CN115611285A - Slurry and preparation method and equipment thereof - Google Patents
Slurry and preparation method and equipment thereof Download PDFInfo
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- CN115611285A CN115611285A CN202211266392.7A CN202211266392A CN115611285A CN 115611285 A CN115611285 A CN 115611285A CN 202211266392 A CN202211266392 A CN 202211266392A CN 115611285 A CN115611285 A CN 115611285A
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- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The application provides a slurry and a preparation method and equipment thereof, belonging to the technical field of carbon black dispersion. The slurry comprises carbon black, a dispersing agent and a solvent, and the reduction rate of the compression oil absorption value of the carbon black in the slurry is less than or equal to 6.67 percent. According to the application, the carbon black is firstly dispersed to obtain the slurry, the slurry has better dispersibility when being applied compared with the single carbon black, the application difficulty is reduced, and the carbon black is firstly prepared into the slurry to be beneficial to the carbon black to construct an electric and heat conducting network. Meanwhile, the destruction rate of the primary structure body of the carbon black in the slurry is low, the slurry has high electric conductivity, heat conductivity and adsorption efficiency after being applied, and the application addition amount can be reduced.
Description
Technical Field
The application relates to the technical field of carbon black dispersion, in particular to slurry and a preparation method and equipment thereof.
Background
The carbon black can be used as a high-quality conductive additive to be generally applied to industries such as various rubbers, plastics, dry batteries, lead-acid batteries, microwave absorption, secondary lithium batteries and the like. Although the addition proportion is not high (1% -10%), the composite material can play a very key role in electric conduction, heat conduction and adsorption of functional solvent (electrolyte adsorption performance) in application.
Carbon black having a high specific surface area (BET) has high electrical conductivity, thermal conductivity and adsorption efficiency, and its addition ratio is low.
However, carbon blacks having a high specific surface area (BET) have poor dispersibility.
Disclosure of Invention
The application provides a slurry, a preparation method and equipment thereof, which have better dispersibility and lower destruction rate of a primary structure of carbon black.
The embodiment of the application is realized as follows:
in a first aspect, the present application illustratively provides a slurry comprising carbon black, a dispersant, and a solvent, wherein the carbon black in the slurry has a compressed oil absorption value (CDBP) reduction of 6.67% or less.
In the technical scheme, the carbon black is firstly dispersed to obtain the slurry, the slurry has better dispersibility compared with the single carbon black in application, the application difficulty is reduced, and the carbon black is firstly prepared into the slurry to be beneficial to the carbon black to construct the electric and heat conducting network. Meanwhile, the destruction rate of the primary structure body of the carbon black in the slurry is low, the slurry has high electrical conductivity, thermal conductivity and adsorption efficiency after being applied, and the application addition amount can be reduced.
In a first possible example of the first aspect of the present application in combination with the first aspect, the rate of change in specific surface area of carbon black in the slurry is 5% or less.
In a second possible example of the first aspect of the present application in combination with the first aspect, the D50 of the slurry is between 0.3 μm and 0.7 μm.
In a third possible example of the first aspect of the present application in combination with the first aspect, the slurry has a storage modulus G' greater than a loss modulus G "below a shear stress of 3 Pa.
In the above examples, it is shown that the slurry has a high stability in a static state.
In a fourth possible example of the first aspect of the present application in combination with the first aspect, the slurry is at 10s -1 Fixed shear rate and slurry viscosity range ofUnder the condition of 500mpa.s-3000mpa.s, the change rate of the viscosity of the slurry within-5-50 ℃ is less than or equal to 30 percent.
In the above examples, it is shown that the viscosity of the slurry has a small change in viscosity between-5 ℃ and 50 ℃, i.e. the viscosity of the slurry does not substantially affect its application.
In a fifth possible example of the first aspect of the present application in combination with the first aspect, the above slurry includes 10wt% to 30wt% of carbon black, and the dispersant is used in an amount of 4wt% to 8wt% of the carbon black.
Optionally, the dispersant is resin, the viscosity average molecular weight of the resin is more than or equal to 100 ten thousand, and the dispersant comprises polyvinylpyrrolidone.
Alternatively, the solvent comprises water or N-methylpyrrolidone.
In the above examples, the amount of dispersant used in the slurry of the present application is low.
The resin with the viscosity average molecular weight of more than 100 ten thousand is used as the dispersing agent, so that the stability of the slurry at room temperature can be improved, namely the slurry can not generate precipitation after being stored at room temperature for a long time.
In a sixth possible example of the first aspect of the present application in combination with the first aspect, the total magnetic substance content in the above slurry is < 1000ppb.
In a seventh possible example of the first aspect of the present application in combination with the first aspect, fe.ltoreq.10ppm and Ni.ltoreq.5 ppm in the above slurry.
In a second aspect, the present application provides a method for preparing the above slurry, comprising: and (3) sequentially performing ultrasonic dispersion and homogeneous dispersion on the primary slurry to prepare slurry, wherein the primary slurry is prepared by mixing a dispersing agent, a solvent and carbon black.
In the technical scheme, the ultrasonic dispersion can improve the flowability of the material in a short time, the homogeneous dispersion can further refine the slurry, and the destruction rate of the primary structure of the carbon black is low due to the ultrasonic dispersion and the homogeneous dispersion, so that the slurry has good dispersibility, and simultaneously has high electrical conductivity, thermal conductivity and adsorption efficiency after the slurry is applied, and the application addition amount can be reduced.
In a first possible example of the second aspect of the present application in combination with the second aspect, the power of the ultrasonic dispersion is 5kW to 20kW.
Optionally, the frequency of ultrasonic dispersion is 15kHz to 30kHz.
In a second possible example of the second aspect of the present application, in combination with the second aspect, a method of preparing a virgin slurry includes:
the dispersant is first mixed with a portion of the solvent to swell the dispersant to produce a first mixture, and the first mixture, carbon black and the remaining solvent are then mixed to produce a preliminary slurry.
Optionally, before mixing the dispersing agent and part of the solvent, heating the solvent to 50-70 ℃, adding the dispersing agent after the temperature of the solvent reaches the target temperature, and swelling for 6-8 h under a stirring state.
Optionally, the dispersant is dosed at a solids content of 25% to 35%.
Optionally, the stirring rate during the swelling process is 30r/min to 60r/min.
Alternatively, the swelling process is performed under vacuum conditions.
Optionally, after the first mixture is prepared, the first mixture and the rest of the solvent are mixed and stirred for 5min to 20min to prepare a second mixture, and then the second mixture is mixed with carbon black and emulsified for 20min to 40min to prepare the primary slurry.
In the above example, mixing the dispersant and a portion of the solvent first enables the dispersant to achieve better swelling, reducing the effect of the dispersant on the viscosity of the slurry. Then other raw materials are added to obtain a primary slurry.
The dispersant with the viscosity average molecular weight of more than 100 ten thousand is difficult to swell in the solvent, and the solvent is heated to the target temperature, so that the swelling of the dispersant is facilitated.
The materials are fed step by step, so that the materials can not be fully soaked, and the formation of large gel blocks is avoided or reduced.
With reference to the second aspect, in a third possible example of the second aspect of the present application, after the slurry is prepared, the slurry is subjected to a desmear process.
In the above example, the impurity removal can remove most of the impurities in the slurry, so that the total magnetic substances and metal elements in the slurry are substantially removed.
In a third aspect, the present application provides an apparatus for carrying out the above-described method for preparing a slurry, comprising: first compounding subassembly, second compounding subassembly, supersound dispersion module and isotropic symmetry.
First compounding subassembly has first feed inlet and first discharge gate.
The second mixing component comprises a second mixing tank and an emulsifying machine, the second mixing tank is provided with a second feed port, a third feed port, a second discharge port and a third discharge port, the second feed port is connected to the first discharge port, the emulsifying machine is provided with a fourth feed port and a fourth discharge port, the fourth feed port is connected to the third discharge port, and the fourth discharge port is connected to the third feed port.
The ultrasonic dispersion module is provided with a fifth feed inlet and a fifth discharge outlet, and the fifth feed inlet is connected to the second discharge outlet.
The homogenizer is provided with a sixth feeding hole and a sixth discharging hole, and the sixth feeding hole is connected with the fifth discharging hole.
In the technical scheme, the equipment can be used for preparing slurry.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings that are required to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present application and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained from the drawings without inventive effort.
FIG. 1 is a schematic structural diagram of an apparatus according to an embodiment of the present application;
FIG. 2 is an amplitude scan of example 1 of the present application;
fig. 3 is an amplitude scan of comparative example 2 of the present application.
Icon: 10-equipment; 100-a first compounding assembly; 110-a first stirred tank; 111-a first tank; 1111-a first feed port; 1112-a first discharge port; 112-a first stirrer; 120-vacuum pump; 130-a heater; 140-heating the pipe; 200-a second compounding assembly; 210-a second stirred tank; 211-a second tank; 2111-a second feed port; 2112-second discharge port; 2113-a third feed port; 2114-a third discharge port; 212-a second agitator; 213-first jacket structure; 220-an emulsifying machine; 221-a fourth feed port; 222-a fourth discharge port; 300-an ultrasonic dispersion module; 301-fifth feed port; 302-fifth discharge port; 310-a first ultrasound module; 320-a second ultrasound module; 330-a third ultrasound module; 400-a homogenizer; 401-sixth feed inlet; 402-a sixth discharge port; 510-a first pump; 520-a second pump; 530-cooling water; a 600-200 mesh filter screen; 700-demagnetizer; 701-a seventh feed inlet; 702-a seventh discharge port; 800-finished product tank; 801-eighth feed inlet; 802-eighth discharge port; 810-second jacket construction.
Detailed Description
Embodiments of the present application will be described in detail below with reference to examples, but those skilled in the art will appreciate that the following examples are only illustrative of the present application and should not be construed as limiting the scope of the present application. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The carbon black can be used as a high-quality conductive additive to be generally applied to industries such as various rubbers, plastics, dry batteries, lead-acid batteries, microwave absorption, secondary lithium batteries and the like. Although the addition proportion is not high (1% -10%), the composite material can play a very key role in electric conduction, heat conduction and adsorption of functional solvent (electrolyte adsorption performance) in application.
With the development requirements of the energy field and the new material process, on one hand, the electrical conductivity, the thermal conductivity and the adsorption efficiency performance of the carbon black in the application need to be improved; on the other hand, the adding proportion of the carbon black in the application needs to be reduced.
The inventors have found through studies that carbon blacks having high specific surface areas (BET) can meet the above requirements. The specific surface area (BET) of the carbon black is in m 2 Increased BET, in terms of/g, means that the carbon black is better at the same massThe large external surface area is used for electric conduction, heat conduction and adsorption. And theoretically the larger the BET, the smaller the primary particles of the material and the greater the number of primary particles. Under the condition that the BET is increased by one time and the mass is the same, the number of the carbon black particles is increased by about eight times, so that a richer conductive network can be constructed under the condition that a small amount of carbon black is added. However, as BET increases, greater application difficulties arise. Carbon black is a nanoscale material, and the BET increases, and carbon particles become smaller and larger with the same mass, and the intermolecular force of carbon black increases. In the mixing process of application, the dispersion degree of difficulty of carbon black also can exponentially increase, and in the mixing process, if the carbon black can not be uniformly dispersed, the problems of local heating, inconsistent electrical property and the like can be caused in the electric conduction and heat conduction processes. Therefore, the solution of the dispersion problem of the high BET carbon black is the root cause for reducing the application bottleneck of the material and improving the material performance.
Because the carbon black is a nanoscale three-dimensional branched chain structure, under the influence of intermolecular force, a plurality of carbon black structures (primary structures) can be entangled into a micron-sized (10-30 mu m) aggregate (secondary structure), the dispersion enables the opening of the carbon black secondary structure, and the carbon black presents better electrical conductivity, thermal conductivity and adsorption efficiency, but if the carbon black is excessively dispersed, the carbon black can be smashed, and the carbon black can completely lose adsorption capacity.
The inventor finds that the carbon black is dispersed to obtain the slurry, the slurry has better dispersibility compared with the single carbon black in application, the application difficulty is reduced, and the carbon black is prepared into the slurry to be beneficial to the carbon black to construct the electric and heat conducting network. Meanwhile, the destruction rate of the primary structure body of the carbon black in the slurry is low, the slurry has high electrical conductivity, thermal conductivity and adsorption efficiency after being applied, and the application addition amount can be reduced.
The following specifically describes a slurry, a preparation method thereof, and equipment in the embodiments of the present application:
a slurry is provided that includes carbon black, a dispersant, and a solvent.
Alternatively, the carbon black may be acetylene or other carbon black.
The dispersant comprises resin, and the viscosity average molecular weight of the resin is more than or equal to 100 ten thousand.
Optionally, the dispersant is polyvinylpyrrolidone having a viscosity average molecular weight of 100 to 150 million.
The solvent includes water or N-methylpyrrolidone.
Optionally, the slurry comprises 10wt% to 30wt% of carbon black, the amount of the dispersant is 4wt% to 8wt% of the carbon black, and the balance is the solvent.
Compared with the dispersant in other slurry with the amount of 10-100 wt% of the carbon black, the dispersant in the slurry has a lower amount, so that the addition amount of the carbon black is increased, and the electrical conductivity, the thermal conductivity and the adsorption efficiency of the carbon black are further increased.
Optionally, the slurry comprises 10wt% to 30wt% of carbon black, the amount of the dispersant is 4wt% to 7wt% of the carbon black, and the balance is the solvent.
The reduction rate of the compression oil absorption value (CDBP) of the carbon black in the slurry is less than or equal to 6.67 percent.
The CDBP reduction rate of carbon black in the slurry = (CDBP of carbon black raw material — CDBP of carbon black in slurry)/CDBP of carbon black raw material 100%.
The CDBP of the carbon black feedstock was tested according to the method of GB/T3780.4-2017.
The testing method of the slurry needs to dry the slurry at 150 ℃ until the weight of the slurry is not reduced, and then the testing is carried out according to the method of GB T3780.4.
Optionally, the carbon black in the slurry has a CDBP reduction of 10% or less.
The BET change rate of the carbon black in the slurry is less than or equal to 5 percent.
BET change rate of carbon black in slurry = (BET of carbon black in slurry-BET of carbon black feedstock)/BET of carbon black feedstock 100%.
The BET of the carbon black feedstock was tested according to the method of GB/T19587-2004.
The testing method of the slurry needs to carry out pretreatment on the slurry, and the pretreatment method comprises the following steps:
s1, centrifuging the slurry to be detected for 10min at a rotating speed of 3000r/min by using a centrifuge;
s2, removing the supernatant of the centrifuged slurry, adding absolute ethyl alcohol with the same amount as the supernatant, and stirring for 5min by using a glass rod until the mixture is uniformly mixed;
s3, centrifuging again for 10min at the rotating speed of 3000r/min by using the centrifuge;
s4, repeating the step S2 and the step S3 twice;
s5, drying for 30min at 150 ℃ by using a hot air oven until the weight of the material is not reduced;
and S6, testing according to the BET testing method of the powder carbon black to obtain the BET of the carbon black in the slurry.
The median particle diameter (D50) of the slurry was 0.3 to 0.7. Mu.m.
When the D50 of the slurry is less than 0.3 mu m, the primary structure of the carbon black is destroyed; when the D50 of the slurry is > 0.7 μm, the carbon black is not completely dispersed from the secondary structure; when the D50 of the slurry is 0.3-0.7 μm, the secondary structure of the carbon black is just opened without damaging the primary structure of the carbon black, so that the slurry has higher electrical conductivity, thermal conductivity and adsorption efficiency after application, and the application addition amount can be reduced.
By way of example, when the carbon black is acetylene black, the D50 of the slurry may be 0.30 μm, 0.43 μm, 0.55 μm, 0.61 μm, or 0.70 μm.
The storage modulus G 'of the slurry is larger than the loss modulus G' below the shear stress of 3Pa, which indicates that the slurry has higher stability in a static state.
The slurry is in 10s -1 The change rate of the viscosity of the slurry within 5 ℃ below zero to 50 ℃ is less than or equal to 30 percent under the conditions of the fixed shear rate and the viscosity range of the slurry being 500mpa.s to 3000mpa.s, which indicates that the viscosity change of the slurry at 5 ℃ below zero to 50 ℃ is small, namely the viscosity of the slurry does not basically influence the application of the slurry.
The total content of magnetic substances in the slurry is less than 1000ppb, fe is less than or equal to 10ppm, and Ni is less than or equal to 5ppm.
When the solvent is N-methyl pyrrolidone, the water content in the slurry is less than 1500ppm.
The slurry of the present application contains fewer impurities.
The application also provides a preparation method of the slurry, which comprises the following steps:
s1, pretreatment of a dispersing agent
Feeding partial solvent, heating the solvent to 50-70 ℃, adding the dispersing agent into the solvent after the temperature of the solvent reaches the target temperature, vacuumizing, and swelling for 6-8 h under low-speed stirring.
The larger the molecular weight of the dispersant is, the more difficult the dispersant is to swell, which causes the viscosity of the slurry to be higher, and the prepared slurry cannot be used. But the high molecular weight dispersant also has the characteristic of good stability of the prepared slurry. According to the method, the dispersant and part of the solvent are mixed at first, and the solvent is heated in advance to swell the dispersant, so that the dispersant is completely dissolved and swelled, and then the addition amount is reduced for use, so that the viscosity of the slurry is reduced. The temperature of the solvent is not suitable to be too high or too low, the solvent is volatilized due to high temperature of the solvent, and the swelling effect is deviated due to too low temperature of the solvent.
Optionally, the solvent is heated to 55 ℃ to 65 ℃.
The dispersant is fed according to the solid content of 25-35%.
The vacuum degree of the vacuum pumping is-80 kPa to-90 kPa.
The vacuumizing can avoid bubbles generated in the swelling and stirring process.
The low-speed stirring speed is 30 r/min-60 r/min.
The resin which is not well swelled can be thrown out by high-speed stirring, and the resin which is not well swelled can not be thrown out by low-speed stirring, so that the resin can be favorably swelled.
S2, preparing primary slurry
After the first mixture is prepared, cooling the first mixture to 30-40 ℃, mixing the cooled first mixture with the rest solvent, stirring for 5-20 min to prepare a second mixture, mixing the second mixture with carbon black, and emulsifying for 20-40 min to prepare the primary slurry.
The materials are fed step by step, so that the materials can not be fully soaked, and the formation of large gel blocks is avoided or reduced.
Optionally, the emulsification is carried out in an emulsifying machine.
Optionally, emulsification is carried out in a high speed emulsifier.
The emulsifying can ensure that the dispersant and the carbon black are fully contacted, so that a solvolysis layer is quickly formed on the surface of the carbon black, and the carbon black is prevented from being agglomerated again in the subsequent dispersing process.
S3, primary dispersion
And sequentially carrying out ultrasonic dispersion and 200-mesh filter screen on the prepared primary slurry to prepare a third mixture.
Ultrasonic dispersion can result in improved material flow in a shorter time, but the D50 is higher than the D50 of the final product.
Optionally, the ultrasonic dispersion is performed in an ultrasonic cavitation device.
Optionally, the power of the ultrasonic dispersion is 5kW to 20kW.
Optionally, the frequency of the ultrasonic dispersion is 15kHz to 30kHz.
S4, final stage Dispersion
And (4) sequentially carrying out homogeneous dispersion and 200-mesh filter screen on the prepared third mixture to prepare a fourth mixture.
Optionally, the homogenous dispersion is performed in a homogenizer.
The D50 of the slurry can reach 0.8-1.5 mu m by homogeneous dispersion.
The dispersion process is that the secondary structure body of the carbon black is decomposed into a plurality of primary structure bodies, the better the dispersion is, the easier the carbon black is to be dispersed to each corner of the whole material system, so that the carbon black has more uniform heat conduction and electric conductivity, and meanwhile, electrolyte or other functional solvents can be uniformly adsorbed to each corner of the material, and the phenomena of local heating and local invalidation of the material are avoided.
The utility model provides an ultrasonic dispersion and homogeneous dispersion all have better dispersion effect, and after the thick liquids were made to the carbon black, the minimize should be to the destruction of its primary structure body, and ultrasonic dispersion and homogeneous dispersion can not damage the primary structure body of carbon black yet, and then guarantee high electric conductivity, heat conductivity and the adsorption efficiency performance of thick liquids in the application.
S5, removing magnetism and impurities
And sequentially carrying out demagnetization and 200-mesh filter screen on the prepared fourth mixture to prepare slurry.
S6, filling
And filling the prepared slurry.
Referring to fig. 1, the present application also includes an apparatus 10 for carrying out the above-described method of preparing a slurry, comprising: a first mixing assembly 100, a second mixing assembly 200, an ultrasonic dispersion module 300, a homogenizer 400, a demagnetizer 700, and a finished product tank 800.
Wherein, the first mixing assembly 100 comprises a first stirring tank 110, a vacuum pump 120 and a heating assembly.
The first agitation tank 110 includes a first tank 111 and a first agitator 112, and the first agitator 112 is partially disposed in the first tank 111 for agitating the fluid in the first tank 111.
The first tank 111 has a first inlet 1111 and a first outlet 1112.
The vacuum pump 120 is connected to the first agitation tank 110, and serves to make the inside of the first agitation tank 110 in a vacuum state.
The heating assembly comprises a heater 130 and a heating pipeline 140, the heating pipeline 140 is connected to the heater 130, the heater 130 is used for heating the fluid in the pipeline 140, the heating pipeline 140 is sleeved outside the first stirring tank 110, and the heating pipeline 140 is used for heating the fluid in the first stirring tank 110.
The first mixing assembly 100 includes a second agitator tank 210 and an emulsifier 220.
The second agitation tank 210 includes a second tank 211 and a second agitator 212, the second agitator 212 is partially disposed in the second tank 211 for agitating the fluid in the second tank 211, and the second agitator 212 has a wall scraping function.
The second tank 211 is externally sleeved with a first jacket structure 213, and the first jacket structure 213 is used for arranging cooling water 530 for cooling the fluid in the second tank 211. The second tank 211 further has a second inlet 2111 and a second outlet 2112, and the second inlet 2111 is connected to the first outlet 1112 through the first pump 510 and a pipe.
The emulsifying machine 220 is provided with a fourth feeding hole 221 and a fourth discharging hole 222, the fourth feeding hole 221 is connected to the third discharging hole 2114 through a pipeline, the fourth discharging hole 222 is connected to the third feeding hole 2113 through a pipeline, and the emulsifying machine 220 is used for enabling the dispersing agent and the carbon black to be in full contact, enabling the surface of the carbon black to rapidly form a solvation layer and avoiding the carbon black from being agglomerated again in the subsequent dispersing process.
The ultrasonic dispersion module 300 comprises at least one ultrasonic cavitation duct having a fifth inlet 301 and a fifth outlet 302, the fifth inlet 301 is connected to the second outlet 2112 through a second pump 520 and a duct.
Optionally, the ultrasonic dispersion module 300 includes a first ultrasonic module 310, a second ultrasonic module 320, and a third ultrasonic module 330, which are connected in sequence, where the first ultrasonic module 310 includes three ultrasonic cavitation pipelines connected in parallel, the second ultrasonic module 320 includes two ultrasonic cavitation pipelines connected in parallel, and the third ultrasonic module 330 includes one parallel ultrasonic cavitation pipeline.
Because the mobility of the slurry is poor before entering the ultrasonic dispersion module 300, the mobility of the slurry is improved by the three ultrasonic cavitation pipelines arranged in parallel, so that the mobility of the slurry is improved, the mobility of the slurry is improved by the two ultrasonic cavitation pipelines arranged in parallel, so that the mobility of the slurry is further improved, and finally, the mobility of the slurry is improved by the ultrasonic cavitation pipeline arranged in parallel, so that the requirement of entering the next-stage dispersion device is met. The ultrasonic dispersion module 300 can realize better dispersion of slurry through the cooperation of the three groups of ultrasonic modules, can also improve the dispersion efficiency, and saves the cost of the equipment 10.
The homogenizer 400 has a sixth inlet 401 and a sixth outlet 402, the sixth inlet 401 is connected to the fifth outlet 302 by a pipe, and a 200-mesh screen 600 is disposed on the pipe connecting the sixth inlet 401 and the fifth outlet 302.
Optionally, the homogenizer 400 is a jet homogenizer 400.
The demagnetizer 700 has a seventh feeding hole 701 and a seventh discharging hole 702, and the seventh feeding hole 701 is connected to the sixth discharging hole 402 through a pipe.
The finished product tank 800 has an eighth inlet 801 and an eighth outlet 802, the eighth inlet 801 is connected to the seventh outlet 702 through a pipe, and the eighth outlet 802 is used for discharging. And a 200-mesh filter screen 600 is arranged on a pipeline connecting the eighth feeding hole 801 and the seventh discharging hole 702.
The finished tank 800 is jacketed with a second jacket structure 810, and cooling water 530 is disposed in the second jacket structure 810 for cooling the slurry in the finished tank 800.
One slurry and a method for preparing the same of the present application will be described in further detail with reference to examples below.
Example 1
The embodiment of the application provides slurry and a preparation method thereof, and the preparation method comprises the following steps:
s1, pretreatment of a dispersing agent
Adding part of N-methyl pyrrolidone into the first tank 111, heating the part of N-methyl pyrrolidone in the first tank 111 to 60 ℃ through a heating assembly, adding PVP K90 (Boehmerin Kagaku Co., ltd.) into the first tank 111 at this time, wherein the viscosity average molecular weight of the PVP K90 is 120 ten thousand, feeding the PVP K90 according to 30% of solid content, vacuumizing the first tank 111 by using a vacuum pump 120 to enable the first tank 111 to be in a vacuum state of-85 kPa, and stirring and swelling for 7 hours at a speed of 40r/min by using a first stirrer 112 to prepare a first mixture.
S2, preparing primary slurry
Pumping the first mixture into the second tank 211 through the first pump 510, cooling the first mixture in the second tank 211 to 35 ℃ by using cooling water 530, then putting the rest N-methylpyrrolidone into the second tank 211, adding acetylene black into the second tank 211 after stirring for 10min by using the second stirrer 212, wherein the dosage of the PVP K90 is 6wt% of the acetylene black, opening the high-speed emulsifying machine 220, and emulsifying for 30min by using the high-speed emulsifying machine 220 to obtain a primary slurry.
S3, primary Dispersion
The prepared primary slurry is pumped to the ultrasonic dispersion module 300 by the second pump 520 for ultrasonic dispersion, and the primary slurry sequentially passes through the first ultrasonic module 310, the second ultrasonic module 320, the third ultrasonic module 330 and the 200-mesh filter screen 600 to prepare a third mixture. The power of the ultrasonic dispersion was 10kW and the frequency was 20kHz.
S4, final stage Dispersion
The third mixture is homogenized and dispersed by a jet homogenizer 400, and then a fourth mixture is obtained by passing through a 200-mesh sieve 600.
S5, removing magnetism and impurities
The prepared fourth mixture is sequentially subjected to demagnetization by a demagnetizer 700 and a 200-mesh filter screen 600 to prepare slurry.
S6, filling
The prepared slurry is filled in a finished product tank 800.
Example 2
The embodiment of the application provides slurry and a preparation method thereof, and the preparation method comprises the following steps:
s1, pretreatment of a dispersing agent
Adding part of N-methyl pyrrolidone into the first tank 111, heating the part of N-methyl pyrrolidone in the first tank 111 to 60 ℃ through a heating assembly, adding PVP K110 (Gaobike corporation) into the first tank 111 at the moment, feeding the PVP K110 according to a solid content of 30%, vacuumizing the first tank 111 by using a vacuum pump 120 to enable the first tank 111 to be in a vacuum state of-85 kPa, and stirring and swelling for 7 hours at a speed of 40r/min by using a first stirrer 112 to obtain a first mixture.
S2, preparing primary slurry
Pumping the first mixture into the second tank 211 through the first pump 510, cooling the first mixture in the second tank 211 to 35 ℃ by using cooling water 530, then putting the rest N-methylpyrrolidone into the second tank 211, stirring for 10min by using the second stirrer 212, then putting acetylene black into the second tank 211, wherein the usage amount of the PVP K110 is 6wt% of the acetylene black, opening the high-speed emulsifying machine 220, and emulsifying for 30min by using the high-speed emulsifying machine 220 to obtain a primary slurry.
S3, primary Dispersion
The prepared primary slurry is pumped to the ultrasonic dispersion module 300 by the second pump 520 for ultrasonic dispersion, and the primary slurry sequentially passes through the first ultrasonic module 310, the second ultrasonic module 320, the third ultrasonic module 330 and the 200-mesh filter screen 600 to prepare a third mixture. The power of the ultrasonic dispersion was 10kW and the frequency was 20kHz.
S4, final stage Dispersion
The third mixture thus obtained is homogenized and dispersed in a jet homogenizer 400, and then passed through a 200 mesh sieve 600 to obtain a fourth mixture.
S5, removing magnetism and impurities
The prepared fourth mixture is sequentially demagnetized by a demagnetizer 700 and filtered by a 200-mesh filter screen 600 to prepare slurry.
S6, filling
The prepared slurry is filled into a finished product tank 800.
Example 3
The embodiment of the application provides slurry and a preparation method thereof, and the preparation method comprises the following steps:
s1, pretreatment of a dispersing agent
Adding part of water into the first tank 111, heating the part of water in the first tank 111 to 60 ℃ through a heating assembly, adding PVP K90 (Bo Ai New open pharmaceutical products Co., ltd.) into the first tank 111, wherein the viscosity average molecular weight of the PVP K90 is 120 ten thousand, feeding the PVP K90 according to 30% of solid content, vacuumizing the first tank 111 by a vacuum pump 120 to enable the first tank to be in a vacuum state of-85 kPa, and stirring and swelling for 7 hours at a speed of 40r/min by a first stirrer 112 to prepare a first mixture.
S2, preparing primary slurry
Pumping the first mixture into the second tank 211 through the first pump 510, cooling the first mixture in the second tank 211 to 35 ℃ by using cooling water 530, then putting the rest water into the second tank 211, putting acetylene black into the second tank 211 after stirring for 10min by using the second stirrer 212, wherein the usage amount of PVP K90 is 6wt% of the acetylene black, opening the high-speed emulsifying machine 220, and emulsifying for 30min by using the high-speed emulsifying machine 220 to obtain a primary slurry.
S3, primary Dispersion
The prepared primary slurry is pumped to the ultrasonic dispersion module 300 by the second pump 520 for ultrasonic dispersion, and the primary slurry sequentially passes through the first ultrasonic module 310, the second ultrasonic module 320, the third ultrasonic module 330 and the 200-mesh filter screen 600 to prepare a third mixture. The power of the ultrasonic dispersion was 10kW and the frequency was 20kHz.
S4, final stage Dispersion
The third mixture is homogenized and dispersed by a jet homogenizer 400, and then a fourth mixture is obtained by passing through a 200-mesh sieve 600.
S5, removing magnetism and impurities
The prepared fourth mixture is sequentially demagnetized by a demagnetizer 700 and filtered by a 200-mesh filter screen 600 to prepare slurry.
S6, filling
The prepared slurry is filled in a finished product tank 800.
Example 4
The embodiment of the application provides slurry and a preparation method thereof, and the preparation method comprises the following steps:
s1, pretreatment of a dispersing agent
Adding part of N-methyl pyrrolidone into the first tank 111, heating the part of N-methyl pyrrolidone in the first tank 111 to 60 ℃ through a heating assembly, adding PVP K30 (New York corporation) into the first tank 111 at the moment, wherein the viscosity average molecular weight of the PVP K30 is 5-8 ten thousand, feeding the PVP K30 according to 30% of solid content, vacuumizing by using a vacuum pump 120 to enable the first tank 111 to be in a vacuum state of-85 kPa, and stirring and swelling for 7 hours at the speed of 40r/min by using a first stirrer 112 to prepare a first mixture.
S2, preparing primary slurry
Pumping the first mixture into the second tank 211 through the first pump 510, cooling the first mixture in the second tank 211 to 35 ℃ by using cooling water 530, then putting the rest N-methylpyrrolidone into the second tank 211, putting acetylene black into the second tank 211 after stirring for 10min by using the second stirrer 212, wherein the usage amount of the PVP K30 is 6wt% of the acetylene black, opening the high-speed emulsifying machine 220, and emulsifying for 30min by using the high-speed emulsifying machine 220 to obtain a primary slurry.
S3, primary Dispersion
The prepared primary slurry is pumped to the ultrasonic dispersion module 300 by the second pump 520 for ultrasonic dispersion, and the primary slurry sequentially passes through the first ultrasonic module 310, the second ultrasonic module 320, the third ultrasonic module 330 and the 200-mesh filter screen 600 to prepare a third mixture. The power of the ultrasonic dispersion was 10kW and the frequency was 20kHz.
S4, final stage Dispersion
The third mixture is homogenized and dispersed by a jet homogenizer 400, and then a fourth mixture is obtained by passing through a 200-mesh sieve 600.
S5, removing magnetism and impurities
The prepared fourth mixture is sequentially demagnetized by a demagnetizer 700 and filtered by a 200-mesh filter screen 600 to prepare slurry.
S6, filling
The prepared slurry is filled in a finished product tank 800.
Example 5
The embodiment of the application provides slurry and a preparation method thereof, and the preparation method comprises the following steps:
s1, pretreatment of a dispersing agent
Adding part of N-methyl pyrrolidone into the first tank 111, heating the part of N-methyl pyrrolidone in the first tank 111 to 60 ℃ through a heating assembly, adding PVP K60 (New York corporation) into the first tank 111 at the moment, wherein the viscosity average molecular weight of the PVP K30 is 30-40 ten thousand, feeding the PVP K60 according to 30% of solid content, vacuumizing by using a vacuum pump 120 to enable the first tank 111 to be in a vacuum state of-85 kPa, and stirring and swelling for 7 hours at a speed of 40r/min by using a first stirrer 112 to prepare a first mixture.
S2, preparing primary slurry
Pumping the first mixture into the second tank 211 through the first pump 510, cooling the first mixture in the second tank 211 to 35 ℃ by using cooling water 530, then putting the rest N-methylpyrrolidone into the second tank 211, putting acetylene black into the second tank 211 after stirring for 10min by using the second stirrer 212, wherein the usage amount of PVP K60 is 6wt% of the acetylene black, opening the high-speed emulsifying machine 220, and emulsifying for 30min by using the high-speed emulsifying machine 220 to obtain a primary slurry.
S3, primary dispersion
The prepared primary slurry is pumped to the ultrasonic dispersion module 300 by the second pump 520 for ultrasonic dispersion, and the primary slurry sequentially passes through the first ultrasonic module 310, the second ultrasonic module 320, the third ultrasonic module 330 and the 200-mesh filter screen 600 to prepare a third mixture. The power of the ultrasonic dispersion was 10kW, and the frequency was 20kHz.
S4, final stage Dispersion
The third mixture is homogenized and dispersed by a jet homogenizer 400, and then a fourth mixture is obtained by passing through a 200-mesh sieve 600.
S5, removing magnetism and impurities
The prepared fourth mixture is sequentially demagnetized by a demagnetizer 700 and filtered by a 200-mesh filter screen 600 to prepare slurry.
S6, filling
The prepared slurry is filled in a finished product tank 800.
Comparative example 1
The comparative example of the application provides a slurry and a preparation method thereof, and the slurry comprises the following steps:
s1, pretreatment of a dispersing agent
Adding part of N-methyl pyrrolidone into the first tank 111, heating the part of N-methyl pyrrolidone in the first tank 111 to 60 ℃ through a heating assembly, adding PVP K90 (Boehmerin Kagaku Co., ltd.) into the first tank 111 at this time, wherein the viscosity average molecular weight of the PVP K90 is 120 ten thousand, feeding the PVP K90 according to 30% of solid content, vacuumizing the first tank 111 by using a vacuum pump 120 to enable the first tank 111 to be in a vacuum state of-85 kPa, and stirring and swelling for 7 hours at a speed of 40r/min by using a first stirrer 112 to prepare a first mixture.
S2, preparing primary slurry
Pumping the first mixture into the second tank 211 through the first pump 510, cooling the first mixture in the second tank 211 to 35 ℃ by using cooling water 530, then putting the rest N-methylpyrrolidone into the second tank 211, putting acetylene black into the second tank 211 after stirring for 10min by using the second stirrer 212, wherein the usage amount of PVP K90 is 6wt% of the acetylene black, opening the high-speed emulsifying machine 220, and emulsifying for 30min by using the high-speed emulsifying machine 220 to obtain a primary slurry.
S3, dispersing
The prepared primary slurry is pumped to the ultrasonic dispersion module 300 by the second pump 520 for ultrasonic dispersion, and the primary slurry sequentially passes through the first ultrasonic module 310, the second ultrasonic module 320, the third ultrasonic module 330 and the 200-mesh filter screen 600 to prepare a third mixture. The power of the ultrasonic dispersion was 10kW and the frequency was 20kHz.
S4, removing magnetism and impurities
The prepared third mixture is sequentially subjected to demagnetization by a demagnetizer 700 and a 200-mesh filter screen 600 to prepare slurry.
S5, filling
The prepared slurry is filled in a finished product tank 800.
Comparative example 2
The comparative example of the application provides a slurry and a preparation method thereof, and the slurry comprises the following steps:
s1, pretreatment of a dispersing agent
Adding part of N-methyl pyrrolidone into the first tank 111, heating the part of N-methyl pyrrolidone in the first tank 111 to 60 ℃ through a heating assembly, adding PVP K90 (Bo ai Xin open pharmaceutical products, inc.) into the first tank 111 at the moment, wherein the viscosity average molecular weight of the PVP K90 is 120 ten thousand, feeding the PVP K90 according to 30% of solid content, vacuumizing by using a vacuum pump 120 to enable the first tank 111 to be in a vacuum state of-85 kPa, and stirring and swelling for 7 hours at a speed of 40r/min by using a first stirrer 112 to prepare a first mixture.
S2, preparing primary slurry
Pumping the first mixture into the second tank 211 through the first pump 510, cooling the first mixture in the second tank 211 to 35 ℃ by using cooling water 530, then putting the rest N-methylpyrrolidone into the second tank 211, putting acetylene black into the second tank 211 after stirring for 10min by using the second stirrer 212, wherein the usage amount of PVP K90 is 6wt% of the acetylene black, opening the high-speed emulsifying machine 220, and emulsifying for 30min by using the high-speed emulsifying machine 220 to obtain a primary slurry.
S3, dispersing
The carbon black slurry was ground with a sand mill until the D50 of the slurry became 0.2 μm or less, with a zirconium ball size of 1 mm.
S4, removing magnetism and impurities
The prepared third mixture is sequentially demagnetized by a demagnetizer 700 and filtered by a 200-mesh filter screen 600 to prepare slurry.
S5, filling
The prepared slurry is filled into a finished product tank 800.
Test example 1
The slurries prepared in examples 1 to 5 and comparative examples 1 to 2 were measured for D50 using a laser particle size tester, and the results are shown in Table 1.
TABLE 1 slurries D50 of examples 1 to 5 and comparative examples 1 to 2
| Item | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Comparative example 1 | Comparative example 2 |
| D50(μm) | 0.30 | 0.43 | 0.55 | 0.61 | 0.70 | 0.87 | 0.23 |
As is apparent from Table 1, the dispersion processes of examples 1 to 5 of the present application include ultrasonic dispersion and homogeneous dispersion, and D50 thereof is between 0.3 μm and 0.7. Mu.m, D50 of the slurry prepared in comparative example 1 including only ultrasonic dispersion is large, opening of the secondary structure of carbon black is not completed, D50 of the slurry prepared in comparative example 2 subjected to dispersion treatment by sanding with a sand mill is small, and the primary structure of carbon black is partially destroyed.
The CDBP reduction rate of the slurries prepared in examples 1 to 5 and comparative examples 1 to 2 was measured, and the results are shown in Table 2.
The CDBP of the carbon black feedstock was tested according to the method of GB/T3780.4-2017.
The testing method of the slurry needs to dry the slurry at 150 ℃ until the weight of the slurry is not reduced, and then the testing is carried out according to the method of GB T3780.4.
TABLE 2 CDBP reduction rates of examples 1 to 5 and comparative examples 1 to 2
As is apparent from Table 2, the dispersion processes of examples 1 to 5 of the present application, which included ultrasonic dispersion and homogeneous dispersion, exhibited a CDBP reduction of 6.67% or less, the slurry obtained in comparative example 1, which included only ultrasonic dispersion, exhibited a lower CDBP reduction, the opening of the secondary structure of carbon black was not completed, the slurry obtained in comparative example 2, which was subjected to the dispersion treatment by sanding with a sand mill, exhibited a higher CDBP reduction, and the primary structure of carbon black was partially destroyed.
The BET change rates of the slurries obtained in examples 1 to 5 and comparative examples 1 to 2 were measured, and the results are shown in Table 3.
The BET of the carbon black feedstock was tested according to the method of GB/T19587-2004.
The testing method of the slurry needs to carry out pretreatment on the slurry, and the pretreatment method comprises the following steps:
s1, centrifuging the slurry to be detected for 10min at a rotating speed of 3000r/min by using a centrifuge;
s2, removing the supernatant of the centrifuged slurry, adding absolute ethyl alcohol with the same amount as the supernatant, and stirring for 5min by using a glass rod until the mixture is uniformly mixed;
s3, centrifuging again for 10min at the rotating speed of 3000r/min by using the centrifuge;
s4, repeating the step S2 and the step S3 twice;
s5, drying for 30min at 150 ℃ by using a hot air oven until the weight of the material is not reduced;
and S6, testing according to the BET testing method of the powder carbon black to obtain the BET of the carbon black in the slurry.
TABLE 3 BET Change Rate of examples 1 to 5 and comparative examples 1 to 2
As is apparent from Table 3, the dispersion processes of examples 1 to 5 of the present application, which included ultrasonic dispersion and homogeneous dispersion, had BET change rates of 5% or less, the BET change rate of comparative example 1, which included only ultrasonic dispersion, was low, the opening of the secondary structure of carbon black was not completed, the BET change rate of comparative example 2, which was subjected to sand grinding dispersion treatment using a sand mill, was high, and the primary structure of carbon black was partially destroyed.
Test example 2
Taking the slurries prepared in examples 1 to 5 and comparative examples 1 to 2, the viscosities of the slurries prepared in examples 1 to 5 were in the range of 500mpa.s to 3000mpa.s, the viscosity of the slurry prepared in comparative example 1 was 6200mpa.s, and the viscosity of the slurry prepared in comparative example 2 was 970mpa.s. Using an Antopa MSR92 instrument for 10s -1 The viscosity change rate of the slurry at a temperature of-5 ℃ to 50 ℃ was measured, and the results are shown in Table 4. In addition, a slurry viscosity greater than 3000mpa.s affects the fluidity thereof, making the application difficult.
TABLE 4 Rate of Change of viscosity of slurries of examples 1 to 5 and comparative examples 1 to 2
As is clear from Table 4, in examples 1 to 3, a resin having a viscosity average molecular weight of 100 ten thousand or more was used as a dispersionThe agent and the slurry are in 10s -1 The viscosity change rate of the slurry within-5 to 50 ℃ is less than or equal to 30 percent at a fixed shear rate; as is clear from comparison of example 1 with examples 4 to 5, the slurry was prepared for 10 seconds using a resin having a viscosity average molecular weight of less than 100 ten thousand as a dispersant -1 The viscosity change rate of the slurry within-5 ℃ to 50 ℃ is more than 30 percent at the fixed shear rate.
The slurries of example 1 and comparative example 2 were amplitude scanned using a rheometer and the amplitude scan patterns are shown in figures 2 to 3.
As can be seen from fig. 2, the storage modulus G' is always greater than the loss modulus G "at shear stress below 3Pa, demonstrating that the slurry of example 1 has extremely high stability characteristics at low shear (at rest).
As can be seen from fig. 3, the storage modulus G 'is always larger than the loss modulus G "at a shear stress of 1Pa or less, and the storage modulus G' is always smaller than the loss modulus G" at shear stresses of 1Pa to 3Pa, demonstrating that the slurry of comparative example 1 has lower stability at low shear (at rest) than the slurry of example 1.
In summary, the slurry in the embodiment of the present application uses resin with a viscosity average molecular weight of more than 100 ten thousand as a dispersant to disperse carbon black, the viscosity of the prepared slurry is controlled to be below 30% at a temperature of-5 ℃ to 50 ℃, and the slurry hardly settles when being sheared below 3Pa, i.e., the slurry has good stability, is convenient to apply, and is hardly influenced by the viscosity change. The D50 of the slurry is between 0.3 and 0.7 microns, so that better dispersion is realized, the CDBP reduction rate is less than or equal to 6.67 percent, the BET change rate is less than or equal to 5 percent, the slurry has higher electrical conductivity, thermal conductivity and adsorption efficiency after application, and the application addition amount can be reduced.
The foregoing description is given for the purpose of illustrating particular embodiments of the present application and is not in any way intended to limit the invention, as numerous modifications and variations will be apparent to those skilled in the art. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present application shall be included in the protection scope of the present application.
Claims (13)
1. The slurry is characterized by comprising carbon black, a dispersing agent and a solvent, wherein the reduction rate of the compression oil absorption value of the carbon black in the slurry is less than or equal to 6.67%.
2. The slurry of claim 1, wherein the carbon black in the slurry has a specific surface area change of 5% or less.
3. The slurry according to claim 1, wherein the D50 of the slurry is 0.3 to 0.7 μm.
4. The slurry of claim 1, wherein the slurry has a storage modulus G' greater than a loss modulus G "below a shear stress of 3 Pa.
5. The slurry of claim 1, wherein the slurry is present for 10s -1 Under the condition that the fixed shear rate and the slurry viscosity range are 500mpa.s-3000mpa.s, the slurry viscosity change rate within-5-50 ℃ is less than or equal to 30 percent.
6. The slurry according to claim 1, characterized in that the total magnetic substance content in the slurry is < 1000ppb.
7. The slurry of claim 1, wherein Fe is 10ppm or less and Ni is 5ppm or less.
8. The slurry according to any one of claims 1 to 7, characterized in that it comprises 10% to 30% by weight of said carbon black, said dispersant being used in an amount of 4% to 8% by weight of said carbon black;
optionally, the dispersing agent is resin, the viscosity average molecular weight of the resin is not less than 100 ten thousand, and the dispersing agent comprises polyvinylpyrrolidone;
optionally, the solvent comprises water or N-methylpyrrolidone.
9. A method for preparing the slurry according to any one of claims 1 to 8, characterized in that the method for preparing the slurry comprises: and sequentially carrying out ultrasonic dispersion and homogeneous dispersion on the primary slurry to prepare the slurry, wherein the primary slurry is prepared by mixing the dispersing agent, the solvent and the carbon black.
10. The method of preparing a slurry according to claim 9, wherein the power of the ultrasonic dispersion is 5 to 20kW;
optionally, the frequency of the ultrasonic dispersion is 15kHz to 30kHz.
11. The method of producing a slurry according to claim 9, wherein the method of producing a virgin slurry comprises:
mixing a dispersant and a part of solvent to swell the dispersant to prepare a first mixture, and mixing the first mixture, the carbon black and the rest of the solvent to prepare the primary slurry;
optionally, before mixing the dispersing agent and part of the solvent, heating the solvent to 50-70 ℃, adding the dispersing agent after the temperature of the solvent reaches a target temperature, and swelling for 6-8 h under a stirring state;
optionally, the dispersant is fed at a solid content of 25-35%;
optionally, the stirring speed in the swelling process is 30 r/min-60 r/min;
alternatively, the swelling process is performed under vacuum conditions;
optionally, after the first mixture is prepared, the first mixture and the rest of the solvent are mixed and stirred for 5min to 20min to prepare a second mixture, and then the second mixture and the carbon black are mixed and emulsified for 20min to 40min to prepare the primary slurry.
12. The method according to claim 9, wherein after the slurry is prepared, the slurry is subjected to a desmear treatment.
13. An apparatus for carrying out the method for preparing a slurry according to any one of claims 9 to 12, characterized in that it comprises:
the first material mixing assembly is provided with a first feeding hole and a first discharging hole;
the second mixing component comprises a second stirring tank and an emulsifying machine, the second stirring tank is provided with a second feeding hole, a third feeding hole, a second discharging hole and a third discharging hole, the second feeding hole is connected to the first discharging hole, the emulsifying machine is provided with a fourth feeding hole and a fourth discharging hole, the fourth feeding hole is connected to the third discharging hole, and the fourth discharging hole is connected to the third feeding hole;
the ultrasonic dispersion module is provided with a fifth feeding hole and a fifth discharging hole, and the fifth feeding hole is connected to the second discharging hole;
the homogenizer is provided with a sixth feeding hole and a sixth discharging hole, and the sixth feeding hole is connected with the fifth discharging hole.
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