CN113401914A - Preparation method of high-dispersion white carbon black special for high-fatigue-resistance tire - Google Patents

Preparation method of high-dispersion white carbon black special for high-fatigue-resistance tire Download PDF

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Publication number
CN113401914A
CN113401914A CN202110745043.2A CN202110745043A CN113401914A CN 113401914 A CN113401914 A CN 113401914A CN 202110745043 A CN202110745043 A CN 202110745043A CN 113401914 A CN113401914 A CN 113401914A
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China
Prior art keywords
sodium silicate
carbon black
solution
white carbon
reaction kettle
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Pending
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CN202110745043.2A
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Chinese (zh)
Inventor
毛善兵
于方琪
王永庆
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Quechen Silicon Chemical Co Ltd
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Quechen Silicon Chemical Co Ltd
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Priority to CN202110745043.2A priority Critical patent/CN113401914A/en
Publication of CN113401914A publication Critical patent/CN113401914A/en
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/113—Silicon oxides; Hydrates thereof
    • C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
    • C01B33/187—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by acidic treatment of silicates
    • C01B33/193—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by acidic treatment of silicates of aqueous solutions of silicates
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00—Use of ingredients characterised by shape
    • C08K7/22—Expanded, porous or hollow particles
    • C08K7/24—Expanded, porous or hollow particles inorganic
    • C08K7/26—Silicon- containing compounds
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/12—Surface area

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Inorganic Chemistry (AREA)
  • Pigments, Carbon Blacks, Or Wood Stains (AREA)
  • Silicon Compounds (AREA)

Abstract

The invention discloses a preparation method of high-dispersion white carbon black special for a high-fatigue-resistance tire. The preparation method comprises the following steps: (1) adding a certain amount of electrolyte solution and stearic acid ethanolamine into a reaction kettle, and heating to 60-65 ℃; (2) then adding a sodium silicate solution into the reaction kettle until the pH value is 9-10, and heating to 70-75 ℃; (3) continuously adding a sodium silicate solution into the reaction kettle, and adding an acidifying agent to keep the pH value at 10-11; (4) and after the sodium silicate solution is added, continuously adding an acidifying agent until the pH value is 5-6, and reacting to obtain the white carbon black. Compared with the existing precipitated white carbon black, the white carbon black prepared by the method can obviously improve the fatigue resistance of the tire and effectively improve the running safety and durability of the tire.

Description

Preparation method of high-dispersion white carbon black special for high-fatigue-resistance tire
Technical Field
The invention belongs to the field of white carbon black, and particularly relates to a preparation method of high-dispersion white carbon black special for a high-fatigue-resistance tire.
Background
Due to the fact that road conditions are complex, the flexibility of an automobile in the driving process, particularly in the load driving process, is large, the hysteresis loss of a tire side rubber material caused by the bending deformation is large, the internal temperature of the tire is continuously increased in the long-time driving process, and cracks formed by thermal oxidation aging and fatigue caused by high temperature can directly cause tire damage. Therefore, the fatigue resistance of the tire is improved, and the running safety and the durability of the tire can be effectively improved.
Disclosure of Invention
The invention aims to provide a preparation method of special high-dispersion white carbon black for a high-fatigue-resistance tire.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of special high-dispersion white carbon black for a high-fatigue-resistance tire comprises the following steps:
(1) adding a certain amount of electrolyte solution and stearic acid ethanolamine into a reaction kettle, and heating to 60-65 ℃;
(2) then adding a sodium silicate solution into the reaction kettle until the pH value is 9-10, and heating to 70-75 ℃;
(3) continuously adding a sodium silicate solution into the reaction kettle, and adding an acidifying agent to keep the pH value at 10-11;
(4) and after the sodium silicate solution is added, continuously adding an acidifying agent until the pH value is 5-6, and reacting to obtain the white carbon black.
Preferably, the electrolyte solution is a sodium sulfate solution.
Preferably, the concentration of the sodium sulfate solution is 8 wt%, and the addition amount is 1/6-1/7 of the volume of the reaction kettle.
Preferably, the addition amount of the stearic acid ethanolamine is SiO20.5-5 per mill of the weight of the sodium silicate.
Preferably, the sodium silicate solution is a sodium silicate solution having a concentration of 20 wt%.
Preferably, in the step (3), the sodium silicate solution is stopped adding after the volume of the reaction solution reaches 2/3-3/4 of the volume of the reaction kettle.
Preferably, the acidifying agent is a sulfuric acid solution.
More preferably, the concentration of the sulfuric acid solution is 10 wt%.
Preferably, in the step (4), the reaction is carried out for 0.1 to 1 hour after the pH value reaches 5 to 6.
Preferably, after the reaction is finished, the white carbon black is obtained by filtering, washing, pulping and drying.
Detailed Description
The present invention will be described in further detail with reference to examples.
The preparation method of the special high-dispersion white carbon black for the high-fatigue-resistance tire comprises the following steps:
(1) adding a certain amount of electrolyte solution and stearic acid ethanolamine into a reaction kettle, and heating to 60-65 ℃;
(2) then adding a sodium silicate solution into the reaction kettle until the pH value is 9-10, and heating to 70-75 ℃;
(3) continuously adding a sodium silicate solution into the reaction kettle, and adding an acidifying agent to keep the pH value at 10-11;
(4) and after the sodium silicate solution is added, continuously adding an acidifying agent until the pH value is 5-6, and reacting to obtain the white carbon black.
In the invention, the electrolyte solution can be selected from a sodium sulfate solution, the concentration of the sodium sulfate solution can be controlled to be 8 wt%, and the addition amount of the sodium sulfate solution is 1/6-1/7 of the volume of the reaction kettle. The purpose of adding the electrolyte is to regulate and control the Zeta potential on the surface of the primary particles of the white carbon black and control the aggregation state of the primary particles.
In the invention, the adding amount of the stearic acid ethanolamine is SiO20.5-5 per mill of the weight of the sodium silicate, and the added ethanolamine stearate plays a role of a reaction regulator.
In the present invention, the sodium silicate solution is a sodium silicate solution having a concentration of 20 wt%. The concentration of the sodium silicate solution is too high, which easily causes the generation and aggregation of a large amount of instantaneous local silicon dioxide, and the concentration of the sodium silicate solution is too low, which causes the concentration of the silicon dioxide slurry to be too thin, and the energy consumption of the post-treatment is higher.
In the present invention, the acidifying agent can be selected from a solution of sulfuric acid having a concentration of 10% by weight. The ionic effect of the electrolyte sodium sulfate is enhanced by using sulfuric acid and sodium ions and sulfate ions generated after the sulfuric acid reacts with the sodium silicate.
After the reaction is complete, the slurry is subjected to appropriate post-treatment: filtering, washing, pulping and drying to obtain the white carbon black.
Example 1
A preparation method of special high-dispersion white carbon black for a high-fatigue-resistance tire comprises the following steps:
(1) adding a sodium sulfate solution with the concentration of 8 wt% into the reaction kettle to 1/6 of the volume of the reaction kettle, and then heating to 60-65 ℃.
(2) Adding stearic acid ethanolamine (CAS: 111-57-9) into a reaction kettle under stirring (60 revolutions per minute), wherein the addition amount of the stearic acid ethanolamine is sodium silicate (SiO2Based) one thousandth of the total weight.
(3) Then adding a sodium silicate solution with the concentration of 20 wt% into the reaction kettle until the pH value of the system is 9-10, and then heating to 70-75 ℃.
(4) And continuously adding the sodium silicate solution into the reaction kettle, simultaneously adding a sulfuric acid solution with the concentration of 10 wt% to keep the pH value of the system at 10-11, and stopping adding the sodium silicate when the volume of the reaction liquid reaches 2/3 of the volume of the reaction kettle.
(5) After the sodium silicate solution is added, continuously adding a sulfuric acid solution with the concentration of 10 wt% until the pH value of the system is 5-6, and carrying out heat preservation reaction for 15 minutes.
(6) And carrying out filter pressing, washing, pulping and spray drying treatment on the reaction slurry to obtain the white carbon black.
The specific surface area of the white carbon black is 180-210 m2(g), the dispersion grade is more than or equal to 9.5.
Compared with the existing commercial precipitation-process white carbon black, the fatigue life of the tire, which is tested by the crack propagation method, can be prolonged by more than 10 percent by adopting the white carbon black prepared by the method.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (10)

1. A preparation method of special high-dispersion white carbon black for a high-fatigue-resistance tire comprises the following steps:
(1) adding a certain amount of electrolyte solution and stearic acid ethanolamine into a reaction kettle, and heating to 60-65 ℃;
(2) then adding a sodium silicate solution into the reaction kettle until the pH value is 9-10, and heating to 70-75 ℃;
(3) continuously adding a sodium silicate solution into the reaction kettle, and adding an acidifying agent to keep the pH value at 10-11;
(4) and after the sodium silicate solution is added, continuously adding an acidifying agent until the pH value is 5-6, and reacting to obtain the white carbon black.
2. The method of claim 1, wherein: the electrolyte solution is a sodium sulfate solution.
3. The method of claim 2, wherein: the concentration of the sodium sulfate solution is 8 wt%, and the addition amount of the sodium sulfate solution is 1/6-1/7 of the volume of the reaction kettle.
4. The method of claim 1, wherein: the addition amount of the stearic acid ethanolamine is SiO20.5-5 per mill of the weight of the sodium silicate.
5. The method of claim 1, wherein: the sodium silicate solution is 20 wt% sodium silicate solution.
6. The method of claim 5, wherein: in the step (3), after the volume of the reaction liquid reaches 2/3-3/4 of the volume of the reaction kettle, the addition of the sodium silicate solution is stopped.
7. The method of claim 1, wherein: the acidifying agent is a sulfuric acid solution.
8. The method of claim 7, wherein: the concentration of the sulfuric acid solution was 10 wt%.
9. The method of claim 1, wherein: in the step (4), after the pH value reaches 5-6, the reaction is carried out for 0.1-1 hour.
10. The method of claim 9, wherein: and after the reaction is finished, filtering, washing, pulping and drying to obtain the white carbon black.
CN202110745043.2A 2021-07-01 2021-07-01 Preparation method of high-dispersion white carbon black special for high-fatigue-resistance tire Pending CN113401914A (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2678259A1 (en) * 1991-06-26 1992-12-31 Rhone Poulenc Chimie NOVEL PRECIPITED SILICES IN THE FORM OF PELLETS OR POWDERS, METHODS OF SYNTHESIS AND USE IN REINFORCING ELASTOMERS.
US20050016651A1 (en) * 2001-06-28 2005-01-27 Michelin Recherche Et Technique S.A. Tire tread reinforced with a silica of low specific surface area
WO2012032099A1 (en) * 2010-09-10 2012-03-15 Basf Se Silicon dioxide dispersions
CN105236429A (en) * 2015-09-14 2016-01-13 安徽确成硅化学有限公司 Ultrahighly-dispersed white carbon black preparation method
CN110028073A (en) * 2018-03-06 2019-07-19 河南骏化发展股份有限公司 A kind of preparation method of polymolecularity precipitated silica
CN110127709A (en) * 2019-06-05 2019-08-16 确成硅化学股份有限公司 A kind of method of gradient pH precipitation method preparation high dispersive silica

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2678259A1 (en) * 1991-06-26 1992-12-31 Rhone Poulenc Chimie NOVEL PRECIPITED SILICES IN THE FORM OF PELLETS OR POWDERS, METHODS OF SYNTHESIS AND USE IN REINFORCING ELASTOMERS.
US20050016651A1 (en) * 2001-06-28 2005-01-27 Michelin Recherche Et Technique S.A. Tire tread reinforced with a silica of low specific surface area
WO2012032099A1 (en) * 2010-09-10 2012-03-15 Basf Se Silicon dioxide dispersions
CN105236429A (en) * 2015-09-14 2016-01-13 安徽确成硅化学有限公司 Ultrahighly-dispersed white carbon black preparation method
CN110028073A (en) * 2018-03-06 2019-07-19 河南骏化发展股份有限公司 A kind of preparation method of polymolecularity precipitated silica
CN110127709A (en) * 2019-06-05 2019-08-16 确成硅化学股份有限公司 A kind of method of gradient pH precipitation method preparation high dispersive silica

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
"一种绿色轮胎用高分散白炭黑的制备方法", 橡塑技术与装备 *
PH COCHET,D.PETIT,L.BARRIQUAND,B.DEJEAN,Y.BOMAL,黄家明: "高分散性沉淀法白炭黑在轮胎中的应用研究", 轮胎工业 *

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