CN115611285B - Slurry, preparation method and equipment thereof - Google Patents
Slurry, preparation method and equipment thereof Download PDFInfo
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- CN115611285B CN115611285B CN202211266392.7A CN202211266392A CN115611285B CN 115611285 B CN115611285 B CN 115611285B CN 202211266392 A CN202211266392 A CN 202211266392A CN 115611285 B CN115611285 B CN 115611285B
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
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Abstract
The application provides slurry, a preparation method and equipment thereof, and belongs to the technical field of carbon black dispersion. The slurry comprises 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 percent. According to the method, the carbon black is firstly dispersed to obtain the slurry, and compared with the independent carbon black, the slurry has better dispersibility in application, so that the application difficulty is reduced, and the carbon black is firstly prepared into the slurry, so that the carbon black is beneficial to constructing an electric conduction and heat conduction network. Meanwhile, the primary structure body of the carbon black in the slurry is low in destruction rate, high in electric conductivity, high in thermal conductivity and high in adsorption efficiency after the slurry is 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, a preparation method and equipment thereof.
Background
Carbon black can be used as a high-quality conductive additive to be widely applied in various industries such as rubber, plastics, dry batteries, lead-acid batteries, microwave absorption, secondary lithium batteries and the like. Although the addition proportion is not high (1% -10%), the adsorption effect of the conductive and heat conductive solvent (electrolyte adsorption performance) is very critical in application.
Carbon black having a high specific surface area (BET) has both high electrical conductivity, thermal conductivity and adsorption efficiency, and a low addition ratio.
However, carbon blacks having high specific surface areas (BET) have poor dispersibility.
Disclosure of Invention
The application provides slurry, a preparation method and equipment thereof, which have better dispersibility and lower destruction rate of a primary structure of carbon black.
Embodiments of the present application are implemented as follows:
in a first aspect, the present examples provide a slurry comprising carbon black, a dispersant, and a solvent, wherein the carbon black in the slurry has a reduction in compression oil absorption value (CDBP) of 6.67% or less.
In the technical scheme, the carbon black is firstly dispersed to obtain the slurry, the slurry has better dispersibility when being applied compared with the independent carbon black, the application difficulty is reduced, and the carbon black is firstly prepared into the slurry, so that the carbon black is beneficial to constructing an electric conduction and heat conduction network. Meanwhile, the primary structure body of the carbon black in the slurry is low in destruction rate, high in electric conductivity, high in thermal conductivity and high in adsorption efficiency after the slurry is applied, and the application addition amount can be reduced.
With reference to the first aspect, in a first possible example of the first aspect of the present application, the rate of change of the specific surface area of the carbon black in the slurry is less than or equal to 5%.
With reference to the first aspect, in a second possible example of the first aspect of the present application, the D50 of the slurry is 0.3 μm to 0.7 μm.
With reference to the first aspect, in a third possible example of the first aspect of the present application, the storage modulus G 'is greater than the loss modulus G' below a shear stress of 3 Pa.
In the above examples, it was shown that the slurry has higher stability in the rest state.
With reference to the first aspect, in a fourth possible example of the first aspect of the present application, the slurry is at 10s -1 The rate of change of the slurry viscosity is less than or equal to 30% at a temperature of-5 ℃ to 50 ℃ under the conditions that the fixed shear rate and the slurry viscosity range are 500mpa.s to 3000 mpa.s.
In the above examples, it was shown that the viscosity of the slurry changed little from-5 ℃ to 50 ℃, i.e. the viscosity of the slurry did not substantially affect its application.
In combination with the first aspect, in a fifth possible example of the first aspect of the present application, the 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 dispersing agent is resin, the viscosity average molecular weight of the resin is more than or equal to 100 ten thousand, and the dispersing agent comprises polyvinylpyrrolidone.
Alternatively, the solvent comprises water or N-methylpyrrolidone.
In the above examples, the dispersant is used in a lower amount in the slurry of the present application.
The resin with the viscosity average molecular weight exceeding 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 for a long time at room temperature.
With reference to the first aspect, in a sixth possible example of the first aspect of the present application, the total magnetic substance content in the slurry is < 1000ppb.
With reference to the first aspect, in a seventh possible example of the first aspect of the present application, fe is less than or equal to 10ppm and ni is less than or equal to 5ppm in the above slurry.
In a second aspect, the present application provides a method for preparing the above slurry, comprising: the primary product slurry is prepared by sequentially carrying out ultrasonic dispersion and homogeneous dispersion, and the primary product slurry is prepared by mixing a dispersing agent, a solvent and carbon black.
In the technical scheme, the ultrasonic dispersion can improve the fluidity of the material in a shorter time, the homogeneous dispersion can further refine the slurry, and the ultrasonic dispersion and the homogeneous dispersion have lower damage rate to the primary structure of the carbon black, so that the slurry has better dispersibility, higher electrical conductivity, thermal conductivity and adsorption efficiency after being applied, and the application addition amount can be reduced.
With reference to the second aspect, in a first possible example of the second aspect of the present application, the power of the ultrasonic dispersion is 5kW to 20kW.
Alternatively, the frequency of ultrasonic dispersion is 15kHz to 30kHz.
With reference to the second aspect, in a second possible example of the second aspect of the present application, the method for preparing a preliminary slurry includes:
the dispersant is first mixed with partial solvent to swell the dispersant to obtain the first mixture, and the first mixture, carbon black and the rest solvent are mixed to obtain the initial slurry.
Optionally, before mixing the dispersant and part of the solvent, heating the solvent to 50-70 ℃, adding the dispersant after the temperature of the solvent reaches the target temperature, and swelling for 6-8 hours under the stirring state.
Optionally, the dispersant is dosed at 25% -35% solids.
Optionally, the stirring rate in the swelling process is 30 r/min-60 r/min.
Alternatively, the swelling process is performed under vacuum.
Optionally, after the first mixture is prepared, the first mixture and the rest solvent are mixed and stirred for 5-20 min to prepare a second mixture, and then the second mixture and the carbon black are mixed and emulsified for 20-40 min to prepare the primary product slurry.
In the above examples, the dispersant and a part of the solvent are mixed first, so that better swelling of the dispersant can be achieved, and the influence of the dispersant on the viscosity of the slurry is reduced. And adding other raw materials to obtain the primary pulp.
Dispersing agents with viscosity average molecular weight exceeding 100 ten thousand are difficult to swell in solvents, and the solvents are heated to target temperature, so that the dispersing agent is favorable for swelling.
The step-by-step feeding can avoid the insufficient infiltration of materials and avoid or reduce the formation of large gel blocks.
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 impurity removal treatment.
In the above examples, the removal of impurities 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 example provides an apparatus for carrying out the above-described method of preparing a slurry, comprising: the ultrasonic dispersing device comprises a first mixing component, a second mixing component, an ultrasonic dispersing module and a homogenizer.
The first mixing component is provided with a first feed inlet and a first discharge outlet.
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 with 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 with the third discharging hole, and the fourth discharging hole is connected with the third feeding hole.
The ultrasonic dispersion module is provided with a fifth feed inlet and a fifth discharge outlet, and the fifth feed inlet is connected with the second discharge outlet.
The homogenizer is provided with a sixth feed inlet and a sixth discharge outlet, and the sixth feed inlet is connected with the fifth discharge outlet.
In the above technical solution, the apparatus of the present application can be used for preparing a slurry.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings that are needed in the embodiments will be briefly described below, it being understood that the following drawings only illustrate some embodiments of the present application and therefore should not be considered limiting the scope, and that other related drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
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 mixing component; 110-a first stirred tank; 111-a first tank; 1111—a first feed inlet; 1112-a first discharge port; 112-a first stirrer; 120-vacuum pump; 130-a heater; 140-heating the pipeline; 200-a second mixing component; 210-a second stirred tank; 211-a second tank; 2111-a second feed port; 2112-a second outlet; 2113-third feed port; 2114-a third discharge port; 212-a second stirrer; 213-a first jacket structure; 220-emulsifying machine; 221-fourth feed inlet; 222-a fourth discharge port; 300-an ultrasonic dispersion module; 301-a fifth feed inlet; 302-a fifth discharge port; 310-a first ultrasonic module; 320-a second ultrasonic module; 330-a third ultrasound module; 400-homogenizer; 401-sixth feed inlet; 402-a sixth discharge port; 510-a first pump; 520-a second pump; 530-cooling water; 600-200 mesh filter screen; 700-demagnetizer; 701-seventh feed port; 702-a seventh discharge port; 800-a finished product tank; 801-eighth feed inlet; 802-eighth discharge port; 810-second jacket structure.
Detailed Description
Embodiments of the present application will be described in detail below with reference to examples, but it will be understood by those skilled in the art that the following examples are only for illustration of the present application and should not be construed as limiting the scope of the present application. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
Carbon black can be used as a high-quality conductive additive to be widely applied in various industries such as rubber, plastics, dry batteries, lead-acid batteries, microwave absorption, secondary lithium batteries and the like. Although the addition proportion is not high (1% -10%), the adsorption effect of the conductive and heat conductive solvent (electrolyte adsorption performance) is very critical in application.
With the development requirements of the energy field and the emerging material technology, on one hand, the electric conductivity, the thermal conductivity and the adsorption efficiency performance of carbon black in application need to be improved; on the other hand, the addition proportion of the carbon black in the application is reduced.
The inventors have found through research that carbon blacks having a high specific surface area (BET) can meet the above-mentioned needs. Specific surface area (BET) unit of carbon black is m 2 Increasing BET per gram means that at the same mass, the carbon black has more external surface area for electrical, thermal and adsorption. And theoretically the larger the BET, the smaller the primary particles of the material, and the larger the number of primary particles. The number of carbon black particles is increased by about eight times under the condition of doubling the BET with the same mass, so that a richer conductive network can be constructed under the condition of adding a small amount of carbon black. However, as BET increases, greater application difficulties arise. Carbon black as a nanoscale material has an increased BET, and carbon particles become smaller and larger under the same mass, and the intermolecular force of carbon black becomes larger. In the mixing process of application, the dispersion difficulty of the carbon black can also increase exponentially, and in the mixing process, if the carbon black cannot be uniformly dispersed, the problems of local heating, inconsistent electrical properties and the like can occur in the processes of electric conduction and heat conduction. Therefore, the problem of dispersing the high BET carbon black is solved, and the problem is the root cause of reducing the application bottleneck of the material and improving the performance of the material.
Since carbon black is a three-dimensional branched structure of nano-scale, under the influence of intermolecular forces, a plurality of carbon black structures (primary structures) are entangled into an aggregate (secondary structure) of micro-scale (10 μm to 30 μm), and the secondary structure of carbon black is dispersed so as to be opened, the carbon black exhibits good electrical conductivity, thermal conductivity and adsorption efficiency, but if the carbon black structure is excessively dispersed, the carbon black structure is broken, the carbon black will lose adsorption capacity completely, and the like.
Through intensive researches, the inventor finds that the slurry is obtained by dispersing the carbon black, the slurry has better dispersibility in application compared with the independent carbon black, the application difficulty is reduced, and the carbon black is prepared into the slurry, so that the carbon black is beneficial to constructing an electric conduction and heat conduction network. Meanwhile, the primary structure body of the carbon black in the slurry is low in destruction rate, high in electric conductivity, high in thermal conductivity and high in adsorption efficiency after the slurry is applied, and the application addition amount can be reduced.
The following specifically describes a slurry, a preparation method and equipment thereof in the embodiment of the present application:
the present application provides a slurry comprising carbon black, a dispersant, and a solvent.
Alternatively, the carbon black may be acetylene black or other carbon black.
The dispersing agent comprises resin, and the viscosity average molecular weight of the resin is more than or equal to 100 ten thousand.
Optionally, the dispersing agent is polyvinylpyrrolidone with a viscosity average molecular weight of 100-150 ten thousand.
The solvent comprises water or N-methylpyrrolidone.
Alternatively, the slurry comprises 10wt% to 30wt% carbon black, the dispersant is used in an amount of 4wt% to 8wt% of the carbon black, and the remainder is solvent.
Compared with the use amount of the dispersing agent in other slurry which is 10-100 wt% of the carbon black, the use amount of the dispersing agent in the slurry is lower, so that the addition amount of the carbon black is improved, and the electrical conductivity, the thermal conductivity and the adsorption efficiency of the carbon black are further improved.
Alternatively, the slurry comprises 10wt% to 30wt% carbon black, the dispersant is used in an amount of 4wt% to 7wt% of the carbon black, and the remainder is 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.
CDBP decrease rate of carbon black in slurry= (CDBP of carbon black in CDBP-slurry of carbon black raw material)/CDBP of carbon black raw material is 100%.
The CDBP of the carbon black raw material was tested according to the method of GB/T3780.4-2017.
The slurry testing method needs to dry the slurry at 150 ℃ until the weight is not reduced, and then tests the slurry according to the GB T3780.4 method.
Alternatively, the CDBP reduction rate of the carbon black in the slurry is less than or equal to 10 percent.
The BET change rate of the carbon black in the slurry is less than or equal to 5 percent.
The BET change rate of carbon black in the slurry= (BET of carbon black-carbon black raw material in slurry)/BET of carbon black raw material is 100%.
The BET of the carbon black raw material was measured according to the method of GB/T19587-2004.
The slurry testing method needs to pre-treat the slurry, and the pre-treatment method comprises the following steps:
s1, centrifuging slurry to be detected by using a centrifuge at a rotating speed of 3000r/min for 10min;
s2, removing supernatant from 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 supernatant is uniformly mixed;
s3, centrifuging for 10min at a rotating speed of 3000r/min by using a centrifugal machine again;
s4, repeating the steps S2 and S3 twice;
s5, drying for 30min at 150 ℃ by using a hot air oven until the weight of the material is not reduced;
s6, testing according to a BET test 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 is 0.3-0.7 μm.
When 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 mu m, the secondary structure of the carbon black is just opened, and the primary structure of the carbon black is not damaged, so that the slurry has higher electric conductivity, thermal conductivity and adsorption efficiency after being applied, and the application addition amount can be reduced.
By way of example, where the carbon black is acetylene carbon 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 'is larger than the loss modulus G' when the shear stress of the slurry is below 3Pa, which indicates that the slurry has higher stability in a static state.
Slurry at 10s -1 The viscosity change rate of the slurry at-5-50 ℃ is less than or equal to 30% under the conditions that the fixed shear rate and the viscosity of the slurry are 500 mpa.s-3000 mpa.s, which shows that the viscosity change of the slurry at-5-50 ℃ is small, i.e. the viscosity of the slurry does not basically influence the application of the slurry.
The total magnetic substance content 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 dispersing agent
Firstly, part of solvent is added, the solvent is heated to 50-70 ℃, after the temperature of the solvent reaches the target temperature, dispersing agent is added into the solvent, vacuumizing is carried out, and swelling is carried out for 6-8 h under low-speed stirring.
The larger the molecular weight of the dispersant is, the less the dispersant is easy to swell, the higher the viscosity of the slurry is, and the prepared slurry cannot be used. But the high molecular weight dispersant also has the characteristic of good stability of the prepared slurry. The viscosity of the slurry is reduced by mixing the dispersing agent with a part of solvent, and heating the solvent in advance to swell the dispersing agent thoroughly, and then reducing the addition amount. And the temperature of the solvent is not too high or too low, the solvent can volatilize due to the high temperature of the solvent, and the swelling effect deviation can be caused due to the too low temperature of the solvent.
Optionally, the solvent is heated to 55 ℃ to 65 ℃.
The dispersant is added according to the solid content of 25-35%.
The vacuum degree of the vacuumizing is-80 kPa to-90 kPa.
The vacuum can avoid generating bubbles in the swelling and stirring process.
The low-speed stirring speed is 30 r/min-60 r/min.
The unswollen resin can be thrown out by high-speed stirring, but the unswollen resin can not be thrown out by low-speed stirring, so that the good swelling of the resin can be realized.
S2, preparing primary pulp
After the first mixture is prepared, the temperature of the first mixture is reduced to 30-40 ℃, the cooled first mixture and the rest solvent are mixed and stirred for 5-20 min to prepare a second mixture, the second mixture and the carbon black are mixed, and emulsification is carried out for 20-40 min to prepare the primary product slurry.
The step-by-step feeding can avoid the insufficient infiltration of materials and avoid or reduce the formation of large gel blocks.
Optionally, the emulsification is performed in an emulsifying machine.
Alternatively, emulsification is performed in a high speed emulsifying machine.
The emulsification can enable the dispersing agent to be fully contacted with the carbon black, so that a solvation layer is formed on the surface of the carbon black rapidly, and the carbon black is prevented from agglomerating again in the subsequent dispersing process.
S3, primary dispersion
And sequentially carrying out ultrasonic dispersion and a 200-mesh filter screen on the prepared primary pulp to prepare a third mixture.
Ultrasonic dispersion can improve the flowability of the material in a shorter time, but the D50 is higher compared to the D50 of the final product.
Optionally, the ultrasonic dispersion is performed in an ultrasonic cavitation device.
Alternatively, the power of the ultrasonic dispersion is 5kW to 20kW.
Alternatively, the frequency of ultrasonic dispersion is 15kHz to 30kHz.
S4, final stage dispersion
And sequentially carrying out homogenizing dispersion and 200-mesh filtering on the prepared third mixture to prepare a fourth mixture.
Alternatively, the homogenization and dispersion are performed in a homogenizer.
The homogeneous dispersion can make the D50 of the slurry reach 0.8-1.5 μm.
The dispersing process is to decompose the secondary structure of the carbon black into a plurality of primary structures, and the better the dispersing, the easier the carbon black is to disperse to each corner of the whole material system, so that the carbon black has more uniform heat and electric conductivity, and simultaneously, electrolyte or other functional solvents can be uniformly adsorbed to each corner of the material, thereby avoiding the phenomena of local heating and local invalidation of the material.
The ultrasonic dispersion and the homogeneous dispersion of the method have good dispersion effect, after the carbon black is prepared into the slurry, the damage to the primary structure body of the carbon black is reduced as much as possible, and the ultrasonic dispersion and the homogeneous dispersion can not damage the primary structure body of the carbon black, so that the high conductivity, the heat conductivity and the adsorption efficiency performance of the slurry in application are ensured.
S5, removing magnetism and impurities
And sequentially carrying out demagnetization and 200-mesh filtering on the prepared fourth mixture to prepare slurry.
S6, filling
And filling the prepared slurry.
Referring to fig. 1, the present application further includes an apparatus 10 for performing the above-described slurry preparation method, 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 tank 800.
Wherein the first mixing assembly 100 comprises a first mixing 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, the first agitator 112 being 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 agitator tank 110 for placing the first agitator 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 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 fluid in the first stirring tank 110.
The first mixing assembly 100 includes a second mixing tank 210 and an emulsifying machine 220.
The second agitator tank 210 includes a second tank 211 and a second agitator 212, the second agitator 212 being partially disposed in the second tank 211 for agitating the fluid in the second tank 211, and the second agitator 212 having a wall scraping effect.
The second tank 211 is sleeved with a first jacket structure 213, and cooling water 530 is arranged in the first jacket structure 213 and used for cooling the fluid in the second tank 211. The second tank 211 further has a second inlet 2111 and a second outlet 2112, the second inlet 2111 being connected to the first outlet 1112 through the first pump 510 and tubing.
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, the emulsifying machine 220 is used for enabling the dispersing agent and the carbon black to fully contact, enabling the surface of the carbon black to quickly form a solvation layer, and avoiding re-agglomeration of the carbon black in the subsequent dispersing process.
The ultrasonic dispersion module 300 includes at least one ultrasonic cavitation tube having a fifth feed port 301 and a fifth discharge port 302, the fifth feed port 301 being connected to the second discharge port 2112 by a second pump 520 and a tube.
Optionally, the ultrasonic dispersing module 300 includes a first ultrasonic module 310, a second ultrasonic module 320 and a third ultrasonic module 330 that are sequentially connected, the first ultrasonic module 310 includes three ultrasonic cavitation pipes that are arranged in parallel, the second ultrasonic module 320 includes two ultrasonic cavitation pipes that are arranged in parallel, and the third ultrasonic module 330 includes one ultrasonic cavitation pipe that is connected in parallel.
Because the fluidity of the slurry is poor before entering the ultrasonic dispersion module 300, the fluidity of the slurry is improved by three ultrasonic cavitation pipelines which are arranged in parallel, the fluidity of the slurry is further improved by two ultrasonic cavitation pipelines which are arranged in parallel, and finally the fluidity of the slurry is improved by one ultrasonic cavitation pipeline which is arranged in parallel, so that the slurry meets the requirement of entering the next-stage dispersion device. The ultrasonic dispersion module 300 of the present application, through the cooperation of three groups of ultrasonic modules, can enable the slurry to realize better dispersion, can also improve the efficiency of dispersion, and saves the cost of the equipment 10.
The homogenizer 400 has a sixth feed inlet 401 and a sixth discharge outlet 402, the sixth feed inlet 401 is connected to the fifth discharge outlet 302 by a pipe, and a 200 mesh screen 600 is provided on the pipe connecting the sixth feed inlet 401 and the fifth discharge outlet 302.
Alternatively, homogenizer 400 is a jet homogenizer 400.
The demagnetizer 700 has a seventh feed port 701 and a seventh discharge port 702, the seventh feed port 701 being connected to the sixth discharge port 402 by a pipe.
The finished tank 800 has an eighth feed port 801 and an eighth discharge port 802, the eighth feed port 801 being connected to the seventh discharge port 702 by a pipe, the eighth discharge port 802 being for discharging. And a 200-mesh filter screen 600 is arranged on a pipeline connecting the eighth feed inlet 801 and the seventh discharge outlet 702.
The finished tank 800 is jacketed with a second jacket structure 810, and cooling water 530 is provided in the second jacket structure 810 for cooling the slurry in the finished tank 800.
A slurry and a method for preparing the same of the present application are described in further detail below with reference to examples.
Example 1
The embodiment of the application provides a slurry and a preparation method thereof, wherein the slurry comprises the following steps:
s1, pretreatment of dispersing agent
Adding part of N-methyl pyrrolidone into the first tank 111, heating part of N-methyl pyrrolidone in the first tank 111 to 60 ℃ by a heating component, adding PVP K90 (Boai New open source pharmaceutical Co., ltd.) into the first tank 111 at the moment, wherein the viscosity average molecular weight of PVP K90 is 120 ten thousand, and the PVP K90 is fed according to the solid content of 30%, vacuumizing by 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 by a first stirrer 112 at a speed of 40r/min to obtain a first mixture.
S2, preparing primary pulp
Pumping the first mixture into a second tank 211 through a first pump 510, cooling the first mixture in the second tank 211 to 35 ℃ through cooling water 530, then adding the rest of N-methyl pyrrolidone into the second tank 211, stirring for 10min through a second stirrer 212, adding acetylene black into the second tank 211, wherein the dosage of PVP K90 is 6wt% of the acetylene black, opening a high-speed emulsifying machine 220, and emulsifying for 30min through the high-speed emulsifying machine 220 to obtain the primary product slurry.
S3, primary dispersion
The prepared primary pulp is pumped to the ultrasonic dispersion module 300 by the second pump 520 for ultrasonic dispersion, and the primary pulp 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 prepared third mixture is subjected to homogenization and dispersion by a jet homogenizer 400, and then is filtered by a 200-mesh filter screen 600 to prepare a fourth mixture.
S5, removing magnetism and impurities
The prepared fourth mixture is sequentially subjected to demagnetizing by a demagnetizer 700 and a 200-mesh filter screen 600 to prepare slurry.
S6, filling
The resulting slurry is filled into a finished tank 800.
Example 2
The embodiment of the application provides a slurry and a preparation method thereof, wherein the slurry comprises the following steps:
s1, pretreatment of dispersing agent
Adding part of N-methyl pyrrolidone into the first tank 111, heating part of N-methyl pyrrolidone in the first tank 111 to 60 ℃ through a heating assembly, adding PVP K110 (Tabi Ke Co.) into the first tank 111, wherein the PVP K110 has a viscosity average molecular weight of 110 ten thousand, the PVP K110 is fed according to the solid content of 30%, vacuumizing by adopting 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 adopting a first stirrer 112 to obtain a first mixture.
S2, preparing primary pulp
Pumping the first mixture into a second tank 211 through a first pump 510, cooling the first mixture in the second tank 211 to 35 ℃ through cooling water 530, then adding the rest of N-methyl pyrrolidone into the second tank 211, stirring for 10min through a second stirrer 212, adding acetylene black into the second tank 211, wherein the dosage of PVP K110 is 6wt% of the acetylene black, opening a high-speed emulsifying machine 220, and emulsifying for 30min through the high-speed emulsifying machine 220 to obtain the primary product slurry.
S3, primary dispersion
The prepared primary pulp is pumped to the ultrasonic dispersion module 300 by the second pump 520 for ultrasonic dispersion, and the primary pulp 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 prepared third mixture is subjected to homogenization and dispersion by a jet homogenizer 400, and then is filtered by a 200-mesh filter screen 600 to prepare a fourth mixture.
S5, removing magnetism and impurities
The prepared fourth mixture is sequentially subjected to demagnetizing by a demagnetizer 700 and a 200-mesh filter screen 600 to prepare slurry.
S6, filling
The resulting slurry is filled into a finished tank 800.
Example 3
The embodiment of the application provides a slurry and a preparation method thereof, wherein the slurry comprises the following steps:
s1, pretreatment of dispersing agent
Adding part of water into the first tank 111, heating part of the water in the first tank 111 to 60 ℃ through a heating assembly, adding PVP K90 (Boai New open source pharmaceutical Co., ltd.) into the first tank 111 at the moment, wherein the viscosity average molecular weight of PVP K90 is 120 ten thousand, PVP K90 is fed according to the solid content of 30%, vacuumizing by adopting 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 adopting a first stirrer 112 to obtain a first mixture.
S2, preparing primary pulp
The first mixture is pumped into a second tank 211 through a first pump 510, the first mixture in the second tank 211 is cooled to 35 ℃ by adopting cooling water 530, then the rest water is put into the second tank 211, acetylene black is put into the second tank 211 after stirring for 10min by adopting a second stirrer 212, the dosage of PVP K90 is 6wt% of the acetylene black, a high-speed emulsifying machine 220 is started, and the high-speed emulsifying machine 220 is adopted to emulsify for 30min, so that the primary product slurry is prepared.
S3, primary dispersion
The prepared primary pulp is pumped to the ultrasonic dispersion module 300 by the second pump 520 for ultrasonic dispersion, and the primary pulp 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 prepared third mixture is subjected to homogenization and dispersion by a jet homogenizer 400, and then is filtered by a 200-mesh filter screen 600 to prepare a fourth mixture.
S5, removing magnetism and impurities
The prepared fourth mixture is sequentially subjected to demagnetizing by a demagnetizer 700 and a 200-mesh filter screen 600 to prepare slurry.
S6, filling
The resulting slurry is filled into a finished tank 800.
Example 4
The embodiment of the application provides a slurry and a preparation method thereof, wherein the slurry comprises the following steps:
s1, pretreatment of dispersing agent
Adding part of N-methyl pyrrolidone into the first tank 111, heating part of N-methyl pyrrolidone in the first tank 111 to 60 ℃ through a heating assembly, adding PVP K30 (new open source company) into the first tank 111 at the moment, adding PVP K30 with the viscosity average molecular weight of 5-8 ten thousand according to the solid content of 30%, 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 obtain a first mixture.
S2, preparing primary pulp
Pumping the first mixture into a second tank 211 through a first pump 510, cooling the first mixture in the second tank 211 to 35 ℃ through cooling water 530, then adding the rest of N-methyl pyrrolidone into the second tank 211, stirring for 10min through a second stirrer 212, adding acetylene black into the second tank 211, wherein the dosage of PVP K30 is 6wt% of the acetylene black, opening a high-speed emulsifying machine 220, and emulsifying for 30min through the high-speed emulsifying machine 220 to obtain the primary product slurry.
S3, primary dispersion
The prepared primary pulp is pumped to the ultrasonic dispersion module 300 by the second pump 520 for ultrasonic dispersion, and the primary pulp 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 prepared third mixture is subjected to homogenization and dispersion by a jet homogenizer 400, and then is filtered by a 200-mesh filter screen 600 to prepare a fourth mixture.
S5, removing magnetism and impurities
The prepared fourth mixture is sequentially subjected to demagnetizing by a demagnetizer 700 and a 200-mesh filter screen 600 to prepare slurry.
S6, filling
The resulting slurry is filled into a finished tank 800.
Example 5
The embodiment of the application provides a slurry and a preparation method thereof, wherein the slurry comprises the following steps:
s1, pretreatment of dispersing agent
Adding part of N-methyl pyrrolidone into the first tank 111, heating part of N-methyl pyrrolidone in the first tank 111 to 60 ℃ through a heating assembly, adding PVP K60 (new open source company) into the first tank 111 at the moment, adding PVP K30 with the viscosity average molecular weight of 30-40 ten thousand, adding PVP K60 according to the solid content of 30%, vacuumizing by adopting 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 adopting a first stirrer 112 to obtain a first mixture.
S2, preparing primary pulp
Pumping the first mixture into a second tank 211 through a first pump 510, cooling the first mixture in the second tank 211 to 35 ℃ through cooling water 530, then adding the rest of N-methyl pyrrolidone into the second tank 211, stirring for 10min through a second stirrer 212, adding acetylene black into the second tank 211, wherein the dosage of PVP K60 is 6wt% of the acetylene black, opening a high-speed emulsifying machine 220, and emulsifying for 30min through the high-speed emulsifying machine 220 to obtain the primary product slurry.
S3, primary dispersion
The prepared primary pulp is pumped to the ultrasonic dispersion module 300 by the second pump 520 for ultrasonic dispersion, and the primary pulp 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 prepared third mixture is subjected to homogenization and dispersion by a jet homogenizer 400, and then is filtered by a 200-mesh filter screen 600 to prepare a fourth mixture.
S5, removing magnetism and impurities
The prepared fourth mixture is sequentially subjected to demagnetizing by a demagnetizer 700 and a 200-mesh filter screen 600 to prepare slurry.
S6, filling
The resulting slurry is filled into a finished tank 800.
Comparative example 1
The comparative example of the present application provides a slurry and a method for preparing the same, comprising the steps of:
s1, pretreatment of dispersing agent
Adding part of N-methyl pyrrolidone into the first tank 111, heating part of N-methyl pyrrolidone in the first tank 111 to 60 ℃ by a heating component, adding PVP K90 (Boai New open source pharmaceutical Co., ltd.) into the first tank 111 at the moment, wherein the viscosity average molecular weight of PVP K90 is 120 ten thousand, and the PVP K90 is fed according to the solid content of 30%, vacuumizing by 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 by a first stirrer 112 at a speed of 40r/min to obtain a first mixture.
S2, preparing primary pulp
Pumping the first mixture into a second tank 211 through a first pump 510, cooling the first mixture in the second tank 211 to 35 ℃ through cooling water 530, then adding the rest of N-methyl pyrrolidone into the second tank 211, stirring for 10min through a second stirrer 212, adding acetylene black into the second tank 211, wherein the dosage of PVP K90 is 6wt% of the acetylene black, opening a high-speed emulsifying machine 220, and emulsifying for 30min through the high-speed emulsifying machine 220 to obtain the primary product slurry.
S3, dispersing
The prepared primary pulp is pumped to the ultrasonic dispersion module 300 by the second pump 520 for ultrasonic dispersion, and the primary pulp 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 demagnetizing by a demagnetizer 700 and a 200-mesh filter screen 600 to prepare slurry.
S5, filling
The resulting slurry is filled into a finished tank 800.
Comparative example 2
The comparative example of the present application provides a slurry and a method for preparing the same, comprising the steps of:
s1, pretreatment of dispersing agent
Adding part of N-methyl pyrrolidone into the first tank 111, heating part of N-methyl pyrrolidone in the first tank 111 to 60 ℃ by a heating component, adding PVP K90 (Boai New open source pharmaceutical Co., ltd.) into the first tank 111 at the moment, wherein the viscosity average molecular weight of PVP K90 is 120 ten thousand, and the PVP K90 is fed according to the solid content of 30%, vacuumizing by 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 by a first stirrer 112 at a speed of 40r/min to obtain a first mixture.
S2, preparing primary pulp
Pumping the first mixture into a second tank 211 through a first pump 510, cooling the first mixture in the second tank 211 to 35 ℃ through cooling water 530, then adding the rest of N-methyl pyrrolidone into the second tank 211, stirring for 10min through a second stirrer 212, adding acetylene black into the second tank 211, wherein the dosage of PVP K90 is 6wt% of the acetylene black, opening a high-speed emulsifying machine 220, and emulsifying for 30min through the high-speed emulsifying machine 220 to obtain the primary product slurry.
S3, dispersing
The carbon black slurry was ground using a sand mill, the zirconium spheres had a size of 1mm, and the slurry was ground until the D50 of the slurry reached 0.2 μm or less.
S4, removing magnetism and impurities
The prepared third mixture is sequentially subjected to demagnetizing by a demagnetizer 700 and a 200-mesh filter screen 600 to prepare slurry.
S5, filling
The resulting slurry is filled into a finished tank 800.
Test example 1
The slurries prepared in examples 1 to 5 and comparative examples 1 to 2 were tested for D50 using a laser particle size tester, and the results are shown in Table 1.
TABLE 1 slurries D50 of examples 1-5 and comparative examples 1-2
| Project | 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 clear from Table 1, the dispersion processes of examples 1 to 5 of the present application include ultrasonic dispersion and homogeneous dispersion, in which D50 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, secondary structure of carbon black opening is not completed, D50 of the slurry prepared in comparative example 2 subjected to sand grinding dispersion treatment by a sand mill is small, and primary structure portion of carbon black is broken.
The CDBP reduction rates of the slurries prepared in examples 1 to 5 and comparative examples 1 to 2 were measured, and the results are shown in table 2.
The CDBP of the carbon black raw material was tested according to the method of GB/T3780.4-2017.
The slurry testing method needs to dry the slurry at 150 ℃ until the weight is not reduced, and then tests the slurry according to the GB T3780.4 method.
TABLE 2 CDBP reduction rates for examples 1-5 and comparative examples 1-2
As is clear from Table 2, the dispersion processes of examples 1 to 5 of the present application include ultrasonic dispersion and homogeneous dispersion, the CDBP decrease rate was 6.67% or less, the slurry prepared in comparative example 1 including only ultrasonic dispersion had a lower CDBP decrease rate, the secondary structure of which carbon black was not completed to be opened, the slurry prepared in comparative example 2 which was subjected to sand grinding dispersion treatment by a sand mill had a larger CDBP decrease rate, and the primary structure portion of the carbon black was destroyed.
The BET change rates of the slurries prepared 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 raw material was measured according to the method of GB/T19587-2004.
The slurry testing method needs to pre-treat the slurry, and the pre-treatment method comprises the following steps:
s1, centrifuging slurry to be detected by using a centrifuge at a rotating speed of 3000r/min for 10min;
s2, removing supernatant from 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 supernatant is uniformly mixed;
s3, centrifuging for 10min at a rotating speed of 3000r/min by using a centrifugal machine again;
s4, repeating the steps S2 and S3 twice;
s5, drying for 30min at 150 ℃ by using a hot air oven until the weight of the material is not reduced;
s6, testing according to a BET test 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 clear from Table 3, the dispersion processes of examples 1 to 5 of the present application include ultrasonic dispersion and homogeneous dispersion, and the BET change rate is 5% or less, and the BET change rate of the slurry prepared in comparative example 1 including only ultrasonic dispersion is low, and the secondary structure of carbon black is not completed, and the BET change rate of the slurry prepared in comparative example 2 subjected to sand mill sand dispersion treatment is large, and the primary structure portion of carbon black is broken.
Test example 2
The viscosities of the slurries prepared in examples 1 to 5 and comparative examples 1 to 2 were 500mpa.s to 3000mpa.s, the viscosities of the slurries prepared in comparative example 1 were 6200mpa.s, and the viscosities of the slurries prepared in comparative example 2 were 970mpa.s. Using An Dongpa MSR92 instrument for 10s -1 The rate of change of the slurry viscosity at a temperature of-5℃to 50℃was measured, and the results are shown in Table 4. In addition, the viscosity of the slurry exceeding 3000mpa.s affects the fluidity thereof, resulting in difficulty in application.
TABLE 4 rates of change of viscosity of the slurries of examples 1 to 5 and comparative examples 1 to 2
As is clear from Table 4, in examples 1 to 3, the resin having a viscosity average molecular weight of 100 ten thousand or more was used as the dispersant, and the slurry was used for 10 seconds -1 The viscosity change rate of the slurry at the fixed shear rate of minus 5 ℃ to 50 ℃ is less than or equal to 30 percent; as is clear from a comparison of example 1 and examples 4 to 5, the resin having a viscosity average molecular weight of < 100 ten thousand was used as the dispersant, and the slurry was used for 10 seconds -1 The rate of change of the slurry viscosity at-5 ℃ to 50 ℃ is more than 30 percent at a fixed shear rate.
The slurries of example 1 and comparative example 2 were subjected to amplitude scanning by a rheometer, and the amplitude scanning patterns are shown in fig. 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 is clear from fig. 3, the storage modulus G 'is always larger than the loss modulus G "when the shear stress is 1Pa or less, and the storage modulus G' is always smaller than the loss modulus G" when the shear stress is 1Pa to 3Pa, which proves that the slurry of comparative example 1 has a lower stability at low shear (in a stationary state) than the slurry of example 1.
In summary, the slurry of the embodiment of the application adopts the resin with the viscosity average molecular weight exceeding 100 ten thousand as the dispersant to disperse the carbon black, the variation of the viscosity of the prepared slurry is controlled to be below 30 percent between minus 5 ℃ and 50 ℃, and the slurry hardly generates sedimentation when the slurry is sheared to be below 3Pa, namely the slurry has better stability, is more convenient in application and is not influenced by the variation of the viscosity of the slurry basically. The D50 of the slurry is between 0.3 and 0.7 mu m, 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 electric conductivity, thermal conductivity and adsorption efficiency after being applied, and the application addition amount can be reduced.
The foregoing is merely a specific embodiment of the present application and is not intended to limit the present application, and various modifications and variations may be made to the present application by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principles of the present application should be included in the protection scope of the present application.
Claims (14)
1. A 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 3.68% -6.67%, and the slurry is 10s -1 Under the conditions that the fixed shear rate and the slurry viscosity range are 500 mpa.s-3000 mpa.s, the slurry viscosity change rate in the temperature range of minus 5 ℃ to 50 ℃ is less than or equal to 30 percent, the specific surface area change rate of carbon black in the slurry is 4.1% -5 percent, and the D50 of the slurry is 0.3 mu m-0.7 mu m;
the slurry comprises 10-30wt% of the carbon black, and the consumption of the dispersing agent is 4-8wt% of the carbon black.
2. The slurry according to claim 1, wherein the slurry has a storage modulus G' greater than a loss modulus g″ at a shear stress of 3Pa or less.
3. The slurry according to claim 1, characterized in that the total magnetic substance content in the slurry is < 1000ppb.
4. The slurry of claim 1, wherein Fe is less than or equal to 10ppm and ni is less than or equal to 5ppm in the slurry.
5. The slurry of claim 1, wherein the dispersant is a resin having a viscosity average molecular weight of 100 tens of thousands or more, and the dispersant comprises polyvinylpyrrolidone.
6. The slurry of claim 1, wherein the solvent comprises water or N-methylpyrrolidone.
7. A method for preparing the slurry according to any one of claims 1 to 6, comprising: heating the solvent to 50-70 ℃, adding the dispersing agent after the temperature of the solvent reaches the target temperature, swelling for 6-8 hours under the stirring state to obtain a first mixture, mixing the first mixture, the carbon black and the rest of the solvent to obtain a primary product slurry, and sequentially carrying out ultrasonic dispersion and homogeneous dispersion on the primary product slurry to obtain the slurry.
8. The method for preparing slurry according to claim 7, wherein the power of ultrasonic dispersion is 5kw to 20kw.
9. The method for preparing slurry according to claim 8, wherein the ultrasonic dispersion frequency is 15khz to 30khz.
10. The method for preparing slurry according to claim 7, wherein the dispersant is added according to a solid content of 25% -35%.
11. The method for producing a slurry according to claim 7, wherein the stirring rate in the swelling process is 30r/min to 60r/min.
12. The method of claim 7, wherein the swelling process is performed under vacuum.
13. The method for preparing a slurry according to claim 7, wherein after the first mixture is prepared, the first mixture and the remaining solvent are mixed and stirred for 5 to 20 minutes to prepare a second mixture, and the second mixture and the carbon black are mixed and emulsified for 20 to 40 minutes to prepare the primary slurry.
14. The method for producing a slurry according to claim 7, wherein the slurry is subjected to a impurity removal treatment after the slurry is produced.
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| CN100438146C (en) * | 2005-10-12 | 2008-11-26 | 比亚迪股份有限公司 | Lithium ion cell, anode therefor and preparing method thereof |
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