WO2017109743A1 - Silice précipitée - Google Patents

Silice précipitée Download PDF

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Publication number
WO2017109743A1
WO2017109743A1 PCT/IB2016/057922 IB2016057922W WO2017109743A1 WO 2017109743 A1 WO2017109743 A1 WO 2017109743A1 IB 2016057922 W IB2016057922 W IB 2016057922W WO 2017109743 A1 WO2017109743 A1 WO 2017109743A1
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Prior art keywords
precipitated silica
range
silica
accordance
surface area
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PCT/IB2016/057922
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English (en)
Inventor
Rautaray Debabrata
Parida PRABHAT KUMAR
Lolage MAYURA
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Tata Chemicals Limited
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Publication of WO2017109743A1 publication Critical patent/WO2017109743A1/fr

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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
    • 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
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/34—Silicon-containing compounds
    • C08K3/36—Silica
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
    • 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
    • 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
    • C01P2006/16—Pore diameter
    • 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
    • C01P2006/19—Oil-absorption capacity, e.g. DBP values
    • 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
    • C01P2006/90—Other properties not specified above

Definitions

  • the present disclosure relates to precipitated silica suitable for use as a reinforcing filler. Specifically, the present disclosure provides precipitated silica having desired surface morphology, porosity and silanol density, which could exhibit high dispersibility in an elastomer.
  • Silica is well-known for use as a reinforcing filler in vulcanizable rubber mixtures, such as those used to form tyres.
  • the reinforcing fillers used in tyre compounding are critical to achieving the performance requirements and substantially assist in strengthening the rubber network thereof, resulting in a substantial increase in stiffness, tensile strength, and resistance to abrasion. This in effect contributes in increasing the longevity of tyres while reducing the fuel consumption.
  • the silica used in the tyre industry is generally precipitated silica, in particular characterized by its particle size, structure and surface activity. It is known that the properties of precipitated silica affect the reinforcement properties thereof. It necessitates the need to identify the characteristic attributes of silica suited for different requirement profile of different applications. Depending on the requirement profile, these properties may vary.
  • An essential parameter for characterizing a precipitated silica is the surface area which is determined either by the adsorption of nitrogen (commonly referred to as BET (after Brunauer, Emmett and Teller) surface area) or, by the adsorption of Cetyl trimethyl ammonium bromide ⁇ CTAB) on the surface of silica (commonly referred to as CTAB sur- face area).
  • BET surface area provides total surface area
  • CTAB surface area provides external surface area of silica.
  • the ratio of said two parameters viz. BET/ CTAB provides a measure of microporosity. Pore volume and pore size distribution are also an important of better rubber to filler interaction. Also, total pore volume plays an important role for rubber penetration in the early stage of mixing.
  • Silica synthesis process follows the condensation of primary particles into aggregates of typical dimensions of 100-200 nm, which are the real reinforcing species in rubber compounds. As the concentration of the aggregate particles increases, an interaction between them leads to the formation of bigger agglomerates.
  • the degree of condensation in aggregates is designated by structure, determines the inter-particle void volume and pore diameter within the aggregates. The measurement of this "structure” is based on the adsorp- tion of dibutyl phthalate (DBP) and is measured by DBP oil absorption value.
  • DBP dibutyl phthalate
  • This coefficient theoretically ranges from 0 to 1, wherein the higher the value of the coefficient, the weaker is the structure of the silica.
  • the Wk coefficient is the ratio of the peak height of the non-degradable particle, the maximum of which lies in the range of 1.0-100 microns, to the peak height of the degraded particles, the maximum of which lies in the range of ⁇ 1 micron.
  • the Wk coefficient is therefore a measure of the "degradability" (dispersibility) of the precipitated silica.
  • EP 0 937 755 discloses that precipitated silicas which possess a BET surface area from about 180 to about 430 m 2 /g and a CTAB surface area from about 160 to 340 m 2 /g and a BET to CTAB ratio of about 1.1 to 1.3 are particularly suitable as carrier mate- rial.
  • a precipitated silica is not meant for application in elastomer and rubber compositions.
  • US20030082090 discloses that precipitated silica having very different BET ( ⁇ 135 m 2 /g)and CTAB surface areas ( ⁇ 75 m 2 /g) while remaining above minimum values are particularly suitable as fillers.
  • surface activity of silica which is usually defined in terms of Sears number influences the properties of silica.
  • Sears number is a measurement of the concentration of silanol groups on the precipitated silica.
  • the silanol groups on the surface of precipitated silica function as potential chemical reaction sites for a coupling reagent, which permit coupling of the silica to the elastomer matrix.
  • the ratio of Sears Number/ CTAB surface area provides the concentration of silanol groups for a given level of CTAB surface area.
  • US 7566433 discloses precipitated silica having a relative breadth ⁇ of pore size distribution of 4.0-10.0 (g nm)/ml, a Sears Number of 28-40 ml/(5 g), a Sears Number /CTAB ratio of 0.18-0.28 ml/(5 m 2 ), and CTAB of 100-200 m 2 /g and suggests that such precipitated silica are particularly suitable as reinforcing fillers. Further, disclosed precipitated silica has a BET/CTAB ratio greater than 1.3 and a zeta potential at pH 5 from -12 to -30 mV.
  • the precipitated silica is obtained by controlling the addition of sulphuric acid such that prevailing alkali number in the reaction medium is 30.0 + 0.3. Additionally, the process employs organic / inorganic salt, as a result of which it contains residues of AI2O3 ranging from 0.01 to 5%.
  • US 7790131 discloses that highly dispersible silica having BET surface area 200- 300 m 2 /g, CTAB surface area ⁇ 170 m 2 /g, DBP number 200-300 g/(100 g), and Sears number 23-35 ml/(5 g) are particularly suited for use as a tire filler for utility vehicles, motor cycles and high speed vehicles.
  • the precipitated silica having said properties is obtained by using organic and/or inorganic salt in the aqueous solution of 0.01 to 5 mol/1 to get the desired properties.
  • a precipitated silica is disclosed.
  • Said precipitated silica has a CTAB surface area in a range of 80-230 m 2 /g; a sears number (V 2 ) in a range of 10 to 30 ml/ (5g); and a ratio of sears number (V 2 ) and CTAB surface area in a range of 0.16 - 0.20 ml/(5 m 2 ).
  • the present disclosure relates to silica having high dispersibility in rubber matrix. Particularly, the present disclosure relates to silica having:
  • CTAB surface area in a range of 80-230 m 2 /g
  • V 2 sears number
  • the CTAB surface area of the precipitated silica is in a range of 130 to 170 m 2 /g.
  • the sears number (V 2 ) of the precipitated silica is in the range of 10 to 25 ml/ (5g).
  • the precipitated silica has a BET/ CTAB in a range of 0.8 to 1.35.
  • the precipitated silica has the BET/ CTAB in a range of 1.1 to 1.25.
  • the precipitated silica has a BET surface area in a range of 100-250 m 2 /g.
  • the precipitated silica has a BET surface area in a range of 100-170 m 2 /g.
  • the precipitated silica has a DBP oil absorption in a range of 240-320 ml/lOOg.
  • the precipitated silica has the DBP oil absorption in a range of 280-320 ml/lOOg.
  • the precipitated silica has a CDBP coefficient in a range of 0.4 to 0.9.
  • the precipitated silica has the CDBP coefficient in a range of 0.5 to 0.9.
  • the precipitated silica has a Wk coefficient number less than 3.
  • the precipitated silica has the Wk coefficient number ranging from 1 to 3.
  • the precipitated silica has an average primary particle size ranging from 8 to 50 nm.
  • the precipitated silica has the average primary particle size ranging from 10-30 nm.
  • the precipitated silica has an average particulate aggregate size ranging from 50 to 3000 nm.
  • the precipitated silica has the aver- age particulate aggregate size ranging from 50 to 600 nm.
  • the precipitated silica has a micro pore volume ranging from 0.01 to 0.06 cm 3 /g.
  • the precipitated silica has the micro pore volume ranging from 0.01 to 0.02 cm 3 /g.
  • the precipitated silica has a micro pore area ranging from 6 to 35 m 2 /g.
  • the precipitated silica has the micro pore area ranging from 10 to 25 m 2 /g.
  • the precipitated silica has a pore diameter ranging from 250 A to 350 A.
  • the precipitated silica has the pore diameter ranging from 250 A to 300 A.
  • the precipitated silica has a moisture loss of 2 to 6% by weight, on drying for two hours at 105°C.
  • the precipitated silica has the moisture loss of 2 to 5% by weight, on drying for two hours at 105°C.
  • the precipitated silica has a tapped density in a range of 0.12 - 0.30 g/cc.
  • the precipitated silica has the tapped density in a range of 0.18 - 0.25 g/cc.
  • the precipitated silica has a bulk density in a range of 90 - 140 g/1.
  • the precipitated silica has the bulk density in a range of 100 to 120 g/1.
  • the precipitated silica has a pH value of 6 - 6.5
  • the precipitated silica has S1O2 content of greater than 96 %.
  • the precipitated silica has the S1O2 content of 97 %.
  • the precipitated silica has a soluble salt content of less than 0.5 to 1%.
  • the precipitated silica has the soluble salt content of less than 0.5%.
  • the precipitated silica has a zeta potential in a range of 20 mV to -50 mV.
  • the precipitated silica has the zeta potential in a range of -30mV to -40 mV.
  • the precipitated silica has an electrical conductivity (4% in water) of less than 1300 ⁇ 8/ cm.
  • the precipitated silica has the electrical conductivity (4% in water) in a range of less of 1200 ⁇ 8/ cm.
  • the precipitated silica according to the present invention can be optionally modified with silanes or organosilanes.
  • the precipitated silica according to the present disclosure can be optionally modified with silanes or organosilanes.
  • a process of preparing the above mentioned precipitated silica comprises of: reacting an aqueous solution of a metal silicate with a mineral acid in the presence of a surfactant solution comprising gelatin and C8-C20 sulfosuccinate blend, at a reaction temperature in a range of about 70 to 100 °C with constant stirring such that a reaction mixture having a pH of about 10 + 0.3 is obtained; - optionally, allowing the reaction mixture to age at a temperature in a range of about 70 to 100 °C for a time period in range of 10 minutes to 30 minutes; adjusting the pH of the reaction mixture to about 4, followed by aging said mixture at a temperature in a range of about 70 to 100 °C for a time period in a range of 10 minutes to 2 hours; and
  • the surfactant solution is prepared by dissolving gelatin in water followed by addition of C8-C20 sulfosuccinate blend at 50 to 80 °C.
  • the surfactant solution comprises gelatin and C8-C20 sulfosuccinate blend in a ratio ranging from 1 : 1 to 1:3, and preferably 1 : 1.5.
  • the surfactant solution may be obtained by combining 4.5 grams of gelatin with 6.75 ml of C8-C20 sulfosuccinate blend, such as Surfactant- OT 85 AE, commercially available from CYTEC.
  • the metal silicate is selected from a group consisting of an alkali metal silicate, an alkaline earth metal silicate and mixture thereof.
  • sodium silicate is used as the metal silicate.
  • the metal silicate can contain from 7- 30 wt% S1O2, and preferably 23 wt S1O2.
  • the aqueous solution of metal silicate is prepared by mixing the alkali metal silicate and/or alkaline earth metal silicate with water for a predetermined time period, preferably for 15 minutes, while stirring.
  • the metal silicate has a pH between 11 - 14, and preferably about 12.5 + 0.5.
  • the mineral acid is selected from a group consisting of sulphuric acid, hydrochloric acid, nitric acid.
  • the mineral acid has a molarity in a range of 0.1 M to 2 M, and preferably around 0.625 M.
  • the aqueous medium is formed of water only.
  • the reaction of the aqueous solution of metal silicate with the mineral acid is carried out by separately adding the aqueous solution of metal silicate, the mineral acid, and the surfactant solution to an aqueous medium heated up to the reaction temperature.
  • a reactor containing the aqueous medium and connected to a heater is simultaneously charged with the aqueous solution of the metal silicate, the mineral acid, and the surfactant solution to carry out aforesaid reaction.
  • the reactor containing the aqueous medium and connected to the heater is first charged with the surfactant solution, followed by the addition of the metal silicate and the mineral acid.
  • the surfactant solution is added to the aqueous medium at a temperature lower than the reaction temperature; and the aqueous medium comprising the surfactant solution is then heated till the reaction temperature.
  • the aqueous solution of metal silicate, the mineral acid, and the surfactant solution are added in a continuous manner.
  • the addition may be stopped intermittently to allow intermittent aging of the reaction mixture. The intermittent aging may be carried out for 10-30 minutes.
  • the aqueous solution of metal silicate, the mineral acid, and the surfactant solution are simultaneously added to the aqueous medium over a time period in a range of 30 minutes to 2 hours.
  • the addition rate of the metal silicate solution and the mineral acid is such that the metal silicate solution and the mineral acid are in a ratio of about 1: 1 (based on volume).
  • the addition rate of the metal silicate solution, and the mineral acid may further be adjusted to maintain the pH of 10 +0.3.
  • the surfactant solution is added such that the surfactant solution has a concentration of about 2.25 to 2.5 % w/w with respect to the silica content of the metal silicate solution.
  • the surfactant solution is added such that the surfactant solution has a concentration of about 2.45 % w/w with respect to the silica content of the metal silicate solution.
  • the surfactant solution comprising .98 % (i.e. 4.5 grams) of gelatin and 1.47% (i.e. 6.75 ml) of Surfactant- OT 85 AE w.r.t. silica content of sodium silicate is added.
  • the reaction is carried out at the reaction temperature in a range of about 70 to 100 °C.
  • the reaction temperature is 95 °C.
  • the reaction mixture comprising metal silicate solution, the mineral acid, and the surfactant solution is continuously stirred.
  • the stirring is carried out at a stirring rate in a range of 50 to 700 rpm.
  • the stirring is carried out at 400 rpm.
  • the reaction mixture once the reaction mixture has attained the pH of 10+0.3, it is allowed to age at the temperature in a range of about 70 to 100 °C for a time period of 10- 100 minutes. Preferably, the aging is carried out for 60 minutes at 95 °C.
  • the pH of the reaction is rapidly brought down to the pH of around 4.
  • the pH of the reaction mixture is adjusted to about 4 from 10+0.3 by addition of the mineral acid.
  • the pH of the reaction mixture is first adjusted to about 2 from 10+0.3 and then to about 4.
  • the pH of the reaction mixture is adjusted to about 2 from 10+0.3 by addition of the mineral acid and then to around 4 by addition of a base.
  • the base may be any base known to a person skilled in the art.
  • the base is sodium hydroxide.
  • the reaction mixture is allowed to age at the pH of about 4 for a time period in a range of 10 minutes to 2 hours. Preferably, the reaction mixture is allowed to age for 1 hour. In accordance with a related embodiment, the aging is carried out at a temperature in a range of 70 to 100 °C. Preferably, the aging is carried out at 95 °C. In accordance with an embodiment, the aging is carried out while continuously stirring the reaction mixture.
  • the precipitated silica obtained upon completion of reaction is filtered followed by washing. Washing is done to eliminate the by products, such as sodium sulphate, obtained as a result of reaction.
  • precipitated silica is then subjected to a drying step.
  • the drying step may be carried out by spray drying, spin flash drying, or vacuum tray drying.
  • the wet cake is subjected to short-term drying, followed by addition of a dispersing agent in a suitable solvent.
  • the dispersion may then be dried to obtain precipitated silica.
  • the dispersion of silica is prepared using a dispersing agent selected from a group consisting of metal salt of saturated and unsaturated fatty esters with long hydrocarbon chain/ fatty acids in an appropriate solvent selected from a group consisting of butanol, butanone, toluene and acetone.
  • a dispersing agent selected from a group consisting of metal salt of saturated and unsaturated fatty esters with long hydrocarbon chain/ fatty acids in an appropriate solvent selected from a group consisting of butanol, butanone, toluene and acetone.
  • the silica according to the present disclosure can be used in tyre rubber, rice roller rubber, shoe sole rubber or any other elastomers.
  • the silica disclosed herein is suitable for use as filler in vulcanizable or vulcanized elastomer compositions.
  • the vulcanized elastomer composition can be used for the manufacture of tyre and other rubber products.
  • said silica may be used as a reinforcing filler in a quantity in a range of 7 to 90 phr. Any conventional process may be used to form vulcaniz- able or vulcanized elastomer compositions using the above disclosed silica as reinforcing filler.
  • Such a precipitated silica having:
  • CTAB surface area in a range of 80-230 m 2 /g
  • V 2 a sears number in a range of 10 to 30 ml/ (5g);
  • Such a precipitated silica having the CTAB surface area in the range of 130-170
  • Such a precipitated silica having the sears number (V 2 ) in the range of 10 to 25 ml/
  • Such a precipitated silica having a BET surface area in a range of 100 to 250 m 2 /g.
  • Such a precipitated silica having a BET/ CTAB area in a range of 0.8 to 1.35.
  • Such a precipitated silica having a DBP oil absorption in a range of 240-320 ml/lOOg.
  • Such a precipitated silica a CDBP coefficient (DA) in range of 0.4 to 0.9.
  • Such a precipitated silica having a Wk coefficient number less than 3.
  • Such a precipitated silica having an average particulate aggregate size ranging from 50 to 3000 nm.
  • Such a precipitated silica having a micro pore volume ranging from 0.01 to 0.06 cm 3 /g.
  • Such a precipitated silica having a pore diameter ranging from 250 A to 350 A.
  • Such a precipitated silica having a moisture loss of 2 to 6% by weight on drying for two hours at 105 °C.
  • EXAMPLE 1 Process of preparing precipitated silica in accordance with present disclosure.
  • This solution has a pH value of 12.5 + 0.5.
  • the sulphuric acid metering pump was switched on and sulphuric acid solution was added at an addition rate of 30 millilitres/minute to the reaction chamber, while continuing the addition of both sodium silicate and water at the addition rate of 30 millilitres/minute.
  • the reaction mixture is stirred at 400 rpm.
  • the addition of sulphuric acid, sodium silicate and water were stopped while continuing the stirring at 400 rpm and 95°C reactor temperature.
  • the reaction mixture was then allowed to age for 30 minutes.
  • the pH of the solution in the reaction chamber was checked. At this point, it was ensured that the pH of the reaction mixture is between pH 9.7 to 10.
  • 300 millilitres of the surfactant solution was added to the reactor.
  • the addition of sulphuric acid and sodium silicate was started at the addition rate of 30 millilitres/minute and water at the addition rate of 45 millilitres/minute while stirring at 95 °C for next 60 minutes.
  • the pH of the solution in the reaction chamber was checked. It was ensured that the pH of the reac- tion mixture is between pH 9.7 to 10.
  • the addition of sulphuric acid, sodium silicate and water were stopped.
  • the reaction mixture was allowed to age for another 70 minutes while stirring at 95°C.
  • sulphuric acid was added to the reaction mixture at 100 millilitres/minute.
  • the pH was measured till the reaction mixture attained a pH of 4.0 - 4.7.
  • the addition of sulphuric acid was stopped.
  • the reaction mixture was allowed to age for 1 hour at 95°C with continuous stirring.
  • Example 2 Process of preparing precipitated silica in accordance with present disclosure.
  • the obtained sodium silica solution has a pH value of 12.5 + 0.5.
  • the 1.25 M sulphuric acid solution is diluted 2 times by mixing 1.5 litre of 1.25 M sulphuric acid solution and 1.5 litre of water.
  • the resultant sulphuric acid solution has a molarity of 0.625 M and pH 1 ⁇ 0.3.
  • Gelatin and C8-C20 sulfosuccinate blend surfactant is prepared by first taking 600 millilitres of distilled water and heating it up to 50-60°C followed by adding to it 3.75 grams of gelatin. The resultant mixture is stirred to dissolve gelatin in water. Subsequently, 5.6 milliliter of C8-C20 sulfosuccinate blend surfactant is added to it followed by stirring to obtain gelatin and C8-C20 sulfosuccinate blend surfactant.
  • pH should be 10 ⁇ 0.3.
  • 1.25 M sulfuric acid solution is added to the reactor to adjust the pH of the reaction mixture to 2 ⁇ 0.5 followed by addition of 5% NaOH solution to bring the pH to 4 ⁇ 0.5.
  • the solution mixture was aged/ maintained at 95 ° C for lhour while stirring at 400 rpm.
  • precipitate was collected from the reactor.
  • the precipitate was centrifuged at 4000 rpm for 5 minutes.
  • the filter cake thus obtained was collected and washed thoroughly with approximately 5 litre of distilled water to remove sodium sulphate.
  • the solid content of the wet cake was checked and found to be 12-15% by drying at 125 °C.
  • a dispersion of 6 - 10 % solid content was prepared thereafter by adding distilled water to obtain silica slurry. Once silica slurry is prepared, metal salt of saturated and unsaturated fatty esters with long hydrocarbon chain/ fatty acids was used as dispersing agent with a 2-4% w/w loading in an appropriate solvent (e.g.

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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)
  • Silicon Compounds (AREA)

Abstract

L'invention concerne une silice précipitée. Ladite silice précipitée présente une surface CTAB dans une plage de 80 à 230 m2/g; un nombre de Sears (V2) compris entre 10 et 30 ml/ (5g) et un rapport entre le nombre de Sears (V2) et une surface CTAB compris entre 0,16 et 0,20 ml/ (5 m2).
PCT/IB2016/057922 2015-12-23 2016-12-22 Silice précipitée WO2017109743A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
IN4839MU2015 2015-12-23
IN4839/MUM/2015 2015-12-23

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WO2017109743A1 true WO2017109743A1 (fr) 2017-06-29

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3393971A4 (fr) * 2015-12-23 2019-06-05 Tata Chemicals Limited Procédé de préparation de silice précipitée
WO2022101015A1 (fr) * 2020-11-10 2022-05-19 Rhodia Operations Compositions de soin buccal de blanchiment

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA2403954A1 (fr) * 2001-09-20 2003-03-20 Degussa Ag Silice precipitee avec rapport bet/ctab eleve
US20120041128A1 (en) * 2008-10-06 2012-02-16 Dimona Silica Industries Highly dispersible silica for rubbers and the process for obtaining it
TWI376352B (en) * 2005-09-09 2012-11-11 Evonik Degussa Gmbh Precipitated silicas with particular pore size distribution
KR101567617B1 (ko) * 2008-04-07 2015-11-09 에보니크 데구사 게엠베하 엘라스토머 혼합물의 보강 충전제로서의 침전 규산

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA2403954A1 (fr) * 2001-09-20 2003-03-20 Degussa Ag Silice precipitee avec rapport bet/ctab eleve
TWI376352B (en) * 2005-09-09 2012-11-11 Evonik Degussa Gmbh Precipitated silicas with particular pore size distribution
KR101567617B1 (ko) * 2008-04-07 2015-11-09 에보니크 데구사 게엠베하 엘라스토머 혼합물의 보강 충전제로서의 침전 규산
US20120041128A1 (en) * 2008-10-06 2012-02-16 Dimona Silica Industries Highly dispersible silica for rubbers and the process for obtaining it

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3393971A4 (fr) * 2015-12-23 2019-06-05 Tata Chemicals Limited Procédé de préparation de silice précipitée
US11242260B2 (en) 2015-12-23 2022-02-08 Tata Chemicals Limited Process for preparing precipitated silica
WO2022101015A1 (fr) * 2020-11-10 2022-05-19 Rhodia Operations Compositions de soin buccal de blanchiment

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