Preparation method of high-dispersity acetylene carbon black and particles
By mixing acetylene carbon black with CH3COOOH solution and conducting conductive treatment, the problem of reduced purity when the dispersion of acetylene carbon black is improved, and acetylene carbon black particles with high dispersion, low resistivity and stable performance are prepared, which meets the high purity and High conductivity requirements.
Patent Information
- Application Number
- CN202411315047.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-09-20
- Publication Date
- 2024-12-17
- Estimated Expiration
- 2044-09-20
AI Technical Summary
When the prior art improves the dispersion of acetylene carbon black, the addition of dispersion additives leads to a decrease in its purity and cannot meet the purity requirements of certain products.
By mixing acetylene carbon black with CH3COOOH solution and conducting conductive treatment, a highly dispersible acetylene carbon black was prepared, and no dispersant or auxiliary agent was introduced to improve its dispersion and conductivity.
The preparation of highly dispersible acetylene carbon black was achieved, the dispersibility value was increased to 17.4, the resistivity was reduced to 1.3Ω·m, the purity was high and the stability was good, and the impurities introduced by the dispersion additive were avoided.
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Figure CN119144175A_ABST
Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of carbon black production, and in particular relates to a method for preparing highly dispersed acetylene carbon black and particles. Background Art
[0002] Acetylene black (also known as acetylene black) is a carbon black obtained by continuous pyrolysis of acetylene with a purity of more than 99% obtained by decomposition and refining of by-product gas during the pyrolysis of calcium carbide or naphtha (raw gasoline). Compared with furnace carbon black, its crystallization and secondary structure are more developed, so its conductivity and liquid absorption are also better. Due to the small amount of impurities such as heavy metals, the loss caused by self-discharge is small. It is mainly used for the negative electrode of nickel-hydrogen batteries, and can also be used in supercapacitors as a conductor.
[0003] At present, in order to improve the dispersibility and stability of carbon black in polar solvent systems, the main method is dispersant-assisted dispersion. For example, Chinese invention patent No. CN201380047462.2 discloses an acetylene black dispersion slurry and a lithium-ion secondary battery. In order to improve the dispersibility of acetylene black, a dispersing aid is added to acetylene black, which can increase the dispersibility value of acetylene black to about 17 and the resistivity to 3Ω·m, thereby making acetylene black more easily dispersed in the dispersion medium and improving the dispersibility of acetylene black. However, since the dispersing aid is added to acetylene black, impurities are indirectly introduced to reduce the purity of acetylene black, resulting in low purity and failure to meet some product requirements. Summary of the invention
[0004] In view of this, the present invention provides a method for preparing highly dispersible acetylene black and particles, so as to solve the technical problem in the prior art that a dispersing aid is added when improving the dispersibility of acetylene black, and impurities are indirectly introduced to reduce the purity of acetylene black, resulting in low purity and failure to meet some product requirements.
[0005] To achieve the above objectives, this application adopts the following scheme:
[0006] A method for preparing highly dispersible acetylene carbon black comprises the following steps:
[0007] Mixing raw material acetylene carbon black with CH3COOOH solution to form a mixture; wherein the mass ratio of the CH3COOOH solution to the raw material acetylene carbon black is (4 to 6):15;
[0008] The mixed material is subjected to a conductive treatment to prepare highly dispersed acetylene carbon black.
[0009] Preferably, the step of “performing a conductive treatment on the mixture to prepare highly dispersed acetylene carbon black” comprises the following steps:
[0010] Provided is a conductive container, the conductive container comprising at least one carbon black modified cylinder, both ends of the carbon black modified cylinder being provided with a cover body, the cover body being provided with a conductive column, and the conductive column being capable of connecting to a power source;
[0011] Introducing the mixed material into the carbon black modified cylinder, covering the cover body, and making the conductive column contact with the mixed material;
[0012] The power-on state is maintained for a first preset time, and the cover is opened to obtain the highly dispersed acetylene carbon black.
[0013] Preferably, in the "first preset time period for maintaining the power-on state", the power-on voltage is 220V to 380V.
[0014] Preferably, in the “maintaining the power-on state for the first preset time period”, the power-on state is maintained until the current in the circuit is constant.
[0015] Preferably, the mass concentration of the CH3COOOH solution is 3% to 5%.
[0016] Preferably, the temperature of the CH3COOOH solution is 60°C to 90°C.
[0017] Preferably, the average particle size of the raw material acetylene carbon black is 30nm to 45nm, and the specific surface area is 55m 2 / g to 70m 2 / g, oxygen content of 0.07% to 0.26%, pH value of 5 to 7, and resistivity of 3Ω·m to 5Ω·m.
[0018] Preferably, the method further comprises drying the prepared highly dispersible acetylene carbon black.
[0019] A highly dispersible acetylene carbon black particle is prepared by the following method: preparing highly dispersible acetylene carbon black by the above-mentioned highly dispersible acetylene carbon black preparation method and drying it; soaking the dried highly dispersible acetylene carbon black in water, and granulating it after soaking to obtain highly dispersible acetylene carbon black particles.
[0020] A highly dispersible acetylene carbon black particle is prepared by the following method: using a CH3COOOH solution to perform an impregnation treatment on a raw material acetylene carbon black, wherein the mass ratio of the CH3COOOH solution to the raw material acetylene carbon black is (4 to 6):15, and the mass concentration of the CH3COOOH solution is 3% to 5%; conducting a conductive treatment on the raw material acetylene carbon black after the impregnation treatment; and granulating and drying the raw material acetylene carbon black after the conductive treatment to obtain highly dispersible acetylene carbon black particles.
[0021] The technical solution adopted in this application has at least the following beneficial effects:
[0022] 1. The present application provides a method for preparing highly dispersed acetylene carbon black. When preparing highly dispersed acetylene carbon black, the raw material acetylene carbon black and the CH3COOOH solution are mixed in a mixer to form a mixture, and then the mixture is subjected to a conductive treatment to obtain highly dispersed acetylene carbon black, wherein the mass ratio of the CH3COOOH solution to the raw material acetylene carbon black is (4 to 6):15, and the prepared highly dispersed acetylene carbon black has a dispersibility value of 17.4 and a hydroxyl value of 0.32 mgKOH / g. Compared with the dispersibility value of 8.21 of the raw material acetylene carbon black, the highly dispersed acetylene carbon black prepared by the method provided in the present application has a higher dispersibility, and when the raw material acetylene carbon black is mixed with the CH3COOOH solution and subjected to a conductive treatment to prepare the highly dispersed acetylene carbon black, no dispersant or auxiliary agent is introduced, so the prepared highly dispersed acetylene carbon black does not have impurities and has a higher purity;
[0023] 2. The resistivity of the highly dispersed acetylene carbon black prepared by the method provided by the present invention is 1.3Ω·m, which is 3Ω·m higher than the resistivity of high-quality acetylene carbon black on the market. It has high dispersibility and high conductivity.
[0024] 3. When the prepared highly dispersed acetylene carbon black was left standing in water at room temperature for 15 days, there was no precipitation, no stratification, and no agglomeration. However, when the raw acetylene carbon black was left standing in water at room temperature for more than 5 days, there was precipitation, stratification, and agglomeration. It can be seen that the method provided in the present invention can prepare highly dispersed acetylene carbon black with good stability. BRIEF DESCRIPTION OF THE DRAWINGS
[0025] Figure 1 It is a line graph of the dispersibility value of acetylene black in Example 2 of the present invention;
[0026] Figure 2 It is a line graph of the hydroxyl value of acetylene black in Example 2 of the present invention;
[0027] Figure 3 It is a line graph of the resistivity of acetylene black in Example 2 of the present invention;
[0028] Figure 4 It is a line graph of the dispersion stability value of acetylene black in Example 2 of the present invention;
[0029] Figure 5 Schematic diagram of the conductive container in the present invention.
[0030] In the figure, there are a conductive container 100 , a carbon black modified barrel 110 , a cover 111 , a conductive column 112 , and a power source 120 . DETAILED DESCRIPTION
[0031] In order to facilitate the understanding of the present application, the present application will be described more comprehensively below in conjunction with the accompanying drawings. And the preferred implementation of the present application is given. However, the present application can be implemented in many different forms and is not limited to the implementation described herein. On the contrary, the purpose of providing these implementations is to make the disclosure of the present application more thoroughly and comprehensively understood.
[0032] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as those generally understood by those skilled in the art to which this application belongs. The terms used herein in the specification of this application are only for the purpose of describing specific embodiments and are not intended to limit this application. The term "and / or" used herein includes any and all combinations of one or more related listed items.
[0033] In this embodiment, a method for preparing highly dispersed acetylene black includes: mixing raw acetylene black with a CH3COOOH solution to form a mixture; wherein the mass ratio of the CH3COOOH solution to the raw acetylene black is (4 to 6):15; and conducting a conductive treatment on the mixture to prepare highly dispersed acetylene black.
[0034] In this embodiment, the raw material acetylene carbon black is acetylene carbon black powder. When preparing highly dispersible acetylene carbon black, the raw material acetylene carbon black and the CH3COOOH solution are mixed in a mixer to form a mixture, and then the mixture is subjected to a conductive treatment to obtain highly dispersible acetylene carbon black. When the mass ratio of the CH3COOOH solution to the raw material acetylene carbon black is (4 to 6):15, the prepared highly dispersible acetylene carbon black has high dispersibility, dispersion stability and conductivity. When the mass ratio of the CH3COOOH solution to the raw material acetylene carbon black is 6:15, the effect is better.
[0035] The prepared highly dispersed acetylene carbon black has a dispersibility value of 17.4 and a hydroxyl value of 0.32 mgKOH / g. Compared with the dispersibility value of 8.21 of the raw material acetylene carbon black, the highly dispersed acetylene carbon black prepared by the method provided in the present application has a higher dispersibility. When the raw material acetylene carbon black is mixed with the CH3COOOH solution for conductive treatment to prepare the highly dispersed acetylene carbon black, no dispersant or auxiliary agent is introduced. Therefore, the prepared highly dispersed acetylene carbon black has no impurities and has a high purity. The resistivity of the highly dispersed acetylene carbon black prepared by the method provided by the present invention is 1.3Ω·m, which is 3Ω·m compared to the resistivity of high-quality acetylene carbon black on the market. It has high dispersibility and high conductivity. When the prepared highly dispersed acetylene carbon black is left standing in normal temperature water for 15 days, there is no precipitation, no stratification, and no agglomeration. When the raw material acetylene carbon black is left standing in normal temperature water for more than 5 days, there is precipitation, stratification, and agglomeration. It can be seen that the method provided in the present invention can prepare highly dispersed acetylene carbon black with good stability.
[0036] Please see Figure 5 , wherein the "conductive treatment of the mixture to prepare highly dispersed acetylene carbon black" includes: providing a conductive container 100, the conductive container 100 includes at least one carbon black modified cylinder 110, both ends of the carbon black modified cylinder 110 are provided with a cover body 111, the cover body 111 is provided with a conductive column 112, and the conductive column 112 can be connected to a power source 120; introducing the mixture into the carbon black modified cylinder 110, covering the cover body 111, and making the conductive column 112 contact with the mixture; keeping the power on state, and after the power on is ended, opening the cover body 111 to obtain the highly conductive acetylene carbon black.
[0037] The conductive container 100 provided in the present application includes at least one carbon black modified cylinder 110, which can be a cylinder or a square cylinder. The size of the carbon black modified cylinder 110 can be set according to actual needs. Preferably, in the present embodiment, two carbon black modified cylinders 110 are provided, which can be used alternately to save time and improve efficiency. Covers 111 are provided at both ends of the carbon black modified cylinder 110, and conductive posts 112 are provided on the cover 111, and the conductive posts 112 are connected to the power supply 120. When in use, the cover 111 is first opened, and the mixture is introduced into the carbon black modified cylinder 110. When the carbon black modified cylinder 110 is filled with the mixture, the cover 111 is closed, and the power supply 120 switch is controlled, and the conductive posts 112 remain powered on to conduct conductive treatment on the mixture.
[0038] Specifically, in the "maintaining the power-on state for the first preset time", the power-on voltage is 220V to 380V. The power-on voltage is preferably 220V.
[0039] Specifically, in the "maintaining the power-on state for the first preset time", the power-on state is maintained until the current in the circuit is constant. When the mixed material in the carbon black modified cylinder 110 is subjected to conductive treatment, the power-on voltage is constant, preferably 220V. When the current is constant, that is, the resistance of the mixed material in the carbon black modified cylinder 110 is basically stable and no longer fluctuates greatly, the power is stopped to obtain highly dispersed acetylene carbon black.
[0040] Preferably, the mass concentration of the CH3COOOH solution is 3% to 5%, preferably 5%.
[0041] Preferably, the temperature of the CH3COOOH solution is 60°C to 90°C, preferably 75°C.
[0042] In the above embodiment, the average particle size of the raw material acetylene carbon black is 30nm to 45nm, and the specific surface area is 55m 2 / g to 70m 2 / g, oxygen content of 0.07% to 0.26%, pH value of 5 to 7, and resistivity of 3Ω·m.
[0043] In some optional embodiments, the method further includes drying the prepared highly dispersed acetylene carbon black.
[0044] A highly dispersible acetylene carbon black particle is prepared by the following method: preparing highly dispersible acetylene carbon black by the above-mentioned highly dispersible acetylene carbon black preparation method and drying it; soaking the dried highly dispersible acetylene carbon black in water, and granulating it after soaking to obtain highly dispersible acetylene carbon black particles.
[0045] The highly dispersed acetylene carbon black prepared by the method for preparing highly dispersed acetylene carbon black provided by the present invention is dried until the water content reaches the conventional requirement, thereby obtaining the dried highly dispersed acetylene carbon black. Then, the dried highly dispersed acetylene carbon black is soaked in water for a period of time, and then granulated to obtain highly dispersed acetylene carbon black particles with high purity and high conductivity.
[0046] A highly dispersible acetylene carbon black particle is prepared by the following method: using a CH3COOOH solution to perform an impregnation treatment on a raw material acetylene carbon black, wherein the mass ratio of the CH3COOOH solution to the raw material acetylene carbon black is (4 to 6):15, and the mass concentration of the CH3COOOH solution is 3% to 5%; conducting a conductive treatment on the raw material acetylene carbon black after the impregnation treatment; and granulating and drying the raw material acetylene carbon black after the conductive treatment to obtain highly dispersible acetylene carbon black particles.
[0047] When preparing highly dispersed acetylene carbon black particles, first, the raw material acetylene carbon black is impregnated with the CH3COOOH solution. Preferably, the mass ratio of the CH3COOOH solution to the raw material acetylene carbon black is 6:15, and the mass concentration of the CH3COOOH solution is 5%. Then, the raw material acetylene carbon black after the impregnation treatment is introduced into the conductive container 100 for conductive treatment to obtain highly dispersed acetylene carbon black particles with higher purity and higher conductivity.
[0048] The following specific experimental examples are used to further illustrate the technical solutions and technical effects of the present invention. It should be noted that the following experimental examples are only for further explaining the present invention and do not limit the technical solutions of the present invention.
[0049] 1. Experimental Materials and Methods
[0050] 1.1 Experimental Materials
[0051] Raw materials: acetylene carbon black and CH3COOOH solution. The raw material acetylene carbon black comes from Ningxia Jinhai Ward Technology Co., Ltd., and the CH3COOOH solution comes from commercial sources.
[0052] The conductive container 100 used in the following embodiments includes a carbon black modified cylinder 110. To facilitate the calculation of resistivity, the cross-sectional area of the carbon black modified cylinder 110 is 0.25 m 2 , the length of the carbon black modified cylinder 110 is 2m;
[0053] The raw material acetylene carbon black has a dispersibility value of 8.21, a hydroxyl value of 0.2 mg KOH / g, a resistivity of 3 Ω·m, and slight precipitation after being placed in room temperature water for 6 days.
[0054] 1.2 Experimental methods
[0055] The experiment is divided into 6 treatment groups, namely comparative example 1, comparative example 2, comparative example 3, embodiment 1, embodiment 2, and embodiment 3. Treated acetylene carbon black (dried acetylene carbon black) is prepared by the 6 treatment groups, and its parameters are detected according to the following detection method:
[0056] Detect the current and voltage during the conductive treatment, calculate the resistance, and calculate the resistivity of the treated acetylene carbon black according to the calculation formula of resistance and resistivity;
[0057] The treated acetylene carbon black was placed in normal temperature water for different periods of time to test its dispersion stability;
[0058] According to the method for detecting carbon black dispersibility provided in the patent number: CN201710367601.X, entitled: Determining carbon black dispersibility using blackness distribution curve, the dispersibility value of the acetylene carbon black treated in the following examples is detected;
[0059] The hydroxyl value of the treated acetylene carbon black was measured by gas chromatography.
[0060] 2. Comparative Example 1: Conductive treatment of raw material acetylene carbon black
[0061] Take the raw material acetylene carbon black and introduce it into the carbon black modification cylinder 110. When the carbon black modification cylinder 110 is full of the raw material acetylene carbon black, cover the cover 111, turn on the power supply 120, and keep the power-on state. The power-on voltage is 220V. When the current in the circuit is constant, turn off the power supply 120 switch to obtain the treated acetylene carbon black, record the current value and voltage value when the current is constant, calculate the resistivity of the treated acetylene carbon black according to the above calculation method, and test its dispersibility, dispersion stability and hydroxyl value. The results are shown in Table 1.
[0062] 3. Comparative Example 2: Conductive treatment of the mixture (raw materials acetylene carbon black, water)
[0063] The difference between this comparative example 2 and the comparative example 1 is that: 75°C water is mixed with the raw material acetylene carbon black in a mass ratio of 6:15 to form a mixture, and the mixture is introduced into the carbon black modification cylinder 110. After the carbon black modification cylinder 110 is filled with the mixture, the cover 111 is closed, and the power supply 120 is turned on to keep the power on state. The other steps are the same as the steps in the comparative example 1. The results are shown in Table 1.
[0064] 4. Comparative Example 3: Non-conductive treatment of the mixed material (raw material acetylene carbon black, CH3COOOH solution)
[0065] The difference between this comparative example 3 and the above comparative example 1 is that a CH3COOOH solution at 75°C is mixed with the raw material acetylene black in a mass ratio of 6:15 to form a mixture, wherein the mass concentration of the CH3COOOH solution is 5%, and no conductive treatment is performed. Acetylene black is obtained after drying. The results are shown in Table 1.
[0066] 5. Example 1: Conductive treatment of the mixture (raw material acetylene carbon black, CH3COOOH solution)
[0067] The difference between this embodiment 1 and the above comparative example 1 is that a CH3COOOH solution at 75°C is mixed with the raw material acetylene black in a mass ratio of 6:15 to form a mixture, the mass concentration of the CH3COOOH solution is 5%, and the other steps are the same as those in the above comparative example 1. The results are shown in Table 1.
[0068] Table 1 Experimental results test table
[0069]
[0070] It can be seen from the data in Comparative Example 1 in Table 1 above that when the raw material acetylene carbon black is directly introduced into the carbon black modification cylinder 110 and energized, the dispersion value of the treated acetylene carbon black is 8.39 and the hydroxyl value is 0.2 mgKOH / g; when energized at a voltage of 220 V, the current is 10 A when the current reaches a constant, and according to the resistivity calculation formula, the resistivity of the acetylene carbon black is 2.75 Ω·m; when the acetylene carbon black is left standing in normal temperature water for 7 days, there is a slight precipitation, no stratification, and no agglomeration after standing for 1 to 6 days;
[0071] It can be seen from the data in Comparative Example 2 in Table 1 above that when the raw material acetylene carbon black is mixed with 75° C. water to form a mixture, the mixture is introduced into the carbon black modification cylinder 110 and energized, and the obtained acetylene carbon black has a dispersibility value of 11.37 and a hydroxyl value of 0.25 mgKOH / g; when energized at a voltage of 220 V, the current is 14 A when the current reaches a constant, and according to the resistivity calculation formula, the resistivity of the acetylene carbon black is 1.96 Ω·m; when the acetylene carbon black is left standing in normal temperature water for 12 days, slight precipitation occurs;
[0072] It can be seen from the data in Comparative Example 3 in Table 1 above that when a 75°C CH3COOOH solution is mixed with the raw material acetylene carbon black in a mass ratio of 6:15 to form a mixture, the dispersion value of the treated acetylene carbon black after drying is 8.9 and the hydroxyl value is 0.21 mgKOH / g; when powered at a voltage of 220V, the current is 11A when the current reaches a constant, and according to the resistivity calculation formula, the resistivity of the acetylene carbon black is 2.6Ω·m; the acetylene carbon black is slightly precipitated when it is left standing in normal temperature water for 8 days;
[0073] It can be seen from the data in Example 1 in Table 1 above that when a 75°C CH3COOOH solution is mixed with the raw material acetylene carbon black in a mass ratio of 6:15 to form a mixture, and the mixture is introduced into the carbon black modification cylinder 110 and energized, the dispersion value of the treated acetylene carbon black is 17.4 and the hydroxyl value is 0.32 mgKOH / g; when energized at a voltage of 220V, the current is 22A when the current reaches a constant, and according to the resistivity calculation formula, the resistivity of the acetylene carbon black is 1.3Ω·m; when the acetylene carbon black is left standing in normal temperature water for 15 days, there is no precipitation, no stratification, and no agglomeration;
[0074] The data in Table 1 above fully reflect that the raw material acetylene carbon black is mixed with a CH3COOOH solution to form a mixture, and the mixture is introduced into the carbon black modification cylinder 110 for electrification. The obtained acetylene carbon black has a larger hydroxyl value, a smaller resistivity, a higher dispersibility value, and better dispersion stability than the acetylene carbon black obtained in Comparative Examples 1, 2, and 3. The smaller the resistivity, the better the conductivity. Therefore, the acetylene carbon black in Example 1 has higher dispersibility and conductivity, and is a highly dispersible acetylene carbon black. In addition, since only a CH3COOOH solution is added for conductive treatment during the preparation process to improve the dispersibility of the acetylene carbon black, without the aid of other dispersants and additives, the prepared highly dispersible acetylene carbon black does not have impurities and has high purity.
[0075] 6. Example 2: Optimization of the mass ratio of raw material acetylene carbon black to CH3COOOH solution
[0076] The difference between this embodiment 2 and the above embodiment 1 is that the mass ratio of the raw material acetylene carbon black to the CH3COOOH solution is changed to form a mixture, and the mass concentration of the CH3COOOH solution at the mass ratio is changed accordingly. The other steps are the same as those in the above embodiment 1. The mass ratio of the raw material acetylene carbon black to the CH3COOOH solution is specifically shown in Table 2:
[0077] Table 2 Mass ratio of raw material acetylene carbon black and CH3COOOH solution
[0078]
[0079]
[0080] After the experiment, the hydroxyl value, resistivity, dispersibility and dispersion stability of the high-dispersibility acetylene carbon black after the first to twenty-fourth experimental treatments were detected and calculated. The specific results are shown in Table 3:
[0081] Table 3 Experimental results of Example 2
[0082]
[0083]
[0084] Please refer to Table 3 and Figure 1, when the mass ratio of CH3COOOH solution to raw material acetylene carbon black is constant, the concentration of CH3COOOH solution is changed. When the concentration of CH3COOOH solution is 1% to 4%, the dispersibility value of high-dispersibility acetylene carbon black shows a gradual upward trend. When the concentration of CH3COOOH solution is greater than 4%, the dispersibility value of high-dispersibility acetylene carbon black basically does not change. When the concentration of CH3COOOH solution is greater than 4%, the dispersibility value of high-dispersibility acetylene carbon black has a downward trend. Therefore, the concentration of the CH3COOOH solution is 3% to 5%; when the concentration of the CH3COOOH solution is constant, the mass ratio of the CH3COOOH solution to raw material acetylene carbon black is changed. When the mass ratio of the CH3COOOH solution to raw material acetylene carbon black is 2 to 6:15, the dispersibility value of high-dispersibility acetylene carbon black shows a gradual upward trend. When the mass ratio of the CH3COOOH solution to raw material acetylene carbon black is greater than 6:15, the dispersibility value of high-dispersibility acetylene carbon black basically does not change.
[0085] Please refer to Table 3 and Figure 2 , when the mass ratio of the CH3COOOH solution to the raw material acetylene carbon black is constant, the concentration of the CH3COOOH solution is changed. When the concentration of the CH3COOOH solution is 1% to 4%, the hydroxyl value of the highly dispersed acetylene carbon black shows a gradual increasing trend. When the concentration of the CH3COOOH solution is greater than 4%, the hydroxyl value of the highly dispersed acetylene carbon black basically no longer changes and shows a stable trend. Therefore, the concentration of the CH3COOOH solution is 3% to 5%; when the concentration of the CH3COOOH solution is constant, the mass ratio of the CH3COOOH solution to the raw material acetylene carbon black is changed. When the mass ratio of the CH3COOOH solution to the raw material acetylene carbon black is 2 to 6:15, the hydroxyl value of the highly dispersed acetylene carbon black shows a gradual increasing trend. When the mass ratio of the CH3COOOH solution to the raw material acetylene carbon black is greater than 6:15, the hydroxyl value of the highly dispersed acetylene carbon black basically no longer changes;
[0086] Please refer to Table 3 and Figure 3, when the mass ratio of CH3COOOH solution to raw material acetylene carbon black is constant, the concentration of CH3COOOH solution is changed. When the concentration of CH3COOOH solution is 1% to 4%, the resistivity of highly dispersed acetylene carbon black shows a trend of gradually decreasing. When the concentration of CH3COOOH solution is greater than 4%, the resistivity of highly dispersed acetylene carbon black basically no longer changes and shows a stable trend. Therefore, the concentration of the CH3COOOH solution is 3% to 5%; when the concentration of CH3COOOH solution is constant, the mass ratio of CH3COOOH solution to raw material acetylene carbon black is changed. When the mass ratio of CH3COOOH solution to raw material acetylene carbon black is 2 to 6:15, the resistivity of highly dispersed acetylene carbon black shows a trend of gradually decreasing. When the mass ratio of CH3COOOH solution to raw material acetylene carbon black is greater than 6:15, the resistivity of highly dispersed acetylene carbon black basically no longer changes;
[0087] Please refer to Table 3 and Figure 4 , when the mass ratio of CH3COOOH solution to raw material acetylene carbon black is 2:15 and 8:15, and the concentration of CH3COOOH solution is greater than 3%, compared with the mass ratio of CH3COOOH solution to raw material acetylene carbon black being 4:15 and 6:15, and the concentration of CH3COOOH solution being greater than 3%, the dispersion stability value of the prepared highly dispersible acetylene carbon black is low. Meanwhile, when the mass ratio of CH3COOOH solution to raw material acetylene carbon black is 4 to 6:15, and the concentration of CH3COOOH solution is greater than 3%, the dispersion stability value of the prepared highly dispersible acetylene carbon black is significantly weak;
[0088] In combination with the experimental data in the chart, when the mass ratio of CH3COOOH solution to raw material acetylene carbon black is greater than 6:15, the dispersion value, hydroxyl value, resistivity and dispersion stability of the obtained high-dispersion acetylene carbon black basically do not change. In other words, when the proportion of CH3COOOH solution is relatively large, the same treatment method basically does not affect the performance of high-dispersion acetylene carbon black. Therefore, in order to save costs and resources, the preferred mass ratio of raw material acetylene carbon black to CH3COOOH solution is 4 to 6:15, preferably 6:15;
[0089] Similarly, when the concentration of the CH3COOOH solution is greater than 5%, the dispersibility value, hydroxyl value, resistivity and dispersion stability of the high-dispersibility acetylene black basically do not change. Therefore, the concentration of the CH3COOOH solution is selected to be 3% to 5%, preferably 5%.
[0090] 7. Example 3: Optimization of CH3COOOH solution temperature
[0091] The difference between this embodiment 3 and the above embodiment 1 is that: the temperature of the CH3COOOH solution is changed, and the raw material acetylene carbon black is mixed with the CH3COOOH solutions of different temperatures to form a mixture. The other steps are the same as those in the above embodiment 1. The temperature of the CH3COOOH solution is specifically shown in Table 4:
[0092] Table 4 Temperature of CH3COOOH solution
[0093]
[0094] After the experiment, the hydroxyl value, resistivity, dispersibility and dispersion stability of the highly dispersible acetylene carbon black prepared in the 25th group and the 26th group were detected and calculated respectively. The specific results are shown in Table 5:
[0095] Table 5 Experimental results of Example 3
[0096]
[0097] It can be seen from the data in Table 5 that when the temperature of the CH3COOOH solution is 60°C, the hydroxyl value of the obtained highly dispersed acetylene carbon black is 0.29 mgKOH / g, the resistivity is 1.4Ω·m, and the dispersibility value is 17.0; when the temperature of the CH3COOOH solution is 90°C, the hydroxyl value of the obtained highly dispersed acetylene carbon black is 0.30 mgKOH / g, the resistivity is 1.4Ω·m, and the dispersibility value is 17.2; all the data are not as good as the data when the temperature of the CH3COOOH solution is 75°C in Example 1;
[0098] It can be seen that the temperature of the CH3COOOH solution has an influence on the dispersibility, dispersion stability and conductivity of the highly dispersible acetylene carbon black, but the influence is not significant. When the temperature of the CH3COOOH solution is 75°C, the dispersibility and conductivity of the prepared highly dispersible acetylene carbon black are better.
[0099] In addition, it has been verified that at a voltage of 380V, the highly dispersed acetylene carbon black can also be successfully prepared by the method provided by the present invention, and the dispersion value, hydroxyl value, resistivity and dispersion stability of the highly dispersed acetylene carbon black prepared at a voltage of 380V are basically the same as the dispersion value, hydroxyl value, resistivity and dispersion stability of the highly dispersed acetylene carbon black prepared at a voltage of 220V in the above Example 1, but the high voltage of 380V consumes energy. Therefore, on the premise of achieving the same effect, it is preferred to use a voltage of 220V to prepare the highly dispersed acetylene carbon black.
[0100] The above description is only a specific implementation mode of the present invention, but the protection scope of the present invention is not limited thereto. Any technician familiar with the technical field can easily think of various equivalent modifications or substitutions within the technical scope disclosed by the present invention, and these modifications or substitutions should be included in the protection scope of the present invention.
Claims
1. A method for preparing highly dispersible acetylene carbon black, characterized in that: The following steps are involved: Mixing raw material acetylene carbon black with CH3COOOH solution to form a mixture; wherein the mass ratio of CH3COOOH to the raw material acetylene carbon black is (4 to 6):15; The mixed material is subjected to a conductive treatment to prepare highly dispersed acetylene carbon black.
2. The method for preparing highly dispersible acetylene black according to claim 1, characterized in that: The "conductive treatment of the mixture to prepare highly dispersed acetylene carbon black" comprises the following steps: Provided is a conductive container, the conductive container comprising at least one carbon black modified cylinder, both ends of the carbon black modified cylinder being provided with a cover body, the cover body being provided with a conductive column, and the conductive column being capable of connecting to a power source; Introducing the mixed material into the carbon black modified cylinder, covering the cover body, and making the conductive column contact with the mixed material; The power-on state is maintained for a first preset time, and the cover is opened to obtain the highly dispersed acetylene carbon black.
3. The method for preparing highly dispersible acetylene carbon black according to claim 2, characterized in that: In the "first preset time period for maintaining the power-on state", the power-on voltage is 220 V to 380 V.
4. The method for preparing highly dispersible acetylene black according to claim 2, characterized in that: In the "maintaining the power-on state for the first preset time", the power-on state is maintained until the current in the circuit is constant.
5. The method for preparing highly dispersible acetylene black according to claim 1, characterized in that: The mass concentration of the CH3COOOH solution is 3% to 5%.
6. The method for preparing highly dispersible acetylene black according to claim 1, characterized in that: The temperature of the CH3COOOH solution is 60°C to 90°C.
7. The method for preparing highly dispersible acetylene black according to claim 1, characterized in that: The average particle size of the raw material acetylene carbon black is 30nm to 45nm, and the specific surface area is 55 m 2 / g to 70 m 2 / g, oxygen content is 0.07% to 0.26%, pH value is 5 to 7, and resistivity is 3Ω·m to 5Ω·m.
8. The method for preparing highly dispersible acetylene black according to claim 1, characterized in that: The method also includes drying the prepared highly dispersed acetylene carbon black.
9. A highly dispersible acetylene carbon black particle, characterized in that: Prepared by the following method: Prepare highly dispersed acetylene carbon black by the method for preparing highly dispersed acetylene carbon black according to any one of claims 1 to 7, and dry it; The dried highly dispersible acetylene carbon black is impregnated with water, and then granulated to obtain highly dispersible acetylene carbon black particles.
10. A highly dispersible acetylene carbon black particle, characterized in that: Prepared by the following method: Using CH3COOOH solution to perform impregnation treatment on the raw material acetylene carbon black, wherein the mass ratio of CH3COOOH solution to the raw material acetylene carbon black is (4 to 6):15, and the mass concentration of CH3COOOH solution is 3% to 5%; Conducting conductive treatment on the raw material acetylene carbon black after impregnation treatment; The raw material acetylene black after the conductive treatment is granulated and dried to obtain highly dispersed acetylene black particles.
Citation Information
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