Preparation method of high dispersibility acetylene carbon black and granule

By treating acetylene black with H2O2 and CH3COOOH solution, followed by slow heating and granulation, the problem of decreased purity after improved dispersibility of acetylene black was solved, achieving high dispersibility and conductivity while maintaining high purity and stability.

CN120005422BActive Publication Date: 2026-08-25NINGXIA JINHAIWORLD TECH CO LTD
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Patent Information

Application Number
CN202411315099.4
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-09-20
Publication Date
2026-08-25
Estimated Expiration
2044-09-20

AI Technical Summary

Technical Problem

In existing technologies, dispersants are added to improve the dispersibility of acetylene black, which leads to a decrease in purity and fails to meet the purity requirements of some products.

Method used

Highly dispersible acetylene black was prepared by mixing H2O2 solution and CH3COOOH solution with acetylene black, slowly heating to 30-40℃ and holding at that temperature for 2-5 hours, followed by drying and granulation.

Benefits of technology

The prepared highly dispersible acetylene carbon black exhibited improved dispersibility to 16.9, reduced resistivity to 1.5 Ω·m, high purity, good stability, and no precipitation or agglomeration.

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Abstract

The application belongs to the technical field of carbon black production, and particularly relates to a high-dispersibility acetylene carbon black preparation method and particles. Raw material acetylene carbon black, H2O2 solution and CH3COOOH solution are mixed to form a mixture; the mass ratio of the H2O2 solution, the CH3COOOH solution and the raw material acetylene carbon black is (2 to 4):(4 to 6):25; the mixture is slowly heated to a predetermined temperature and then kept for a predetermined time to prepare high-dispersibility acetylene carbon black; the dispersibility value of the prepared high-dispersibility acetylene carbon black is 16.9, and the hydroxyl value is 0.34; no dispersant or auxiliary agent is introduced during preparation, the prepared high-dispersibility acetylene carbon black has no impurities and has high purity; the resistivity of the high-dispersibility acetylene carbon black prepared by the method is 1.5 omega*m, and compared with the resistivity 3 omega*m of high-quality acetylene carbon black on the market, the high-dispersibility acetylene carbon black has high dispersibility and high conductivity.
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Description

Technical Field

[0001] This invention belongs to the field of carbon black production technology, specifically relating to a method for preparing highly dispersible acetylene carbon black and its granules. Background Technology

[0002] Acetylene black is a carbon black obtained by continuously pyrolyzing acetylene with a purity of over 99%, which is obtained by decomposing and refining acetylene, a byproduct of the pyrolysis of calcium carbide or naphtha (crude gasoline). Compared with furnace black, it has a more developed crystal structure and secondary structure, resulting in better electrical conductivity and liquid absorption. Due to its lower levels of heavy metals and other impurities, it suffers less loss due to self-discharge. It is mainly used as the negative electrode in nickel-metal hydride batteries and can also be used as a conductor in supercapacitors.

[0003] Currently, 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 CN201380047462.2 discloses an acetylene black dispersion slurry and a lithium-ion secondary battery. To improve the dispersibility of acetylene black, a dispersant is added to it, which can increase the dispersibility value of acetylene black to about 17 and the resistivity to 3 Ω·m, thus making it easier for acetylene black to disperse in the dispersion medium and improving its dispersibility. However, because a dispersant is added to acetylene black, impurities are indirectly introduced, reducing the purity of acetylene black and resulting in low purity that does not meet the requirements of some products. Summary of the Invention

[0004] In view of this, the present invention provides a method for preparing highly dispersible acetylene black and granules to solve the technical problem in the prior art where adding dispersing aids to improve the dispersibility of acetylene black indirectly introduces impurities, reducing the purity of acetylene black and resulting in low purity that does not meet the requirements of some products.

[0005] To achieve the above objectives, this application adopts the following approach:

[0006] A method for preparing highly dispersible acetylene black includes the following steps:

[0007] Raw material acetylene black, H2O2 solution and CH3COOOH solution are mixed to form a mixture; wherein the mass ratio of H2O2 solution, CH3COOOH solution and raw material acetylene black is (2 to 4):(4 to 6):25; the mixture is slowly heated to a predetermined temperature and then kept at that temperature for a predetermined time to prepare highly dispersible acetylene black.

[0008] Preferably, the predetermined temperature is 30°C to 40°C.

[0009] Preferably, the predetermined time is 2 hours to 5 hours.

[0010] Preferably, the mass concentration of the H2O2 solution is 3 wt% to 5 wt%.

[0011] Preferably, the mass concentration of the CH3COOOH solution is 1 wt% to 2 wt%.

[0012] Preferably, the mass ratio of the H2O2 solution, the CH3COOOH solution, and the raw material acetylene black is 4:6:25.

[0013] Preferably, the acetylene black raw material has an average particle size of 30 nm to 45 nm and a specific surface area of ​​55 m². 2 / g to 70m 2 / g, oxygen content of 0.07% to 0.26%, pH value of 5 to 7, resistivity of 3 Ω·m to 5 Ω·m.

[0014] Preferably, in the step of "slowly heating the mixture to a predetermined temperature and then holding it at that temperature for a predetermined time", the heating rate is 10°C / h to 15°C / h.

[0015] A highly dispersible acetylene carbon black particle is prepared by the following method:

[0016] Highly dispersible acetylene black is prepared by the above-described method and dried; the dried highly dispersible acetylene black is then impregnated with water and granulated to obtain highly dispersible acetylene black particles.

[0017] A highly dispersible acetylene carbon black particle is prepared by the following method:

[0018] Acetylene black is impregnated with H2O2 solution and CH3COOOH solution, wherein the mass ratio of H2O2 solution, CH3COOOH solution and acetylene black is (2 to 4):(4 to 6):25, the mass concentration of H2O2 solution is 3 wt% to 5 wt%, and the mass concentration of CH3COOOH solution is 1 wt% to 2 wt%. The impregnated acetylene black is then slowly heated to a predetermined temperature and held at that temperature for a predetermined time to prepare highly dispersible acetylene black, wherein the predetermined temperature is 30°C to 40°C and the predetermined time is 2 to 5 hours. The highly dispersible acetylene black is then granulated and dried to obtain highly dispersible acetylene black granules.

[0019] The technical solution adopted in this application has at least the following beneficial effects:

[0020] 1. This application provides a method for preparing highly dispersible acetylene black. The method involves mixing the raw acetylene black with an H2O2 solution and a CH3COOOH solution in a mixer to form a mixture. The mixture is then slowly heated to a predetermined temperature and held at that temperature for a predetermined time to obtain highly dispersible acetylene black. The mass ratio of the H2O2 solution, the CH3COOOH solution, and the raw acetylene black is (2 to 4):(4 to 6):25. The highly dispersible acetylene black has a dispersibility value of 16.9 and a hydroxyl value of 0.34 mgKOH / g. Compared with the dispersibility value of 8.21 of the raw acetylene black, the highly dispersible acetylene black prepared by the method provided in this application has higher dispersibility. In the process of preparing highly dispersible acetylene black by mixing the raw acetylene black with H2O2 solution and CH3COOOH solution and slowly heating to a predetermined temperature and holding for a predetermined time, no dispersant or auxiliary agent is introduced. Therefore, the highly dispersible acetylene black prepared is free of impurities and has high purity.

[0021] 2. The highly dispersible acetylene carbon black prepared by the method provided in this invention has a resistivity of 1.5 Ω·m, which is higher than the resistivity of 3 Ω·m of high-quality acetylene carbon black on the market. It has both high dispersibility and high conductivity.

[0022] 3. When the prepared highly dispersible acetylene black was left to stand in room temperature water for 15 days, there was no precipitation, no stratification, and no agglomeration. In contrast, the raw acetylene black showed precipitation, stratification, and agglomeration when left to stand in room temperature water for more than 5 days. It can be seen that the method provided in this invention can prepare highly dispersible acetylene black with good stability. Detailed Implementation

[0023] To facilitate understanding of this application, a more comprehensive description of the application will be provided below with reference to embodiments. Preferred embodiments of the application are also given. However, this application can be implemented in many different forms and is not limited to the embodiments described herein. Rather, these embodiments are provided to enable a more thorough and complete understanding of the disclosure of this application.

[0024] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the application. The term "and / or" as used herein includes any and all combinations of one or more of the associated listed items.

[0025] In this embodiment, a method for preparing highly dispersible acetylene black includes: mixing raw acetylene black, H2O2 solution, and CH3COOOH solution to form a mixture; wherein the mass ratio of the H2O2 solution, the CH3COOOH solution, and the raw acetylene black is (2 to 4):(4 to 6):25; slowly heating the mixture to a predetermined temperature and holding it at that temperature for a predetermined time to prepare highly dispersible acetylene black.

[0026] In this embodiment, the raw material acetylene black is acetylene black powder. To prepare highly dispersible acetylene black, the raw material acetylene black is mixed with the H2O2 solution and the CH3COOOH solution in a mixer to form a mixture. The mixture is then slowly heated to a predetermined temperature and held at that temperature for a predetermined time to obtain highly dispersible acetylene black. When the mass ratio of the raw material acetylene black is (2 to 4):(4 to 6):25, the prepared highly dispersible acetylene black exhibits high dispersibility, dispersion stability, and conductivity. The effect is even better when the mass ratio of the H2O2 solution, CH3COOOH solution, and raw material acetylene black is 4:6:25.

[0027] The prepared highly dispersible acetylene black has a dispersibility value of 16.9 and a hydroxyl value of 0.34 mgKOH / g. Compared with the dispersibility value of 8.21 of the raw acetylene black, the highly dispersible acetylene black prepared by the method provided in this application has higher dispersibility. Furthermore, when preparing highly dispersible acetylene black by mixing the raw acetylene black with H2O2 solution for conductive treatment, no dispersant or auxiliary agent is introduced. Therefore, the prepared highly dispersible acetylene black is free of impurities and has high purity. The resistivity of the highly dispersible acetylene black prepared by the method provided in this invention is 1.5 Ω·m, compared with the resistivity of 3 Ω·m of commercially available high-quality acetylene black, exhibiting both high dispersibility and high conductivity. When the prepared highly dispersible acetylene black is left to stand in room temperature water for 15 days, there is no precipitation, no stratification, and no agglomeration. In contrast, the raw acetylene black, when left to stand in room temperature water for more than 5 days, exhibits precipitation, stratification, and agglomeration. This demonstrates that the method provided in this invention can prepare highly dispersible acetylene black with good stability.

[0028] The predetermined temperature is 30°C to 40°C; the predetermined time is 2 hours to 5 hours.

[0029] Specifically, the mass concentration of the H2O2 solution is 3 wt% to 5 wt%, preferably 5 wt%; the mass concentration of the CH3COOOH solution is 1 wt% to 2 wt%, preferably 2 wt%.

[0030] In the above embodiments, the acetylene carbon black raw material has an average particle size of 30 nm to 45 nm and a specific surface area of ​​55 m². 2 / g to 70m2 / g, oxygen content of 0.07% to 0.26%, pH value of 5 to 7, resistivity of 3 Ω·m to 5 Ω·m.

[0031] Preferably, in the step of "slowly heating the mixture to a predetermined temperature and then holding it at that temperature for a predetermined time", the heating rate is 10°C / h to 15°C / h.

[0032] A highly dispersible acetylene carbon black particle is prepared by the following method:

[0033] Highly dispersible acetylene black is prepared by the above-described method and dried; the dried highly dispersible acetylene black is then impregnated with water and granulated to obtain highly dispersible acetylene black particles.

[0034] The highly dispersible acetylene black prepared by the method provided in this invention is dried until the moisture content reaches the conventional limit, thus obtaining dried highly dispersible acetylene black. Then, the dried highly dispersible acetylene black is soaked in water for a period of time and then granulated to obtain highly dispersible acetylene black particles with high purity and high conductivity.

[0035] A highly dispersible acetylene carbon black particle is prepared by the following method:

[0036] Acetylene black is impregnated with H2O2 solution and CH3COOOH solution, wherein the mass ratio of H2O2 solution, CH3COOOH solution and acetylene black is (2 to 4):(4 to 6):25, the mass concentration of H2O2 solution is 3 wt% to 5 wt%, and the mass concentration of CH3COOOH solution is 1 wt% to 2 wt%. The impregnated acetylene black is then slowly heated to a predetermined temperature and held at that temperature for a predetermined time to prepare highly dispersible acetylene black, wherein the predetermined temperature is 30°C to 40°C and the predetermined time is 2 to 5 hours. The highly dispersible acetylene black is then granulated and dried to obtain highly dispersible acetylene black granules.

[0037] In preparing highly dispersible acetylene black particles, firstly, the raw acetylene black is impregnated with the H2O2 solution and CH3COOOH solution. Preferably, the mass ratio of the H2O2 solution, the CH3COOOH solution, and the raw acetylene black is 4:6:25, the mass concentration of the H2O2 solution is 5wt%, and the mass concentration of the CH3COOOH solution is 2wt%. Then, preferably, the impregnated raw acetylene black is slowly heated to 35°C, held at that temperature for 3.5 hours, and then granulated and dried to obtain highly dispersible acetylene black particles with high purity and high conductivity.

[0038] The following specific experimental examples further illustrate the technical solution and effects of the present invention. It should be noted that the following experimental examples are only for further explanation of the present invention and do not limit the technical solution of the present invention.

[0039] 1. Experimental Materials and Methods

[0040] 1.1 Experimental Materials

[0041] The raw materials are acetylene black, H2O2 solution, and CH3COOOH solution. The acetylene black is from Ningxia Jinhai Wode Technology Co., Ltd., and the H2O2 solution and CH3COOOH solution are commercially available.

[0042] 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 precipitates when left to stand in room temperature water for more than 5 days.

[0043] 1.2 Experimental Methods

[0044] The experiment was divided into 11 treatment groups: Comparative Example 1, Comparative Example 2, Comparative Example 3, Comparative Example 4, Comparative Example 5, Example 1, Example 2, Example 3, Example 4, Example 5, and Example 6. Acetylene black (dried acetylene black) was prepared from each of the 11 treatment groups, and its parameters were measured according to the following detection methods:

[0045] According to the patent number: CN201710367601.X, entitled "Detection method for carbon black dispersibility provided in determining carbon black dispersibility using blackness distribution curve", the dispersibility value of the acetylene carbon black treated in the following examples was detected.

[0046] The resistivity of the treated acetylene black was measured using an acetylene black resistivity meter (domestic TBY-30 model).

[0047] The hydroxyl value of the treated acetylene black was determined by gas chromatography.

[0048] The treated acetylene black was placed in room temperature water for different durations to test its dispersion stability.

[0049] 2. Comparative Example 1: Heat treatment of raw material acetylene black

[0050] The raw material acetylene black was slowly heated to 35℃ and held at that temperature for 3.5 h. The heating rate was 13℃ / h. After the holding period, the treated acetylene black was obtained. Its dispersibility, hydroxyl value and dispersion stability were tested. The results are shown in Table 1.

[0051] 3. Comparative Example 2: Heat treatment of the mixture (raw materials: acetylene black and water)

[0052] The difference between Comparative Example 2 and Comparative Example 1 above is that water and raw material acetylene black are mixed at a mass ratio of 10:25 to form a mixture. The mixture is slowly heated and then dried. Other steps are the same as those in Comparative Example 1 above. The results are shown in Table 1.

[0053] 4. Comparative Example 3: The mixture (raw materials: acetylene black, H2O2 solution, CH3COOOH solution) was not heated.

[0054] The difference between Comparative Example 3 and Comparative Example 1 above is that: H2O2 solution, CH3COOOH solution and raw material acetylene black were mixed in a mass ratio of 4:6:25 to form a mixture. The mass concentration of H2O2 solution was 5wt% and the mass concentration of CH3COOOH solution was 2wt%. After standing for 3.5h without heating treatment, the treated acetylene black was obtained after drying. The results are shown in Table 1.

[0055] 5. Comparative Example 4: Heat treatment of the mixture (raw materials: acetylene black and H2O2 solution)

[0056] The difference between Comparative Example 4 and Comparative Example 1 above is that: H2O2 solution and raw material acetylene carbon black were mixed at a mass ratio of 4:25 to form a mixture. The mass concentration of H2O2 solution was 5wt%. The mixture was slowly heated and then dried. Other steps were the same as those in Comparative Example 1 above. The results are shown in Table 1.

[0057] 6. Comparative Example 5: Heat treatment of the mixture (raw materials: acetylene black and CH3COOOH solution)

[0058] The difference between Comparative Example 5 and Comparative Example 1 above is that: CH3COOOH solution and raw material acetylene black are mixed at a mass ratio of 6:25 to form a mixture. The mass concentration of CH3COOOH solution is 2wt%. The mixture is slowly heated and then dried. Other steps are the same as those in Comparative Example 1 above. The results are shown in Table 1.

[0059] 7. Example 1: Heat treatment of the mixture (raw materials: acetylene black, H2O2 solution, CH3COOOH solution)

[0060] The difference between Example 1 and Comparative Example 1 is that: H2O2 solution, CH3COOOH solution, and raw material acetylene black were mixed in a mass ratio of 4:6:25 to form a mixture. The mass concentration of H2O2 solution was 5wt%, and the mass concentration of CH3COOOH solution was 2wt%. The mixture was slowly heated, and then dried. Other steps were the same as those in Comparative Example 1. The results are shown in Table 1.

[0061] Table 1 Experimental Results Detection Table

[0062]

[0063] As can be seen from the data in Comparative Example 1 in Table 1 above, when the raw material acetylene black is directly heated, the resulting acetylene black has a dispersibility value of 8.3, a hydroxyl value of 0.2 mg KOH / g, and a resistivity of 3 Ω·m. When acetylene black is left to stand in room temperature water for 6 days, there is slight precipitation. When acetylene black is left to stand in room temperature water for 1 to 5 days, there is no precipitation, no stratification, and no agglomeration.

[0064] As can be seen from the data in Comparative Example 2 in Table 1 above, when raw material acetylene black is mixed with water to form a mixture, and the mixture is heated, the resulting acetylene black has a dispersibility value of 9.2, a hydroxyl value of 0.25 mgKOH / g, and a resistivity of 2.7 Ω·m. When the acetylene black is left to stand in room temperature water for 7 days, slight precipitation occurs.

[0065] As can be seen from the data in Comparative Example 3 in Table 1 above, when H2O2 solution and CH3COOOH solution are mixed with raw material acetylene carbon black to form a mixture, and the treated acetylene carbon black is dried, the dispersibility value is 8.8, the hydroxyl value is 0.23 mgKOH / g, and the resistivity is 2.8 Ω·m. When the acetylene carbon black is left to stand in room temperature water for 6 days, slight precipitation occurs.

[0066] As can be seen from the data in Comparative Examples 4 and 5 in Table 1 above, when H2O2 solution is used alone to mix with raw acetylene carbon black or CH3COOOH solution is used alone to mix with raw acetylene carbon black to form a mixture, and the mixture is slowly heated, the resulting acetylene carbon black has better dispersibility, hydroxyl value, resistivity and dispersion stability than the acetylene carbon black obtained in Comparative Examples 1 to 3.

[0067] As can be seen from the data in Example 1 in Table 1 above, when H2O2 solution and CH3COOOH solution are mixed with raw material acetylene carbon black to form a mixture, and the mixture is slowly heated, the resulting acetylene carbon black has a dispersibility value of 16.9, a hydroxyl value of 0.34 mgKOH / g, and a resistivity of 1.5 Ω·m. When the acetylene carbon black is left to stand in room temperature water for 15 days, there is no precipitation, no stratification, and no agglomeration.

[0068] The data in Table 1 above fully demonstrates that by mixing raw material acetylene black with H2O2 solution and CH3COOOH solution to form a mixture, and then slowly heating the mixture, the resulting acetylene black has a larger hydroxyl value, lower resistivity, higher dispersibility, and better dispersion stability compared to the acetylene black obtained in Comparative Examples 1 to 5. Lower resistivity indicates better conductivity. Therefore, the acetylene black in Example 1 has high dispersibility and conductivity, making it a highly dispersible acetylene black. Furthermore, because only H2O2 solution and CH3COOOH solution were added for heating during preparation to improve the dispersibility of the acetylene black, without the use of other dispersants or additives, the resulting highly dispersible acetylene black is free of impurities and has high purity.

[0069] 8. Example 2: Optimal mass ratio of raw material acetylene black to H2O2 solution

[0070] The difference between Example 2 and Example 1 above is that the mass ratio of raw material acetylene black to H2O2 solution is changed to form a mixture. The mass concentration of H2O2 solution is 5 wt%, and the mass concentration of CH3COOOH solution is 2 wt%. The mixture is slowly heated. Other steps are the same as those in Example 1 above. The specific mass ratio of raw material acetylene black to H2O2 solution is shown in Table 2.

[0071] Table 2 Mass ratio of raw material acetylene black to H2O2 solution

[0072]

[0073] After the experiment, the hydroxyl value, resistivity, dispersibility value, and dispersion stability of the highly dispersible acetylene black after the first to fourth experimental groups were measured respectively. The specific results are shown in Table 3.

[0074] Table 3. Experimental Results Detection Table for Example 2

[0075]

[0076] As can be seen from the data in Table 3 above, when the mass ratio of H2O2 solution, CH3COOOH solution, and raw material acetylene black is 1:6:25, 2:6:25, and 3:6:25, the dispersibility, conductivity, and dispersion stability of the prepared acetylene black are all inferior to those of the acetylene black prepared in Example 1 when the mass ratio of H2O2 solution, CH3COOOH solution, and raw material acetylene black is 4:6:25. When the mass ratio of H2O2 solution, CH3COOOH solution, and raw material acetylene black is 5:6:25, the dispersibility of the prepared acetylene black actually decreases.

[0077] 9. Example 3: Optimal mass ratio of raw material acetylene black to CH3COOOH solution

[0078] The difference between Example 3 and Example 1 above is that the mass ratio of raw material acetylene black to CH3COOOH solution is changed to form a mixture. The mass concentration of H2O2 solution is 5wt%, and the mass concentration of CH3COOOH solution is 2wt%. The mixture is slowly heated. Other steps are the same as those in Example 1 above. The specific mass ratio of raw material acetylene black to CH3COOOH solution is shown in Table 4.

[0079] Table 4. Mass ratio of raw material acetylene black to CH3COOOH solution

[0080]

[0081] After the experiment, the hydroxyl value, resistivity, dispersibility value, and dispersion stability of the highly dispersible acetylene black after the fifth to eighth experimental groups were measured respectively. The specific results are shown in Table 5.

[0082] Table 5. Experimental Results Detection Table for Example 3

[0083]

[0084] As can be seen from the data in Table 5 above, when the mass ratio of H2O2 solution, CH3COOOH solution, and raw material acetylene black is 4:3:25, 4:4:25, and 4:5:25, the dispersibility, conductivity, and dispersion stability of the prepared acetylene black are all inferior to those of the acetylene black prepared in Example 1 when the mass ratio of H2O2 solution, CH3COOOH solution, and raw material acetylene black is 4:6:25. Furthermore, when the mass ratio of H2O2 solution, CH3COOOH solution, and raw material acetylene black is 4:7:25, the dispersibility and conductivity of the prepared acetylene black actually decrease.

[0085] 10. Example 4: Mass concentration of H2O2 solution

[0086] The difference between Example 4 and Example 1 above is that when the mass ratio of raw material acetylene carbon black to H2O2 solution and CH3COOOH solution is 4:6:25, and the mass concentration of CH3COOOH solution is 2wt%, the mass concentration of H2O2 solution is changed. The other steps are the same as in Example 1 above. The specific mass concentration of the H2O2 solution is shown in Table 6.

[0087] Table 6. Mass concentration of H2O2 solution

[0088]

[0089] After the experiment, the hydroxyl value, resistivity, dispersibility value, and dispersion stability of the highly dispersible acetylene black after the ninth to twelfth experimental groups were measured respectively. The specific results are shown in Table 7.

[0090] Table 7. Experimental Results Detection Table for Example 4

[0091]

[0092] As can be seen from the data in Table 7 above, when the mass ratio of H2O2 solution, CH3COOOH solution, and raw material acetylene black is 4:6:25, and the mass concentration of CH3COOOH solution is 2wt%, the dispersibility, conductivity, and dispersion stability of the prepared acetylene black are all inferior to those of the acetylene black prepared when the mass concentration of H2O2 solution is 5wt% in Example 1.

[0093] 11. Example 5: Mass concentration of CH3COOOH solution

[0094] The difference between Example 5 and Example 1 above is that when the mass ratio of raw material acetylene black to H2O2 solution and CH3COOOH solution is 4:6:25, and the mass concentration of H2O2 solution is 5wt%, the mass concentration of CH3COOOH solution is changed. Other steps are the same as in Example 1 above. The specific mass concentration of the CH3COOOH solution is shown in Table 8.

[0095] Table 8. Mass concentration of CH3COOOH solution

[0096]

[0097] After the experiment, the hydroxyl value, resistivity, dispersibility value, and dispersion stability of the highly dispersible acetylene black after the thirteenth and fourteenth experimental groups were measured and calculated. The specific results are shown in Table 9.

[0098] Table 9. Experimental Results Detection Table for Example 5

[0099]

[0100] As can be seen from the data in Table 9 above, when the mass ratio of H2O2 solution, CH3COOOH solution, and raw material acetylene black is 4:6:25, and the mass concentration of H2O2 solution is 5wt%, the dispersibility, conductivity, and dispersion stability of the prepared acetylene black are all inferior to those of the acetylene black prepared when the mass concentration of CH3COOOH solution is 2wt% in Example 1. Since a high mass concentration of CH3COOOH solution can easily cause an explosion, the performance of acetylene black prepared when the mass concentration of CH3COOOH solution is greater than 2wt% will not be investigated further.

[0101] 12. Example 6: The effect of preset temperature on experimental results

[0102] The difference between this embodiment 6 and embodiment 1 above is that the preset temperature is changed when the mixture is slowly heated. The other steps are the same as those in embodiment 1 above. The preset temperature is specifically shown in Table 10.

[0103] Table 10 Preset Temperature Settings

[0104]

[0105] After the experiment, the hydroxyl value, resistivity, dispersibility value, and dispersion stability of the highly dispersible acetylene black after the fifteenth and sixteenth experimental treatments were measured and calculated. The specific results are shown in Table 11.

[0106] Table 11 Experimental Results Detection Table for Example 6

[0107]

[0108] As can be seen from the data in Table 11 above, when the mass ratio of H2O2 solution, CH3COOOH solution, and raw material acetylene black is 4:6:25, the mass concentration of H2O2 solution is 5wt%, and the mass concentration of CH3COOOH solution is 2wt%, and these are mixed to form a mixture, the acetylene black prepared by slowly heating the mixture at preset temperatures of 30℃ and 40℃ has lower dispersibility, conductivity, and dispersion stability than the acetylene black prepared at a preset temperature of 35℃ in Example 1.

[0109] The above description is merely a specific embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any person skilled in the art can easily conceive of various equivalent modifications or substitutions within the technical scope disclosed in the present invention, and such modifications or substitutions should all be covered within the scope of protection of the present invention.

Claims

1. A method for preparing highly dispersible acetylene black, characterized in that, Includes the following steps: A mixture is formed by mixing raw material acetylene black, H2O2 solution, and CH3COOOH solution; wherein the mass ratio of the H2O2 solution, the CH3COOOH solution, and the raw material acetylene black is (3 to 4):6:25, the mass concentration of the H2O2 solution is 3wt% to 5wt%, the mass concentration of the CH3COOOH solution is 1wt% to 2wt%, and the average particle size of the raw material acetylene black is 30nm to 45nm, and the specific surface area is 55 m². 2 / g to 70 m 2 / g, oxygen content of 0.07% to 0.26%, pH value of 5 to 7, resistivity of 3 Ω·m to 5 Ω·m; The mixture is slowly heated to 30°C to 40°C and then kept at that temperature for 2 to 5 hours to prepare highly dispersible acetylene black, wherein the heating rate of the mixture is 10°C / h to 15°C / h.

2. The method for preparing highly dispersible acetylene black according to claim 1, characterized in that, The mass ratio of the H2O2 solution, the CH3COOOH solution, and the raw material acetylene black is 4:6:

25.

3. A highly dispersible acetylene carbon black particle, characterized in that, Prepared by the following method: Highly dispersible acetylene black is prepared by the method for preparing highly dispersible acetylene black according to any one of claims 1 to 2, and then dried. The dried highly dispersible acetylene black was impregnated with water, and then granulated to obtain highly dispersible acetylene black particles.

Citation Information

Patent Citations

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  • Method of measuring dispersibility of carbon black with blackness distribution curve

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  • Method for producing aqueous dispersion of surface-treated carbon black particles and aqueous dispersion of surface-treated carbon black particles

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