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CN-121994671-A - Method for testing specific surface area of white carbon black

CN121994671ACN 121994671 ACN121994671 ACN 121994671ACN-121994671-A

Abstract

The invention provides a method for testing the specific surface area of white carbon black. S1, taking a part of white carbon black to be tested as a white carbon black sample, testing the specific surface area of the white carbon black by a nitrogen adsorption method, and calculating according to a formula (I) to obtain a sample weighing amount: (I) The method comprises the steps of (1) measuring the specific surface area of a white carbon black sample by a nitrogen adsorption method, wherein x is the unit of m 2 /g, y is the unit of g, S2 is the unit of g, the other part of white carbon black to be measured is weighed by the unit of g, the other part of white carbon black to be measured is mixed with cetyltrimethylammonium bromide solution to obtain suspension, S3 is subjected to solid-liquid separation treatment to obtain supernatant, S4 is used for diluting the supernatant and carrying out potential titration by adopting sodium dioctyl sulfosuccinate solution, the volume consumption of the sodium dioctyl sulfosuccinate solution is recorded after the titration end point is reached, and the specific surface area of the white carbon black to be measured is calculated and is recorded as S CTAB .

Inventors

  • SHENG LIPING
  • LIU XUEJIAO

Assignees

  • 思通检测技术有限公司

Dates

Publication Date
20260508
Application Date
20260120

Claims (10)

  1. 1. The method for testing the specific surface area of the white carbon black is characterized by comprising the following steps of: Step S1, taking a part of white carbon black to be detected as a white carbon black sample, testing the specific surface area of the white carbon black by a nitrogen adsorption method, and calculating according to a formula (I) to obtain a sample weighing amount: (I) Wherein x is the specific surface area of the white carbon black sample measured by adopting the nitrogen adsorption method, and the unit is m 2 /g; S2, weighing the other part of the white carbon black to be measured according to the sample weighing amount, and mixing the white carbon black to be measured with a cetyltrimethylammonium bromide solution to obtain a suspension; S3, carrying out solid-liquid separation treatment on the suspension to obtain a supernatant; and S4, diluting the supernatant, carrying out potential titration by adopting a dioctyl sodium sulfosuccinate solution, recording the volume consumption of the dioctyl sodium sulfosuccinate solution after the titration end point is reached, and calculating to obtain the specific surface area of the white carbon black to be detected, wherein the specific surface area is recorded as S CTAB .
  2. 2. The method for testing the specific surface area of white carbon black according to claim 1, wherein x is more than or equal to 60m 2 /g.
  3. 3. The method for testing the specific surface area of white carbon black according to claim 1, wherein x is more than or equal to 250m 2 /g; Preferably, x is any one of the values of 250-420 m 2 /g.
  4. 4. The method according to any one of claims 1 to 3, wherein in the step S2, the cetyltrimethylammonium bromide solution has a volume of 30mL and a molar concentration of 0.0151mol/L.
  5. 5. The method for testing the specific surface area of white carbon black according to claim 4, wherein stirring is performed in the mixing process in the step S2, the stirring time is 35-50 min, and the stirring rotating speed is 400-600 r/min.
  6. 6. The method for testing the specific surface area of white carbon black according to claim 5, wherein the solid-liquid separation treatment is a centrifugal treatment, preferably the rotation speed is 4000-9000 r/min, and the time is 20-60 min.
  7. 7. The method according to claim 4 or 5, wherein the step S3 further comprises a filtering process.
  8. 8. The method according to any one of claims 1 to 7, wherein the step S4 includes: Taking 5mL of the supernatant, diluting the supernatant with water to 25-70 mL to obtain a solution to be tested, titrating the solution to be tested by adopting part of the dioctyl sodium sulfosuccinate solution until the titration is finished, and recording the volume consumption V of the solution to be tested, wherein the unit is mL; 2.5mL of the cetyltrimethylammonium bromide solution is taken, and diluted to 25-70 mL by water to obtain a blank control solution, the rest of the sodium dioctyl sulfosuccinate solution is adopted to titrate the blank control solution until the titration is ended, and the volume consumption amount V 0 is recorded, wherein the unit is mL; Calculating by adopting a formula (II) to obtain the specific surface area of the white carbon black to be detected: and (II), wherein y is the sample weighing amount, the unit is g, X is the mass ratio of the white carbon black to be measured lost after the white carbon black to be measured is heated to constant weight at 105 ℃, the unit is 1, and the unit of S CTAB is m 2 /g.
  9. 9. The method for testing the specific surface area of white carbon black according to claim 8, wherein the molar concentration of the dioctyl sodium sulfosuccinate solution is 0.00389mol/L.
  10. 10. The method according to claim 8, wherein the volume of the test solution obtained after dilution in the step S4 is 60mL, and/or the volume of the blank solution obtained after dilution is 60mL.

Description

Method for testing specific surface area of white carbon black Technical Field The invention relates to a specific surface area of white carbon black, in particular to a method for testing the specific surface area of white carbon black. Background In recent years, with the development of green tires, the application of white carbon black is more and more, and according to the different types of white carbon black with specific surface area, in order to improve the wear resistance of the tire, many white carbon blacks with high specific surface area are generated, and the specific surface area can reach three hundred square meters per gram or even higher. The current test principle of white carbon black CTAB is that Cetyl Trimethyl Ammonium Bromide (CTAB) solution is added into a precipitated hydrated silica sample to be tested, the solution is dispersed to be balanced through mechanical oscillation, CTAB is adsorbed by the sample to form suspension, the suspension is centrifugally separated, the amount of non-adsorbed CTAB is titrated by a turbidimeter, and the specific surface area of a dry sample can be obtained through calculation. However, the sample size requirements for the CTAB test of white carbon black in the related art no longer meet the CTAB specific surface area test requirements of precipitation-process white carbon black with high specific surface area. Furthermore, the testing of CTAB specific surface area depends on proper sample weighing. If the sample is too high, the added CTAB macromolecules are all or mostly adsorbed on the surface of the white carbon black, and the residual CTAB macromolecules which react with the OT (dioctyl sodium sulfosuccinate) solution in a titration way have low or almost no content, so that the test result is abnormal, if the sample is too low, the CTAB macromolecules adsorbed on the surface of the white carbon black are less, and most of the CTAB macromolecules are separated and then react with the OT solution in a titration way, so that the OT consumed in each test is more, the test time is longer, and the result can be influenced. Therefore, reasonable sample weighing can ensure quick test and accuracy of results. On the basis, research and development of a method capable of improving the accuracy of the white carbon black specific surface area test result are of great significance. Disclosure of Invention The invention mainly aims to provide a method for testing the specific surface area of white carbon black, which aims to solve the problem that the accuracy of the specific surface area test result of the white carbon black in the prior art is to be improved. In order to achieve the above purpose, the invention provides a method for testing specific surface area of white carbon black, comprising the following steps of S1, taking a part of white carbon black to be tested as a white carbon black sample, testing the specific surface area by a nitrogen adsorption method, and calculating according to a formula (I) to obtain a sample weighing amount: (I) The method comprises the steps of (1) measuring the specific surface area of a white carbon black sample by a nitrogen adsorption method, wherein x is the unit of m 2/g, y is the unit of g, step S2 is to measure the other part of white carbon black to be measured by the sample, mixing the other part of white carbon black with cetyltrimethylammonium bromide solution to obtain suspension, step S3 is to conduct solid-liquid separation treatment on the suspension to obtain supernatant, step S4 is to dilute the supernatant and conduct potential titration by adopting dioctyl sodium sulfosuccinate solution, the volume consumption of the dioctyl sodium sulfosuccinate solution is recorded after the titration end point is reached, and the specific surface area of the white carbon black to be measured is calculated and recorded as S CTAB. Further, x is not less than 60m 2/g. Further, x is not less than 250m 2/g. Further, x is any one of the values of 250-420 m 2/g. Further, in step S2, the volume of the cetyltrimethylammonium bromide solution was 30mL, and the molar concentration was 0.0151mol/L. Further, stirring is carried out in the mixing process in the step S2, the stirring time is 35-50 min, and the stirring rotating speed is 400-600 r/min. Further, the solid-liquid separation treatment is centrifugal treatment, preferably the rotation speed is 4000-9000 r/min, and the time is 20-60 min. Further, step S3 further includes a filtering process. Further, the step S4 comprises the steps of taking 5mL of supernatant, diluting to 25-70 mL with water to obtain a liquid to be detected, titrating the liquid to be detected by adopting a part of sodium dioctyl sulfosuccinate solution until the titration is finished, recording the volume consumption amount V of the liquid to be detected as mL, taking 2.5mL of cetyltrimethylammonium bromide solution, diluting to 25-70 mL with water to obtain a blank control solution, titrating th