the carbide slag slurry containing the micro-nano bubbles returns to the dispersion treatment tank, after the carbide slag slurry containing the micro-nano bubbles in the dispersion treatment tank is subjected to dispersion treatment for 20min at the stirring speed of 300r/min and the temperature of 20 ℃, the carbide slag slurry enters a hydraulic cyclone separation device for hydraulic cyclone separation at the feeding pressure of 0.2MPa through a carbide slag slurry pump, and impurities are removed; the ratio of the volume of the water source entering the micro-nano bubble generator per hour to the volume of the water source in the dispersion treatment is 1: 5;

(3) introducing the first slag slurry obtained by the overflow of the upper part of the hydrocyclone separation into a secondary separation tank, and carrying out secondary separation and impurity removal at 50r/min to obtain floating slag at the upper part and obtain a carbide slag slurry product at the middle part;

the scum enters a scum groove, and enters a first filtering device for filtering after being subjected to first stirring and dispersing to obtain first slag and first solution; the carbide slag slurry product enters a second filtering device and is filtered to obtain refined carbide slag and a second solution;

and the second slag slurry obtained at the bottom of the hydrocyclone separation enters a coarse slag tank, is subjected to second stirring and dispersion, and then enters a third filtering device for filtering to obtain second slag and a third solution, and the first solution, the second solution and the third solution are used as recyclable solutions and are circulated to a dispersion treatment tank for dispersion treatment.

Application example 3

The application example provides a method for removing impurities in carbide slag by micro-nano bubble coupling hydrocyclone separation, which is carried out by adopting the device provided by the embodiment 1, and specifically comprises the following steps:

(1) adding 10g of modifier into each ton of carbide slag according to a molar ratio of 50:1, mixing the modifier and the carbide slag to form a modifier consisting of 2-diethylphenol and an auxiliary agent (an organic compound containing 1 carboxyl group, 1 phosphonic acid group and 3 carbon alkyl groups, 3-phosphonic acid propionic acid and produced from Michelin), wherein the modifier is used as a water source, and the water source and a gas source enter a micro-nano bubble generating device to form the carbide slag containing micro-nano bubbles of 300 nm-100 mu m; the air source of the micro-nano bubble generating device is ammonia with the volume fraction of 5%, helium is balance gas, and the volume flow of the air source entering the micro-nano bubble generating device accounts for 5% of the volume flow of the water source entering the micro-nano bubble generating device;

(2) the carbide slag slurry containing the micro-nano bubbles returns to the dispersion treatment tank, after the carbide slag slurry containing the micro-nano bubbles in the dispersion treatment tank is subjected to dispersion treatment for 10 hours at a stirring speed of 50r/min and a temperature of 70 ℃ by a spray head on the side surface of the dispersion treatment tank, the carbide slag slurry enters a hydraulic cyclone separation device at a feeding pressure of 2MPa to perform hydraulic cyclone separation, and impurities are removed; the ratio of the volume of the water source entering the micro-nano bubble generator per hour to the volume of the water source in the dispersion treatment is 1: 0.5;

(3) introducing the first slag slurry obtained by the overflow of the upper part of the hydrocyclone separation into a secondary separation tank, and removing impurities by secondary separation at 200r/min to obtain floating slag at the upper part and carbide slag slurry products at the middle part;

the scum enters a scum groove, and enters a first filtering device for filtering after being subjected to first stirring and dispersing to obtain first slag and first solution; the carbide slag slurry product enters a second filtering device and is filtered to obtain refined carbide slag and a second solution;

and the second slag slurry obtained at the bottom of the hydrocyclone separation enters a coarse slag tank, is subjected to second stirring and dispersion, and then enters a third filtering device for filtering to obtain second slag and a third solution, and the first solution, the second solution and the third solution are used as recyclable solutions and are circulated to a dispersion treatment tank for dispersion treatment.

Application example 4

The conditions were the same as in example 1 except that the molar ratio of 1, 2-butanediol to the auxiliary in the modifier was 100: 1.

Comparative example 1

And (3) blowing air with the same flow rate as that in the example 1 into bubbles with the diameter of 1-10 mm to disperse the carbide slag slurry and the modifier in the dispersion tank, wherein the other conditions are the same as those in the example 1.

Comparative example 2

The conditions were the same as in example 1 except that no modifier was added.

Comparative example 3

The conditions were the same as in example 1 except that no hydrocyclone separation was performed, specifically: and (3) allowing the carbide slag slurry containing the micro-nano bubbles to enter a separation tank for stirring, suspending and separating, overflowing the upper part to obtain a first slag slurry, and obtaining a second slag slurry at the bottom.

The refined carbide slag obtained in examples 1 to 4 and comparative examples 1 to 3 was subjected to sampling test, and the test results are shown in table 1.

TABLE 1

	Ca (OH) in refined calcium carbide slag2Content (wt.)	Total rate of removal of impurities	Content of silicon dioxide in refined carbide slag
				Application example 1	99.4wt%	93.7%	0.21wt%
Application example 2	98.4wt%	83.2%	0.44wt%
				Application example 3	98.9wt%	88.4%	0.37wt%
Application example 4	97.5wt%	73.7%	1.05wt%
				Comparative example 1	93.5wt%	31.6%	1.73wt%
Comparative example 2	92.5wt%	21.1%	1.88wt%
				Comparative example 3	92.1wt%	17.0%	1.71wt%

From table 1, the following points can be seen:

(1) according to the comprehensive application examples 1-3, the method for removing impurities in carbide slag by micro-nano bubble coupling hydrocyclone separation has the advantage of high impurity removal efficiency, the total impurity removal rate is over 70 percent, the total impurity removal rate is over 80 percent under the optimal condition, and Ca (OH) in the obtained refined carbide slag₂The content is more than or equal to 97wt%, preferably more than or equal to 98wt%, and the silicon content in the refined carbide slag is less than or equal to 1.1wt%, preferably less than or equal to 0.5 wt%;

(2) it can be seen from the comprehensive application example 1 and the comparative examples 1 to 3 that the technical scheme of combining the modifier, the micro-nano bubbles and the hydrocyclone separation is adopted in the application example 1, and compared with the technical scheme that the micro-nano bubbles, the modifier and the hydrocyclone separation are not adopted in the comparative examples 1 to 3, the total impurity removal rate in the application example 1 is 93.7%, and Ca (OH) in the refined carbide slag is₂The content of the impurities is 99.4wt%, while the total removal rates of the impurities in comparative examples 1 to 3 are only 31.6%, 21.1% and 17.0%, respectively, and Ca (OH) in the refined carbide slag₂The contents of the modifier, the micro-nano bubbles and the hydraulic cyclone separation are 93.5wt%, 92.5wt% and 92.1wt%, respectively, so that the deep removal of impurities in the carbide slag is realized synergistically through the combination of the modifier, the micro-nano bubbles and the hydraulic cyclone separation, and the utilization value of a final product is improved;

(3) it can be seen from the comprehensive application examples 1 and 4 that the modifier composed of 1, 2-butanediol and the auxiliary agent in a molar ratio of 10:1 in application example 1 has a total impurity removal rate of 93.7% in application example 1 and Ca (OH) in the refined carbide slag compared with the modifier composed of 1, 2-butanediol and the auxiliary agent in a molar ratio of 100:1 in application example 4₂99.4wt% of refined calcium carbideThe content of silicon dioxide in the slag is only 0.21wt%, while the total impurity removal rate in application example 4 is only 73.7%, and Ca (OH) in the refined carbide slag₂The content is only 97.5wt%, and the content of silicon dioxide in the refined carbide slag is 1.05wt%, thereby showing that the invention synergistically improves the removal effect of impurities such as silicon by further optimizing the modifier with a specific molar ratio.

In conclusion, the method for removing impurities in carbide slag by micro-nano bubble coupled hydrocyclone separation can effectively separate impurities containing carbon, silicon, aluminum or iron and the like in the carbide slag, has the advantage of high impurity removal efficiency, and has the advantages of continuous industrial operation and easily controlled process parameters.

The applicant declares that the present invention illustrates the detailed structural features of the present invention through the above embodiments, but the present invention is not limited to the above detailed structural features, that is, it does not mean that the present invention must be implemented depending on the above detailed structural features. It should be understood by those skilled in the art that any modifications of the present invention, equivalent substitutions of selected components of the present invention, additions of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.