阅读说明：本技术 复合分散剂用于协同分散沉淀法白炭黑粉体的工艺 (Process for using composite dispersant for synergistically dispersing white carbon black powder by precipitation method ) 是由 刘雪霆 崔鹏 于 2021-09-06 设计创作，主要内容包括：本发明公开了复合分散剂用于协同分散沉淀法白炭黑粉体的工艺,包括以下步骤：S1：取模数为1,浓度为0.556mol/L的偏硅酸钠水溶液,向该溶液中加入一定质量分数的复合分散剂,即得混合溶液；S2：将步骤S1中的混合溶液加热到55℃后,开始加入浓度为1mol/L的硫酸水溶液,在转速为700转/分钟的情况下调节pH至7,然后把温度调到70℃静止陈化1小时,即得产物；S3：将步骤S2中产物用6000转/分钟的离心机离心8-10分钟,得到的产物在60℃烘箱中进行干燥。本发明使用少量的分散剂就可以显著降低白炭黑的团聚粒径,避免长时间研磨带来的高能耗,噪音和粉尘等问题,显著降低了能耗。(The invention discloses a process for using a composite dispersant to synergistically disperse precipitated white carbon black powder, which comprises the following steps: s1: taking a sodium metasilicate aqueous solution with the modulus of 1 and the concentration of 0.556mol/L, and adding a certain mass fraction of composite dispersant into the solution to obtain a mixed solution; s2: heating the mixed solution in the step S1 to 55 ℃, adding 1mol/L sulfuric acid aqueous solution, adjusting the pH to 7 under the condition that the rotating speed is 700 r/min, then adjusting the temperature to 70 ℃, standing and aging for 1 hour to obtain a product; s3: and (4) centrifuging the product obtained in the step S2 by using a centrifuge of 6000 rpm for 8-10 minutes, and drying the obtained product in an oven at 60 ℃. According to the invention, the agglomerated particle size of the white carbon black can be obviously reduced by using a small amount of the dispersing agent, the problems of high energy consumption, noise, dust and the like caused by long-time grinding are avoided, and the energy consumption is obviously reduced.)

1. The process for using the composite dispersant to synergistically disperse the white carbon black powder by the precipitation method is characterized by comprising the following steps of:

s1: taking a sodium metasilicate aqueous solution with the modulus of 1 and the concentration of 0.556mol/L, and adding a certain mass fraction of composite dispersant into the solution to obtain a mixed solution;

s2: heating the mixed solution in the step S1 to 55 ℃, adding 1mol/L sulfuric acid aqueous solution, adjusting the pH to 7 under the condition that the rotating speed is 700 r/min, then adjusting the temperature to 70 ℃, standing and aging for 1 hour to obtain a product;

s3: and (4) centrifuging the product in the step S2 by using a centrifuge of 6000 rpm for 8-10 minutes, and drying the obtained product in an oven at 60 ℃.

2. The process for preparing white carbon black powder by using the composite dispersant according to claim 1 in a collaborative dispersion precipitation method is characterized in that: the composite dispersant is organic solvent ethanol, wherein the volume ratio of the organic solvent ethanol to water is 10%.

3. The process for preparing white carbon black powder by using the composite dispersant according to claim 1 in a collaborative dispersion precipitation method is characterized in that: the composite dispersant is organic solvent ethanol and cationic dispersant, and the cationic dispersant includes but is not limited to cetyl trimethyl ammonium bromide;

wherein the volume ratio of the organic solvent ethanol to the water is 10 percent, and the mass ratio of the cationic dispersant cetyl trimethyl ammonium bromide is 0.53 percent.

4. The process for preparing white carbon black powder by using the composite dispersant according to claim 1 in a collaborative dispersion precipitation method is characterized in that: the composite dispersant is organic solvent ethanol and anionic dispersant, and the anionic dispersant comprises but is not limited to sodium dodecyl benzene sulfonate;

wherein the volume ratio of the organic solvent ethanol to the water is 10 percent, and the mass ratio of the anionic dispersant sodium dodecyl benzene sulfonate is 0.53 percent.

5. The process for preparing white carbon black powder by using the composite dispersant according to claim 1 in a collaborative dispersion precipitation method is characterized in that: the composite dispersant is organic solvent ethanol and polymer dispersant, and the polymer dispersant is polyacrylamide;

wherein the volume ratio of the organic solvent ethanol is 10 percent, and the mass ratio of the polymer dispersant polyacrylamide is 0.53 percent.

6. The process for preparing white carbon black powder by using the composite dispersant according to claim 1 in a collaborative dispersion precipitation method is characterized in that: the composite dispersant is organic solvent ethanol and polymer dispersant, and the polymer dispersant is polyvinylpyrrolidone;

wherein the volume ratio of the organic solvent ethanol is 10 percent, and the mass ratio of the polymer dispersant polyvinylpyrrolidone is 0.53 percent.

7. The process for preparing white carbon black powder by using the composite dispersant according to claim 1 in a collaborative dispersion precipitation method is characterized in that: the composite dispersant is organic solvent ethanol, anionic dispersant and polymer dispersant, wherein the anionic dispersant is sodium dodecyl benzene sulfonate, and the polymer dispersant is polyvinylpyrrolidone;

wherein the volume ratio of the organic solvent ethanol is 10 percent, and the mass ratio of the sodium dodecyl benzene sulfonate and the polyvinylpyrrolidone is 1.21 percent.

Technical Field

The invention relates to the technical field of white carbon black, in particular to a process for using a composite dispersant for synergistically dispersing white carbon black powder by a precipitation method.

Background

With the development of society, the safety and environmental protection awareness of consumers is improved, and higher requirements are put forward on the performances of tires, so that tire manufacturers are inevitably required to continuously optimize and improve the performances of the tires, such as wet land holding capacity, rolling resistance reduction, wear resistance and the like.

White carbon black has been rapidly developed in recent years as an important reinforcing agent in rubber materials, and has been particularly regarded as a reinforcing filler for tire tread rubber. Because the surface of the white carbon black has a large number of hydroxyl groups, when the white carbon black is used for the tread, the hydroxyl groups can interact with water molecules on the road surface, the combination with the road surface on a wet and slippery road surface is facilitated, the wet grip is improved, meanwhile, the use of the white carbon black can also improve the rolling resistance, the abrasion and the traction performance of the tire, and the tire performance is obviously improved by using the tread comprising the white carbon black disclosed in the patent EP 0853010. Applications in the tire industry include heavy duty tires, passenger car tires, agricultural tires, and the like. In the traditional bias tire, the white carbon black can improve the tear resistance of the tire tread and the adhesive capacity between rubber and a cord. With the increasing requirements on tire meridionization, environmental protection, energy conservation and comfort, the application of white carbon black in tires is more and more important. At present, in the aspects of improving the ground gripping performance of tires, reducing rolling resistance, enhancing the requirements on wear resistance and the like, the rubber formula using white carbon black and carbon black together shows excellent performance. Meanwhile, white carbon black is used for replacing traditional carbon black in the formula to produce green tires, and the production of the green tires becomes a consensus of tire enterprises.

However, there are still some problems with current white carbon filled compounds: the strong interaction exists among white carbon black particles, and the surface treatment of most of the white carbon black particles with medium price is imperfect, so that the white carbon black is difficult to process, difficult to disperse and poor in compatibility with the common rubber of tread rubber. Due to the characteristics, the white carbon black sizing material has poor process performance, the viscosity of the unvulcanized sizing material is improved, the vulcanization speed is delayed, and a coupling agent is usually used for improving the dispersion effect, but the problems of cost increase and the like are caused. Therefore, the composite dispersing agent is urgently needed to be better dispersed in the using process of the white carbon black, the agglomeration phenomenon of the white carbon black prepared by a precipitation method is effectively reduced, the interaction among white carbon black filler particles is reduced, and the dispersion of the particles is promoted by various interactions of the composite dispersing agent and the filler, so that the processing performance of the white carbon black is improved, and the use cost is reduced.

Therefore, the inventor aims to provide a process for using the composite dispersant to synergistically disperse precipitated silica powder so as to achieve the purpose of higher practical value by taking full consideration of the abundant design development and actual manufacturing experience of the related industry for years and researching and improving the existing structure and defects.

Disclosure of Invention

In order to solve the problems mentioned in the background art, the invention provides a process for using a composite dispersant to synergistically disperse precipitated silica powder.

In order to achieve the purpose, the invention adopts the following technical scheme:

the process of using the composite dispersant for synergistically dispersing the white carbon black powder by the precipitation method comprises the following steps:

s1: taking a sodium metasilicate aqueous solution with the modulus of 1 and the concentration of 0.556mol/L, and adding a certain mass fraction of composite dispersant into the solution to obtain a mixed solution;

s2: heating the mixed solution in the step S1 to 55 ℃, adding 1mol/L sulfuric acid aqueous solution, adjusting the pH to 7 under the condition that the rotating speed is 700 r/min, then adjusting the temperature to 70 ℃, standing and aging for 1 hour to obtain a product;

s3: and (4) centrifuging the product in the step S2 by using a centrifuge of 6000 rpm for 8-10 minutes, and drying the obtained product in an oven at 60 ℃.

Preferably, the composite dispersant is organic solvent ethanol, wherein the volume ratio of the organic solvent ethanol to the water is 10%.

Preferably, the composite dispersant is an organic solvent ethanol and a cationic dispersant, and the cationic dispersant includes but is not limited to cetyl trimethyl ammonium bromide;

wherein the volume percentage of the organic solvent ethanol is 10 percent, and the mass percentage of the cationic dispersant cetyl trimethyl ammonium bromide is 0.53 percent.

Preferably, the composite dispersant is an organic solvent ethanol and an anionic dispersant, and the anionic dispersant includes but is not limited to sodium dodecyl benzene sulfonate;

wherein the volume of the organic solvent ethanol accounts for 10 percent, and the mass of the anionic dispersant sodium dodecyl benzene sulfonate accounts for 0.53 percent.

Preferably, the composite dispersant is organic solvent ethanol and polymer dispersant, and the polymer dispersant is polyacrylamide;

wherein the volume ratio of the organic solvent ethanol is 10 percent, and the mass ratio of the polymer dispersant polyacrylamide is 0.53 percent.

Preferably, the composite dispersant is organic solvent ethanol and polymer dispersant, and the polymer dispersant is polyvinylpyrrolidone;

wherein the volume ratio of the organic solvent ethanol is 10 percent, and the mass ratio of the polymer dispersant polyvinylpyrrolidone is 0.53 percent.

Preferably, the composite dispersant is an organic solvent ethanol, an anionic dispersant and a polymer dispersant, wherein the anionic dispersant is sodium dodecyl benzene sulfonate, and the polymer dispersant is polyvinylpyrrolidone;

wherein the volume ratio of the organic solvent ethanol is 10 percent, and the mass ratio of the sodium dodecyl benzene sulfonate and the polyvinylpyrrolidone is 1.21 percent.

Compared with the prior art, the invention has the beneficial effects that:

the composite dispersant system designed by the invention can effectively reduce the agglomeration phenomenon of the precipitated white carbon black, the agglomeration particle size and the agglomeration degree of the white carbon black can be continuously reduced by utilizing the synergistic effect of various dispersants, a feasible thought is provided for solving the industrial problem that the agglomeration phenomenon in the production of the precipitated white carbon black is difficult to overcome, the agglomerated median particle size of the prepared product is reduced to below 10 mu m, the primary particle size is about 20nm, the service performance requirements of the white carbon black in the emerging high-end fields of green tires, transparent heat-resistant silicon rubber and the like can be remarkably improved, and the grade and the application field of the product are improved. According to the invention, a small amount of dispersant is used to effectively disperse the white carbon black particles, so that the problems of high energy consumption, noise, dust and the like caused by long-time grinding method for preparing the dispersible white carbon black are avoided, and the energy consumption is obviously reduced.

Drawings

In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.

FIG. 1 is a TEM analysis of example 1 of the present invention;

FIG. 2 is a TEM analysis chart of example 2 of the present invention;

FIG. 3 is a TEM analysis chart of example 3 of the present invention;

FIG. 4 is a TEM analysis chart of example 4 of the present invention;

FIG. 5 is a TEM analysis chart of example 5 of the present invention;

FIG. 6 is a TEM analysis of example 6 of the present invention;

FIG. 7 is a TEM analysis of comparative example 1 of the present invention;

Detailed Description

In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

Example 1

Referring to fig. 1, the process of using the composite dispersant for synergistically dispersing precipitated silica white powder comprises the following steps:

s1: taking a sodium metasilicate solution with the modulus of 1 and the concentration of 0.556mol/L, and adding a certain mass fraction of a composite dispersant into the solution to obtain a mixed solution;

s2: heating the mixed solution in the step S1 to 55 ℃, adding 1mol/L sulfuric acid aqueous solution, adjusting the pH to 7 under the condition that the rotating speed is 700 r/min, then adjusting the temperature to 70 ℃, standing and aging for 1 hour to obtain a product;

s3: and (4) centrifuging the product in the step S2 by using a centrifuge of 6000 rpm for 8-10 minutes, and drying the obtained product in an oven at 60 ℃.

The composite dispersant is organic solvent ethanol, wherein the volume percentage of the organic solvent ethanol is 10%.

Example 2

Referring to fig. 2, the process of using the composite dispersant for synergistically dispersing precipitated silica white powder comprises the following steps:

s1: taking a sodium metasilicate solution with the modulus of 1 and the concentration of 0.556mol/L, and adding a certain mass fraction of a composite dispersant into the solution to obtain a mixed solution;

s2: heating the mixed solution in the step S1 to 55 ℃, adding sulfuric acid with the concentration of 1mol/L, adjusting the pH to 7 under the condition that the rotating speed is 700 r/min, then adjusting the temperature to 70 ℃, standing and aging for 1 hour to obtain a product;

s3: and (4) centrifuging the product in the step S2 by using a centrifuge of 6000 rpm for 8-10 minutes, and drying the obtained product in an oven at 60 ℃.

The composite dispersant is organic solvent ethanol and cationic dispersant, and the cationic dispersant is cetyl trimethyl ammonium bromide;

wherein the volume percentage of the organic solvent ethanol is 10 percent, and the mass percentage of the cationic dispersant cetyl trimethyl ammonium bromide is 0.53 percent.

Example 3

Referring to fig. 3, the process of using the composite dispersant for synergistically dispersing precipitated silica white powder comprises the following steps:

s1: taking a sodium metasilicate solution with the modulus of 1 and the concentration of 0.556mol/L, and adding a certain mass fraction of a composite dispersant into the solution to obtain a mixed solution;

s2: heating the mixed solution in the step S1 to 55 ℃, adding sulfuric acid with the concentration of 1mol/L, adjusting the pH to 7 under the condition that the rotating speed is 700 r/min, then adjusting the temperature to 70 ℃, standing and aging for 1 hour to obtain a product;

s3: and (4) centrifuging the product in the step S2 by using a centrifuge of 6000 rpm for 8-10 minutes, and drying the obtained product in an oven at 60 ℃.

The composite dispersant is organic solvent ethanol and anionic dispersant, and the anionic dispersant is sodium dodecyl benzene sulfonate;

wherein the volume of the organic solvent ethanol accounts for 10 percent, and the mass of the anionic dispersant sodium dodecyl benzene sulfonate accounts for 0.53 percent.

Example 4

Referring to fig. 4, the process of using the composite dispersant for synergistically dispersing precipitated silica white powder comprises the following steps:

s1: taking a sodium metasilicate solution with the modulus of 1 and the concentration of 0.556mol/L, and adding a certain mass fraction of a composite dispersant into the solution to obtain a mixed solution;

s2: heating the mixed solution in the step S1 to 55 ℃, adding sulfuric acid with the concentration of 1mol/L, adjusting the pH to 7 under the condition that the rotating speed is 700 r/min, then adjusting the temperature to 70 ℃, standing and aging for 1 hour to obtain a product;

s3: and (4) centrifuging the product in the step S2 by using a centrifuge of 6000 rpm for 8-10 minutes, and drying the obtained product in an oven at 60 ℃.

The composite dispersant is organic solvent ethanol and polymer dispersant, and the polymer dispersant is polyacrylamide;

wherein the volume ratio of the organic solvent ethanol is 10 percent, and the mass ratio of the polymer dispersant polyacrylamide is 0.53 percent.

Example 5

Referring to fig. 5, the process of using the composite dispersant for synergistically dispersing precipitated silica white powder comprises the following steps:

s1: taking a sodium metasilicate solution with the modulus of 1 and the concentration of 0.556mol/L, and adding a certain mass fraction of a composite dispersant into the solution to obtain a mixed solution;

s2: heating the mixed solution in the step S1 to 55 ℃, adding sulfuric acid with the concentration of 1mol/L, adjusting the pH to 7 under the condition that the rotating speed is 700 r/min, then adjusting the temperature to 70 ℃, standing and aging for 1 hour to obtain a product;

s3: and (4) centrifuging the product in the step S2 by using a centrifuge of 6000 rpm for 8-10 minutes, and drying the obtained product in an oven at 60 ℃.

The composite dispersant is organic solvent ethanol and polymer dispersant, and the polymer dispersant is polyvinylpyrrolidone;

wherein the volume ratio of the organic solvent ethanol is 10 percent, and the mass ratio of the polymer dispersant polyvinylpyrrolidone is 0.53 percent.

Example 6

Referring to fig. 6, the process of using the composite dispersant for synergistically dispersing precipitated silica white powder comprises the following steps:

s1: taking a sodium metasilicate solution with the modulus of 1 and the concentration of 0.556mol/L, and adding a certain mass fraction of a composite dispersant into the solution to obtain a mixed solution;

s2: heating the mixed solution in the step S1 to 55 ℃, adding sulfuric acid with the concentration of 1mol/L, adjusting the pH to 7 under the condition that the rotating speed is 700 r/min, then adjusting the temperature to 70 ℃, standing and aging for 1 hour to obtain a product;

s3: and (4) centrifuging the product in the step S2 by using a centrifuge of 6000 rpm for 8-10 minutes, and drying the obtained product in an oven at 60 ℃.

The composite dispersant is organic solvent ethanol, anionic dispersant and polymer dispersant, wherein the anionic dispersant is sodium dodecyl benzene sulfonate, and the polymer dispersant is polyvinylpyrrolidone;

wherein the volume ratio of the organic solvent ethanol is 10 percent, and the mass ratio of the sodium dodecyl benzene sulfonate and the polyvinylpyrrolidone is 1.21 percent.

Comparative example 1

Referring to fig. 7, the process for using the composite dispersant to synergistically disperse precipitated silica powder is characterized by comprising the following steps of:

s1: taking sodium metasilicate solution with the modulus of 1 and the concentration of 0.556 mol/L;

s2: heating the solution in the step S1 to 55 ℃, adding sulfuric acid with the concentration of 1mol/L, adjusting the pH to 7 under the condition that the rotating speed is 700 r/min, then adjusting the temperature to 70 ℃, standing and aging for 1 hour to obtain a product;

s3: and (4) centrifuging the product in the step S2 by using a centrifuge of 6000 rpm for 8-10 minutes, and drying the obtained product in an oven at 60 ℃.

Sampling and analyzing: standard test specimens were prepared and the test results are shown in Table 1.

Table 1 laser particle size analysis results of the samples prepared

Note: in the table CTAB denotes cetyltrimethylammonium bromide.

As can be seen from table 1 and TEM analysis in fig. 1 to 7, all of the organic solvent ethanol, cationic dispersant (CTAB, etc.), anionic dispersant (sodium dodecylbenzenesulfonate, etc.), polymer dispersant (polyacrylamide, polyvinylpyrrolidone, etc.) can be added to reduce the median agglomerated particle size (D (0.5)) of the silica particles, and to suppress the occurrence of agglomeration, and from D (0.5) ═ 46.017 μm when no dispersant is added to D (0.5) ═ 41.608 to 14.686 μm when a composite dispersant is added, in particular, when three components of ethanol, polyvinylpyrrolidone and sodium dodecylbenzenesulfonate are added, the median agglomerated particle size D (0.5) is minimized to 10.85 μm, and the primary particle size is about 20 nm;

the organic solvent can reduce the surface tension of particles and the number of silicon hydroxyl groups on the surface, reduce the formation of Si-O-Si bonds between particles during drying and dehydration, introduce charges on the particle surface to increase the electrostatic repulsion between particles, and the polymer dispersant plays a role in blocking the particles to avoid approaching, so that the three components have the synergistic dispersion effect. It is expected that the particle size of the particles can be further reduced on the basis of optimizing the surface electrical property and molecular structure of the dispersant.

The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.