CN106315598A - Method for preparing high-dispersity white carbon black for radial tire - Google Patents

Method for preparing high-dispersity white carbon black for radial tire Download PDF

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CN106315598A
CN106315598A CN201610646062.9A CN201610646062A CN106315598A CN 106315598 A CN106315598 A CN 106315598A CN 201610646062 A CN201610646062 A CN 201610646062A CN 106315598 A CN106315598 A CN 106315598A
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solution
white carbon
preparation
sulphuric acid
mixed solution
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CN106315598B (en
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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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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/113Silicon oxides; Hydrates thereof
    • C01B33/12Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/18Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
    • C01B33/187Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by acidic treatment of silicates
    • C01B33/193Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by acidic treatment of silicates of aqueous solutions of silicates
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/34Silicon-containing compounds
    • C08K3/36Silica
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/12Surface area
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/80Compositional purity

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Tires In General (AREA)

Abstract

The invention discloses a method for preparing high-dispersity white carbon black for a radial tire. The method includes the following steps that a sodium silicate solution with the density of 1.1-1.2 g/cm<3> is prepared; a mixed solution of sulfuric acid and sulfate is prepared according to the molar ratio of 1:(0.5-1), wherein the concentration of sulfuric acid in the mixed solution is 2-4 mol/L; the mixed solution is added into the sodium silicate solution under the stirring condition according to the volume ratio of (1-3):10, and the mixture is heated to 60-70 DEG C to obtain a precursor solution; the sodium silicate solution is added into the precursor solution according to the volume ratio of 1:(2-5), pH of a system is controlled to be 7-9 by means of sulfuric acid in the addition process, and after addition, stirring continues for 0.5-1 h; sulfuric acid is added into the obtained mixed solution till pH of the mixed solution is 4-5, the mixed solution is still standing, and the white carbon black is obtained. The method is easy to operate and low in cost, and the obtained white carbon black has good dispersity in rubber.

Description

The preparation method of the high-dispersion white carbon black of one meridian line tyre
Technical field
The present invention relates to the preparation method of the high-dispersion white carbon black of a meridian line tyre.
Background technology
Radial is that body cord is arranged by meridian direction, has cord circumferential array or delaying close to circumferential array Rush a kind of novel tire that layer tightly binds round on carcass.Radial, because of scientific and reasonable for structure, makes stress improve, and takes turns than oblique line Mold has many excellent performances:
(1) service life is long.The belt bigger owing to having rigidity between radial tire tread and casingply, therefore When tire rolls on road surface, circumferential deformation is little, and Relative sliding is little.Big because of the radial elastic of tire body again, make tyre contact patch Long-pending increase, pressure reduces, therefore tread wear is strong, and resistance to puncture, is difficult to blow out, and distance travelled is many than common diagonal-ply tire 30%。
(2) resistance to rolling is little, and oil consumption is low.Owing to radial curtain cloth layer is few, travel temperature low, rapid heat dissipation, again because of Circumferential deformation is little, therefore resistance to rolling is than the common little 15%-20% of oblique line tire, coasting distance many about 25%, therefore, uses meridian Tire not only can improve the travel speed of automobile, also can improve automobile fuel ecomomy (typically can reduce oil consumption 5%-12%).
(3) bearing capacity is big.The deformation direction main with tire due to the arrangement of radial cord is consistent, thus makes curtain Line strength obtains sufficiently effective utilization, therefore higher by more than 10% than common diagonal-ply tire bearing capacity.
(4) damping performance is good.Because the radial elastic of radial ply tire is big, deformation is big radially (to be perpendicular to direction, ground), can To relax the impact of uneven road surface, make automobile hold pliable improvement, ride comfort under the arm, also reduce vehicle simultaneously and be hit damage Probability, contribute to extend vehicle service life.
White carbon is a kind of excellent reinforcing agent for rubber.Radial crown add appropriate white White carbon black can improve the performances such as its wear-resisting, durable and resistance to puncture, can improve the grasp property of tire tread road pavement simultaneously, reduces and rolls Resistance and dynamic heat build up, existing can meet on the market radial use require precipitated silica product the most less, and Predominantly imported product.
Summary of the invention
It is an object of the invention to provide the preparation method of the high-dispersion white carbon black of a meridian line tyre.
In order to solve above-mentioned technical problem, the invention provides following technical scheme:
The preparation method of the high-dispersion white carbon black of one meridian line tyre, comprises the steps:
(1) preparation density is 1.1~1.2g/cm3Water glass solution;
(2) being 1:0.5~1 by the mol ratio of sulphuric acid Yu sulfate, preparation sulphuric acid and the mixed solution of sulfate, in mixed solution The concentration of sulphuric acid is 2~4mol/L;
(3) under agitation, it is 1~3:10 by volume, the mixed solution of step (2) is added in water glass solution, is heated to 60~70 DEG C obtain precursor aqueous solution;
(4) adding water glass solution in the precursor aqueous solution of step (3), precursor aqueous solution is 1:2 with the volume ratio of water glass solution ~5, in adition process, by sulphuric acid control system pH 7~9, after addition, continue stirring 0.5~1 hour;
(5) mixed liquor obtained by step (4) adds sulphuric acid, be 4~5 to pH of mixed, stand 1~3 hour, then mistake Filter, wash, be dried to obtain white carbon.
Preferably, the modulus of step (1) described waterglass is 2.6~2.9.
Preferably, described sulfate is sodium sulfate or potassium sulfate.
Preferably, the mixing speed of step (3) is 100~300 revs/min.
The inventive method is simple to operate, low cost, and prepared white carbon has good dispersibility in rubber.Use The rubber property indices of this white carbon disclosure satisfy that radial uses requirement.
Detailed description of the invention
Hereinafter the preferred embodiments of the present invention are illustrated, it will be appreciated that preferred embodiment described herein is only used In the description and interpretation present invention, it is not intended to limit the present invention.
Embodiment 1
The preparation method of the high-dispersion white carbon black of one meridian line tyre, step is as follows:
(1) preparation density is 1.1g/cm3Water glass solution, the modulus of waterglass is 2.6;
(2) it is 1:0.5 by the mol ratio of sulphuric acid Yu sodium sulfate, preparation sulphuric acid and the mixed solution of sodium sulfate, sulfur in mixed solution The concentration of acid is 4mol/L;
(3) under the stirring of 200 revs/min, the mixed solution of step (2) is added in water glass solution, be heated to 60 DEG C and obtain To precursor aqueous solution, the mixed solution of step (2) and the volume ratio of water glass solution are 1:5;
(4) it is 1:3 by the volume ratio of precursor aqueous solution Yu water glass solution, in the precursor aqueous solution of step (3), adds waterglass molten Liquid, in whole adition process, by addition sulphuric acid control system pH 7~9, after addition, continues stirring 1 hour;
(5) mixed liquor obtained by step (4) adds sulphuric acid, until pH of mixed is 4, then stands 2 hours, then pass through Filter, wash, be dried, i.e. obtain high-dispersion white carbon black.
Embodiment 2
The preparation method of the high-dispersion white carbon black of one meridian line tyre, step is as follows:
(1) preparation density is 1.15g/cm3Water glass solution, the modulus of waterglass is 2.8;
(2) it is 1:0.8 by the mol ratio of sulphuric acid Yu sodium sulfate, preparation sulphuric acid and the mixed solution of sodium sulfate, sulfur in mixed solution The concentration of acid is 3mol/L;
(3) under the stirring of 300 revs/min, the mixed solution of step (2) is added in water glass solution, be heated to 65 DEG C and obtain To precursor aqueous solution, the mixed solution of step (2) and the volume ratio of water glass solution are 1:10;
(4) it is 1:2 by the volume ratio of precursor aqueous solution Yu water glass solution, in the precursor aqueous solution of step (3), adds waterglass molten Liquid, in whole adition process, by addition sulphuric acid control system pH 7~9, after addition, continues stirring 0.5 hour;
(5) mixed liquor obtained by step (4) adds sulphuric acid, until pH of mixed is 4, then stands 1 hour, then pass through Filter, wash, be dried, i.e. obtain high-dispersion white carbon black.
Embodiment 3
The preparation method of the high-dispersion white carbon black of one meridian line tyre, step is as follows:
(1) preparation density is 1.2g/cm3Water glass solution, the modulus of waterglass is 2.9;
(2) it is 1:1 by the mol ratio of sulphuric acid Yu sodium sulfate, preparation sulphuric acid and the mixed solution of sodium sulfate, sulphuric acid in mixed solution Concentration be 2mol/L;
(3) under the stirring of 100 revs/min, the mixed solution of step (2) is added in water glass solution, be heated to 70 DEG C and obtain To precursor aqueous solution, the mixed solution of step (2) and the volume ratio of water glass solution are 1:3;
(4) it is 1:5 by the volume ratio of precursor aqueous solution Yu water glass solution, in the precursor aqueous solution of step (3), adds waterglass molten Liquid, in whole adition process, by addition sulphuric acid control system pH 7~9, after addition, continues stirring 0.5 hour;
(5) mixed liquor obtained by step (4) adds sulphuric acid, until pH of mixed is 5, then stands 3 hours, then pass through Filter, wash, be dried, i.e. obtain high-dispersion white carbon black.
The physical and chemical index of described high-dispersion white carbon black is as follows:
Burning decrement≤5 wt%;
Dioxide-containing silica >=93 wt%;
Water solubles content≤1 wt%;
Specific surface area (BET): 150-170 m2/g。
By 100 parts of natural rubbers: 15 parts of high-dispersion white carbon blacks, add the additive that other rubber industry is conventional, according to routine Method prepares vulcanite.Performance is as follows:
Mooney scorch (130 DEG C): 18.5-18.9 min;
Hot strength: 27-28 MPa;
Akron abrasion loss: 0.090-0.095 cm3
Comparative example
The preparation process of white carbon is as follows:
(1) preparation density is 1.2g/cm3Water glass solution, the modulus of waterglass is 2.9;
(2) compound concentration is the sulfuric acid solution of 2mol/L and concentration is the metabisulfite solution of 2mol/L;
(3) under the stirring of 100 revs/min, metabisulfite solution is added in water glass solution, be heated to 70 DEG C, be subsequently adding Sulfuric acid solution, stirring obtains precursor aqueous solution after half an hour, wherein, metabisulfite solution, sulfuric acid solution and the volume of water glass solution Ratio is 1:1:3;
(4) it is 1:5 by the volume ratio of precursor aqueous solution Yu water glass solution, in the precursor aqueous solution of step (3), adds waterglass molten Liquid, in whole adition process, controls system pH 7~9 by adding sulphuric acid;
(5) mixed liquor obtained by step (4) continuously adds sulphuric acid, until pH of mixed is 5, then stand 3 hours, then Through filtering, washing, it is dried, obtains white carbon.
By 100 parts of natural rubbers: vulcanite prepared by 15 parts of white carbons, and other is same as in Example 3.Performance is as follows:
Mooney scorch (130 DEG C): 16.1-16.4 min;
Hot strength: 24-25 MPa;
Akron abrasion loss: 0.110-0.120 cm3
Finally it is noted that the foregoing is only the preferred embodiments of the present invention, it is not limited to the present invention, Although being described in detail the present invention with reference to previous embodiment, for a person skilled in the art, it still may be used So that the technical scheme described in foregoing embodiments to be modified, or wherein portion of techniques feature is carried out equivalent. All within the spirit and principles in the present invention, any modification, equivalent substitution and improvement etc. made, should be included in the present invention's Within protection domain.

Claims (4)

1. the preparation method of the high-dispersion white carbon black of a meridian line tyre, comprises the steps:
(1) preparation density is 1.1~1.2g/cm3Water glass solution;
(2) being 1:0.5~1 by the mol ratio of sulphuric acid Yu sulfate, preparation sulphuric acid and the mixed solution of sulfate, in mixed solution The concentration of sulphuric acid is 2~4mol/L;
(3) under agitation, it is 1~3:10 by volume, the mixed solution of step (2) is added in water glass solution, is heated to 60~70 DEG C obtain precursor aqueous solution;
(4) adding water glass solution in the precursor aqueous solution of step (3), precursor aqueous solution is 1:2 with the volume ratio of water glass solution ~5, in adition process, by sulphuric acid control system pH 7~9, after addition, continue stirring 0.5~1 hour;
(5) mixed liquor obtained by step (4) adds sulphuric acid, be 4~5 to pH of mixed, stand 1~3 hour, then mistake Filter, wash, be dried to obtain white carbon.
Preparation method the most according to claim 1, it is characterised in that: the modulus of step (1) described waterglass be 2.6~ 2.9。
Preparation method the most according to claim 1, it is characterised in that: described sulfate is sodium sulfate or potassium sulfate.
Preparation method the most according to claim 1, it is characterised in that: the mixing speed of step (3) is 100~300 revs/min Clock.
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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109231222A (en) * 2018-11-05 2019-01-18 无锡恒诚硅业有限公司 A kind of high structural, HR highly reinforcing white carbon black and its preparation method and application
CN109231223A (en) * 2018-11-05 2019-01-18 无锡恒诚硅业有限公司 A kind of high structural, high-reinforcement white carbon black and its preparation method and application
CN111777800A (en) * 2020-07-03 2020-10-16 确成硅化学股份有限公司 Preparation method of white carbon black for green tire
CN112678838A (en) * 2020-12-29 2021-04-20 无锡恒诚硅业有限公司 Low rolling resistance precipitated silica, and preparation method and application thereof
CN113651332A (en) * 2021-08-11 2021-11-16 常州大学 Preparation method of high-performance white carbon black based on styrene butadiene rubber reinforcement

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102408115A (en) * 2011-08-22 2012-04-11 通化双龙化工股份有限公司 Method for controlling gel amount in white carbon black by using precipitation method
CN103435046A (en) * 2013-08-06 2013-12-11 龙星化工股份有限公司 Preparation technology of high-dispersity white carbon black for snow tire

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102408115A (en) * 2011-08-22 2012-04-11 通化双龙化工股份有限公司 Method for controlling gel amount in white carbon black by using precipitation method
CN103435046A (en) * 2013-08-06 2013-12-11 龙星化工股份有限公司 Preparation technology of high-dispersity white carbon black for snow tire

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109231222A (en) * 2018-11-05 2019-01-18 无锡恒诚硅业有限公司 A kind of high structural, HR highly reinforcing white carbon black and its preparation method and application
CN109231223A (en) * 2018-11-05 2019-01-18 无锡恒诚硅业有限公司 A kind of high structural, high-reinforcement white carbon black and its preparation method and application
CN111777800A (en) * 2020-07-03 2020-10-16 确成硅化学股份有限公司 Preparation method of white carbon black for green tire
CN112678838A (en) * 2020-12-29 2021-04-20 无锡恒诚硅业有限公司 Low rolling resistance precipitated silica, and preparation method and application thereof
CN113651332A (en) * 2021-08-11 2021-11-16 常州大学 Preparation method of high-performance white carbon black based on styrene butadiene rubber reinforcement
CN113651332B (en) * 2021-08-11 2023-10-27 常州大学 Preparation method of high-performance white carbon black based on styrene-butadiene rubber reinforcement

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