EP1093843A1 - Emulgiervorrichtung und Verfahren zur Herstellung von Silikonölemulsion oder Suspension von vernetzten Silikonpartikeln - Google Patents

Emulgiervorrichtung und Verfahren zur Herstellung von Silikonölemulsion oder Suspension von vernetzten Silikonpartikeln Download PDF

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Publication number
EP1093843A1
EP1093843A1 EP00309249A EP00309249A EP1093843A1 EP 1093843 A1 EP1093843 A1 EP 1093843A1 EP 00309249 A EP00309249 A EP 00309249A EP 00309249 A EP00309249 A EP 00309249A EP 1093843 A1 EP1093843 A1 EP 1093843A1
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EP
European Patent Office
Prior art keywords
rotor
emulsion
motor
suspension
silicone
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP00309249A
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English (en)
French (fr)
Inventor
Yoshitsugu Morita
Ryuji Tachibana
Keiji Yoshida
Koichi Ozaki
Toyohiko Yamadera
Kazuo Kobayashi
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
DuPont Toray Specialty Materials KK
Original Assignee
Dow Corning Toray Silicone Co Ltd
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Filing date
Publication date
Application filed by Dow Corning Toray Silicone Co Ltd filed Critical Dow Corning Toray Silicone Co Ltd
Publication of EP1093843A1 publication Critical patent/EP1093843A1/de
Withdrawn legal-status Critical Current

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C7/00—Crushing or disintegrating by disc mills
    • B02C7/11—Details
    • B02C7/16—Driving mechanisms
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/40—Mixing liquids with liquids; Emulsifying
    • B01F23/41—Emulsifying
    • B01F23/4105—Methods of emulsifying
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/40—Mixing liquids with liquids; Emulsifying
    • B01F23/43—Mixing liquids with liquids; Emulsifying using driven stirrers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
    • B01F35/20—Measuring; Control or regulation
    • B01F35/21—Measuring
    • B01F35/212—Measuring of the driving system data, e.g. torque, speed or power data
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C7/00—Crushing or disintegrating by disc mills
    • B02C7/175—Disc mills specially adapted for paste-like material, e.g. paint, chocolate, colloids

Definitions

  • This invention is directed to an emulsifier and to a method for manufacturing a silicone oil emulsion or a crosslinked silicone particle suspension. More particularly, it relates to (i) an emulsifier with which the particle size of an emulsion or a suspension can be continuously adjusted, (ii) a method for manufacturing a silicone oil emulsion with which the particle size of the emulsion can be continuously adjusted, and (iii) a method for manufacturing a crosslinked silicone particle suspension with which the particle size of the suspension can be continuously adjusted.
  • an emulsion or suspension is manufactured by using an emulsifier having a rotor that is rotated by a motor and a stator and produces an emulsification action by shear force with the rotor are known. Also known are (i) methods for manufacturing an emulsion of a silicone oil by emulsifying a silicone oil, an emulsifying agent, and water in this emulsifier, as well as (ii) methods for manufacturing a suspension of crosslinked silicone particles by emulsifying a liquid crosslinkable silicone composition, an emulsifying agent, and water in this emulsifier, to obtain an emulsion of a liquid crosslinkable silicone composition, and then crosslinking this composition that is emulsified in water.
  • the particle size of an emulsion or suspension is adjusted generally by (i) adjusting the clearance between the rotor and stator, (ii) changing the type of emulsifying agent, or (iii) increasing or decreasing the amount in which the emulsifying agent is employed.
  • the present invention is directed to an emulsifier having a rotor that is rotated by a motor and a stator that produces an emulsification action by shear force with the rotor, characterized by having an apparatus for modulating the frequency of the input current to the motor in order to vary the rotational speed of the rotor.
  • the present invention is also directed to a method for manufacturing an emulsion of a silicone oil by emulsifying a silicone oil, an emulsifying agent, and water, in an emulsifier having a rotor that is rotated by a motor and a stator, that produces an emulsification action by shear force with the rotor, characterized in that the particle size of the emulsion is adjusted by varying the rotational speed of the rotor.
  • the present invention is further directed to a method for manufacturing a suspension of crosslinked silicone particles by emulsifying a liquid crosslinkable silicone composition, an emulsifying agent, and water, in an emulsifier having a rotor that is rotated by a motor and a stator, that produces an emulsification action by shear force with the rotor, thereby obtaining an emulsion of a liquid crosslinkable silicone composition, and then crosslinking the composition that is emulsified in water, characterized in that the particle size of the suspension is adjusted by varying the rotational speed of the rotor.
  • the accompanying Figure is a pictorial representation shown partly in cross section, and a schematic diagram of the emulsifier device of the present invention.
  • 1 represents the emulsifier device generally
  • 2 is the raw material supply port
  • 3 is a rotor
  • 4 is the stator
  • 5 is the motor
  • 6 is an inverter
  • 7 is the finished product discharge port.
  • the emulsifier device of the present invention has a rotor that is rotated by a motor and a stator that produces an emulsification action by shear force with the rotor.
  • the device is characterized by having an apparatus for modulating the frequency of the input current to the motor, in order to vary the rotational speed of the rotor.
  • Examples of the device include a colloid mill, homomixer, and an inline mixer, with the colloid mill being preferred.
  • the rotor may supported on the rotary shaft of the motor such that it transmits the rotation of the motor, or the rotation of the motor may be transmitted by gears, a belt, and a chain.
  • An apparatus termed an inverter is used as a mechanism for modulating the frequency of the input current to the motor, in order to vary the rotational speed of the rotor.
  • the inverter is able to vary the rotational speed of the motor directly by modulating the frequency of the input current to the motor, which allows the emulsifier to be more compact.
  • the particle size of an emulsion or suspension can be adjusted continuously, so it is possible to continuously prepare an emulsion or suspension with a large particle size to an emulsion or suspension with a small particle size.
  • the emulsifier device 1 of the present invention includes a raw mate supply port 2 through which the raw material is supplied; a rotor 3 and a stator 4 for emulsifying the raw material; a motor 5 for rotating the rotor 3; an inverter 6 that functions as the apparatus for modulating the frequency of the input current to the motor 5, in order to vary the rotational speed of the motor 5; and a finished product discharge port 7 from which the emulsified finished product is removed.
  • the rotation of the motor 5 may be transmitted to the rotor 3 by other means as noted above.
  • An emulsifying action is produced by the shear force in the clearance between the rotor 3 and stator 4, and it is preferred that this clearance be between 1 and 1000 ⁇ m. It is also preferred that the rotational speed of the rotor be between 1000 and 20,000 rpm. If the viscosity of the raw material to be emulsified is over 5000 mPa ⁇ s at 25 °C, it is preferred that the rotational speed of the rotor be between 10,000 and 20,000 rpm. If the viscosity of the raw material is no more than 5000 mPa ⁇ s at 25 °C, however, there are no limitations on the rotational speed of the rotor, and in this case, allows for adjustment to a broader range of particle size.
  • a method for manufacturing an emulsion or suspension of a silicone oil by emulsifying a silicone oil, an emulsifying agent, and water, in an emulsifier having a rotor that is rotated by a motor and a stator, and which produces an emulsification action by shear force with the rotor.
  • the method is characterized in that the particle size of the emulsion is adjusted by varying the rotational speed of the rotor. It is preferred that the emulsion or suspension particle diameter be adjusted to be within a range of 0.1 to 500 ⁇ m, for example, and in particular, for the volume average diameter of these particles to be within a range of 1 to 100 ⁇ m.
  • Some examples of means for varying the rotational speed of the rotor in the manufacturing method of the invention include (i) methods involving modulating the frequency of the input current to the motor, in order to vary the rotational speed of the rotor, and (ii) methods involving using a transmission to vary the speed at which the rotation of the motor is transmitted, however, the former method (i) is preferred.
  • An inverter can be used as the mechanism for modulating the frequency of the input current to the motor. The inverter is able to vary the rotational speed of the motor directly by modulating the frequency of the input current to the motor, and this feature allows the emulsifier to be more compact.
  • silicone oil used in the manufacturing method of the present invention there are no particular limitations on the silicone oil used in the manufacturing method of the present invention.
  • Some examples include silicone oils with a molecular structure that is cyclic, straight chain, partially branched straight chain, and branched chain.
  • Particular examples of silicone oils include dimethylpolysiloxanes capped at both ends of the molecular chain with trimethylsiloxy groups, dimethylpolysiloxanes capped at both ends of the molecular chain with silanol groups, and cyclic dimethylsiloxanes.
  • silicone oils some of the methyl groups may be substituted with phenyl groups, vinyl groups, 3,3,3-trifluoropropyl groups, 3-aminoaryl groups, and 3-glycidoxypropyl groups.
  • phenyl groups vinyl groups, 3,3,3-trifluoropropyl groups, 3-aminoaryl groups, and 3-glycidoxypropyl groups.
  • viscosity of the silicone oil a range of 5 to 1,000,000 mPa ⁇ s at 25 °C is preferred, with a range of 5 to 5000 mPa ⁇ s being most preferred.
  • emulsifying agent used in the manufacturing method of the present invention.
  • cationic surfactants which can be used include primary to tertiary aliphatic amine salts, alkyltrimethyl ammonium salts, dialkyldimethyl ammonium salts, tetraalkyl ammonium salts, trialkylbenzyl ammonium salts, alkyl pyridinium salts, and polyethylene polyamine fatty acid amide salts.
  • anionic surfactants which can be used include fatty acid salts, alkylbenzene sulfonates, alkyl sulfonates, alkyl naphthalene sulfonates, ⁇ -olefin sulfonates, dialkyl sulfosuccinates, ⁇ -sulfonated fatty acid salts, N-acyl-N-methyllaurate, alkylsulfates, sulfated lipids, polyoxyethylene alkyl ether sulfates, polyoxyethylene alkylphenyl ether sulfates, polyoxyethylene styrenated phenyl ether sulfates, alkylphosphates, polyoxyethylene alkyl ether phosphates, polyoxyethylene alkylphenyl ether phosphates, and naphthalene sulfonate formaldehyde condensates.
  • amphoteric surfactants examples include:
  • nonionic surfactants which can be used include polyoxyethylene alkyl ethers, polyoxyethylene alkenyl ethers, polyoxyethylene alkylphenyl ethers, polyoxyethylene polystyrylphenyl ethers, polyoxyethylene polyoxypropylene glycols, polyoxyethylene polyoxypropylene alkyl ethers, sorbitan fatty acid esters, glycerol fatty acid esters, deca-glycerol fatty acid esters, polyglycerol fatty acid esters, propylene glycol pentaerythritol fatty acid esters, polyhydric alcohol fatty acid partial esters, polyoxyethylene sorbitan fatty acid esters, polyoxyethylene glycerol fatty acid esters, polyoxyethylene polyhydric alcohol fatty acid partial esters, polyoxyethylene fatty acid esters, polyglycerol fatty acid esters, polyoxyethylenated castor oil, fatty acid diethanolamides, polyoxyethylene alkylamines,
  • the water used in the manufacturing method of the present invention can be any of a variety of types of water including ion exchanged water.
  • the silicone oil, the emulsifying agent, and water can each be put into the emulsifier individually, or they can first be mixed and then put into the emulsifier.
  • the particle size of a continuously obtained emulsion can be adjusted by varying the rotational speed of the rotor.
  • the preferred method of varying the rotational speed of the rotor is to modulate the frequency of the input current to the motor.
  • the emulsifying agent be used in an amount of 0.05 to 100 weight parts, and that the water be used in an amount of 20 to 1000 weight parts, each based on 100 weight parts of silicone oil. In these proportions, the stability of the emulsion will be better, More preferably, the amount of the emulsifying agent to be used should be in an amount of 0.1 to 50 weight parts, and the water in an amount of 20 to 1000 weight parts, again each being based on 100 weight parts of silicone oil.
  • An emulsion with a particle size ranging from large to extremely small can be continuously prepared by the manufacturing method of the present invention.
  • the silicone oil emulsion can be used as a raw material for matting agents, defoaming agents, fiber treatment agents, and in cosmetics.
  • the present invention includes a method for manufacturing a suspension of crosslinked silicone particles by (i) emulsifying a liquid crosslinkable silicone composition, an emulsifying agent, and water, in an emulsifier having a rotor that is rotated by a motor and a stator; (ii) producing an emulsification action by shear force with the rotor; (iii) obtaining an emulsion of a liquid crosslinkable silicone composition; and (iv) crosslinking the composition that is emulsified in water.
  • This embodiment is also characterized in that the particle size of the suspension is adjusted by varying the rotational speed of the rotor.
  • the suspension particle diameter be adjusted to within a range of 0.1 to 500 ⁇ m, and that the volume average diameter of the particles be within a range of 1 to 100 ⁇ m.
  • Two examples of the means of varying the rotational speed of the rotor include (i) modulating the frequency of the input current to the motor to vary the rotational speed of the rotor, and (ii) using a transmission to vary the speed at which the rotation of the motor is transmitted.
  • the former means (i) is preferred.
  • An inverter can be used as the mechanism for modulating the frequency of the input current to the motor. The inverter is able to vary the rotational speed of the motor directly by modulating the frequency of the input current to the motor, and this feature allows the emulsifier to be more compact.
  • liquid crosslinkable silicone compositions used in the manufacturing method of this embodiment of the present invention.
  • Some examples include liquid crosslinkable silicone compositions crosslinked by a hydrosilylation reaction, liquid crosslinkable silicone compositions crosslinked by a condensation reaction, liquid crosslinkable silicone compositions crosslinked by ultraviolet irradiation, and liquid crosslinkable silicone compositions crosslinked by an organic peroxide.
  • Liquid crosslinkable silicone compositions crosslinked by a hydrosilylation reaction or by a condensation reaction are most preferred. While there are no particular limitations on the viscosity of the liquid crosslinkable silicone composition, it is preferred it be in the range of 5 to 1,000,000 mPa ⁇ s at 25 °C , most preferably in the range of 5 to 5000 mPa ⁇ s.
  • An example of a silicone composition that can be crosslinked by a hydrosilylation reaction and used in the manufacturing method of the present invention is one composed of at least one (i) organopolysiloxane having two or more alkenyl groups per molecule, an (ii) organopolysiloxane having two or more silicon atom bonded hydrogen atoms per molecule, and (iii) a hydrosilylation reaction catalyst.
  • Alkenyl groups in organopolysiloxane (i) include the vinyl group, allyl group, pentenyl group, and hexenyl group, with the vinyl group being preferred.
  • Organopolysiloxane (i) may contain groups bonded to silicon atoms other than the alkenyl groups such as the methyl group, ethyl group, propyl group, butyl group, or other alkyl group; the cyclopentyl group, cyclohexyl group, or other cycloalkyl group; the phenyl group, tolyl group, xylyl group, or other aryl group; the benzyl group, phenethyl group, 3-phenylpropyl group, or other aralkyl group; the 3-chloropropyl group, 3,3,3-trifluoropropyl group, or other halogen substituted hydrocarbon group; and other monovalent hydrocarbon groups.
  • alkenyl groups such as the methyl group, ethyl group, propyl group, butyl group, or other alkyl group; the cyclopentyl group, cyclohexyl group, or other cycloalkyl
  • Its molecular structure includes linear, cyclic, reticulated, and partially branched linear structures, but to form elastomeric crosslinked silicone particles, the linear or partially branched linear structure is preferred.
  • organopolysiloxane (ii) examples include the same monovalent hydrocarbon groups as listed above.
  • examples of the molecular structure of organopolysiloxane (ii) include linear, cyclic, reticulated, and partially branched linear structures.
  • viscosity of organopolysiloxane (ii) provided it allows the crosslinkable silicone composition to be dispersed in water. A range of 1 to 10,000 mPa ⁇ s at 25 °C is preferred however.
  • the amount of organopolysiloxane (ii) used to prepare the crosslinkable silicone composition should be sufficient to crosslink the composition, and is preferably between 0.3 and 200 weight parts per 100 weight parts of organopolysiloxane (i).
  • a catalyst is required in the hydrosilylation reaction, and the catalyst serves to promote the crosslinking reaction of the crosslinkable silicone composition.
  • the catalyst is platinum-based, and some examples include chloroplatinic acid, an alcohol solution of chloroplatinic acid, an olefin complex of platinum, an alkenylsiloxane complex of platinum, platinum black, and platinum carried on silica.
  • the crosslinkable silicone composition into which the hdrosilylation reaction catalyst has been added can be dispersed in water, or the crosslinkable silicone composition excluding the catalyst may be dispersed in water and then added to the water, which in either case allows the crosslinkable silicone composition containing the catalyst to be prepared in water.
  • an aqueous dispersion containing the hydrosilylation reaction catalyst with an average particle diameter of 1 ⁇ m or less.
  • the amount of catalyst used in the crosslinkable silicone composition should be sufficient to promote the crosslinking reaction of the crosslinkable silicone composition.
  • the amount of platinum metal in the catalyst should be between 1 x 10 -7 and 1 x 10 -3 weight parts per 100 weight parts of organopolysiloxane (i).
  • a suitable composition that can be used in the manufacturing method of the invention is one composed of (i) at least one organopolysiloxane having two or more hydroxyl groups, alkoxy groups, oxime groups, acetoxy groups, aminooxy groups, or other such hydrolyzable groups, which are bonded to silicon atoms in the molecule, (ii) a silane based crosslinking agent having three or more alkoxy groups, oxime groups, acetoxy groups, aminooxy groups, or other such hydrolyzable groups, bonded to silicon atoms in the molecule, and (iii) a condensation reaction catalyst such as an organotin or organotitanium compound.
  • alkoxy groups in organopolysiloxane (i) include the methoxy group, ethoxy group, and methoxyethoxy group.
  • oxime groups include the dimethyl ketoxime group and the methyl ethyl ketoxime group.
  • Examples of some other types of groups which can be bonded to silicon atoms in organopolysiloxane (i) include the methyl group, ethyl group, propyl group, butyl group, and other alkyl groups; the cyclopentyl group, cyclohexyl group, and other cycloalkyl groups; the vinyl group, allyl group, butenyl group, pentenyl group, and hexenyl group; the phenyl group, tolyl group, xylyl group, and other aryl groups; the benzyl group, phenethyl group, 3-phenylpropyl group, and other aralkyl groups; the 3-chloropropyl group, 3,3,3-trifluoropropyl group, and other halogen substituted hydrocarbon groups.
  • organopolysiloxane (i) can be linear, cyclic, reticulated, or it can be partially branched linear. However, to form elastomeric crosslinked silicone particles, a linear or partially branched linear structure is preferred. There are no particular limitations on the viscosity of organopolysiloxane (i) provided it allows the crosslinkable silicone composition to be dispersed in water. A range of 20 to 100,000 mPa ⁇ s at 25 °C is preferred, while a range of 20 to 10,000 mPa ⁇ s is most preferred.
  • silane based crosslinking agent (ii) The alkoxy groups and the oxime groups in the silane based crosslinking agent (ii) are the same as the groups noted above.
  • suitable silane based crosslinking agents (ii) are methyltrimethoxysilane, vinyltrimethoxysilane, methyltrioximesilane, and vinyltrioximesilane.
  • the amount of silane based crosslinking agent (ii) in the crosslinkable silicone composition should be sufficient to crosslink the composition, and is preferably between 0.3 and 200 weight parts per 100 weight parts of organopolysiloxane (i).
  • the condensation reaction catalyst i.e., the organotin or organotitanium compound, promotes the crosslinking reaction of the crosslinkable silicone composition
  • some representative examples include dibutyltin dilaurate, dibutyltin diacetate, tin octenoate, dibutyltin dioctoate, tin laurate, tetrabutyl titanate, tetrapropyl titanate, and dibutoxybis-ethyl acetate.
  • the amount of condensation reaction catalyst used in the crosslinkable silicone composition should be sufficient to crosslink the composition, and is preferably between 0.01 and 5 weight parts per 100 weight parts of organopolysiloxane (i), with a range of 0.05 to 2 weight parts being most preferred.
  • a filler may be included in the crosslinkable silicone composition as an optional component for adjusting the fluidity of the composition or for increasing the mechanical strength of the crosslinked silicone particles obtained.
  • Some examples of fillers include precipitated silica, fumed silica, baked silica, fumed titanium oxide, and other such reinforcing fillers; pulverized quartz, diatomaceous earth, aluminosilicic acid, iron oxide, zinc oxide, calcium carbonate, and other such non-reinforcing fillers.
  • the filler can be one which has been surface treated with hexamethylsilazane, trimethylchlorosilane, polydimethylsiloxane, polymethylhydrogensiloxane, or other organosilicon compound.
  • Nonionic surfactants which can be used include polyoxyethylene alkyl ethers, polyoxyethylene polyoxypropylene alkyl ethers, polyoxyethylene alkylphenyl ethers, polyethylene glycol fatty acid esters, sorbitan fatty acid esters, polyoxyethylene sorbitan fatty acid esters, polyoxyethylene sorbitol fatty acid esters, glycerol fatty acid esters, polyoxyethylene glycerol fatty acid esters, polyglycerol fatty acid esters, propylene glycol fatty acid esters, polyethylene glycol, polypropylene glycol, and ethylene oxide adducts of diethylene glycol trimethylnonanol.
  • anionic surfactants which can be used are hexylbenzene sulfonic acid, octylbenzene sulfonic acid, decylbenzene sulfonic acid, dodecylbenzene sulfonic acid, cetylbenzene sulfonic acid, myristylbenzene sulfonic acid, and the sodium salts of such anionic surfactants.
  • Suitable cationic surfactants include octyltrimethyl ammonium hydroxide, dodecyltrimethyl ammonium hydroxide, hexadecyltrimethyl ammonium hydroxide, octyldimethylbenzyl ammonium hydroxide, decyldimethylbenzyl ammonium hydroxide, dioctadecyldimethyl ammonium hydroxide, tallow trimethyl ammonium hydroxide, and palm oil trimethyl ammonium hydroxide. Mixtures of two or more of these types of surfactants can also be employed. Nonionic surfactants are the most preferred.
  • the water used can be any of a variety of types of water including ion exchanged water.
  • the liquid crosslinkable silicone composition, the emulsifying agent, and water can each be placed in the emulsifier individually, or the components can first be mixed and then placed in the device. It is preferred that the liquid crosslinkable silicone composition first be cooled to 5 °C or less to suppress the crosslinking reaction until the composition is emulsified. More preferred ranges are between -60 °C and +5 °C or between -30 °C and 0 °C.
  • the crosslinkable silicone composition excluding the hydrosilylation reaction catalyst may be emulsified, and the hydrosilylation reaction catalyst can then be added to the emulsion, in which case, the hydrosilylation reaction catalyst should be added as a dispersion with an average particle size of 1 ⁇ m or less.
  • the particle size of the emulsion of the liquid crosslinkable silicone composition can continuously be adjusted by varying the rotational speed of the rotor, and this in turn allows the particle size of a suspension of crosslinked silicone particles to be adjusted.
  • modulating the frequency of the input current to the motor is the preferred method of varying the rotational speed of the rotor.
  • a suspension of crosslinked silicone particles can then be prepared by simply leaving the resulting emulsion of liquid crosslinkable silicone composition at room temperature, heating the suspension, or placing it in a hot water bath, to crosslink the liquid crosslinkable silicone composition emulsified in water.
  • the resulting crosslinked silicone particles should have an elastomeric form such as rubber or gel.
  • the emulsifying agent be used in an amount of 0.05 to 100 weight parts, and water in an amount of 20 to 1000 weight parts, each per 100 weight parts of silicone oil. More preferred ranges are 0.1 to 50 weight parts and 20 to 1000 weight parts, respectively. These ranges should be employed because the stability of the suspension will be poor if the emulsifying agent content is below these ranges, and the use of the suspension will be limited if the ranges are exceeded. In addition, preparation of a uniform suspension is difficult if the water content is below the ranges, and the stability of the suspension decreases if the ranges are exceeded.
  • An emulsion with particle size ranging from large to extremely small can be continuously prepared by the method according to this invention. It can be used as a raw material for matting agents, defoaming agents, fiber treating agents, and in cosmetic applications.
  • viscosity is the value determined at 25 °C
  • the emulsifier device was a type 2F Colloid Mill manufactured by Manton Gaulin in which an inverter, i.e., current frequency modulator, was added to the motor.
  • the rotational speed in revolutions per minute (rpm) of the rotor of the Colloid Mill is the equivalent of about 330 times the frequency of the input current to the motor.
  • the clearance between the rotor and the stator was in graduations of 25.4 ⁇ m (0.001 inch).
  • the particle size of the silicone oil emulsion and the particle size of the crosslinked silicone particle suspension were measured using a laser diffraction particle size distribution meter Model LA-500 manufactured by Horiba. A median diameter was obtained which was is a particle diameter corresponding to 50 % of the cumulative distribution, and this value was used as the volume average particle size.
  • a liquid silicone rubber composition with a viscosity of 300 mPa ⁇ s. was prepared by uniformly mixing into this mixture an isopropyl alcohol solution of chloroplatinic acid. It was added in an amount such that platinum metal atoms in the alcohol solution accounted for 20 ppm weight units with respect to the dimethylvinylsiloxy terminated polydimethylsiloxane.
  • the liquid silicone rubber composition was allowed to stand at room temperature for 1 day.
  • the Type A Durometer Hardness of the silicone rubber was measured according to Japanese Industrial Standard JIS K 6253 and determined to be 29.
  • the total amount of the liquid silicone rubber composition was then mixed with 60 weight parts of an aqueous solution of 1.5 weight percent of polyoxyethylene nonylphenyl ether with an HLB of 13.1.
  • the mixture was emulsified in a colloid mill using three graduations of clearance, in which the frequency of the input current to the motor was 20 Hz, 30 Hz, 40 Hz, and 50 Hz, respectively.
  • four different liquid silicone rubber composition emulsions were prepared. Their characteristics are set forth in Table 1.
  • the emulsions were allowed to stand for 1 day at room temperature to cure the liquid silicone rubber composition and prepare silicone rubber particle suspensions. Their characteristics are also set forth in Table 1.
  • Working Example 1 was repeated in all respects, except that a Colloid Mill without an inverter was used in which the frequency of input current to the motor remained at 50 Hz. The clearance graduations were also changed to 10. Characteristics of the emulsion are set forth in Table 1. The emulsion was allowed to stand for 1 day at room temperature to cure the liquid silicone rubber composition and prepare a silicone rubber particle suspension. Its characteristics are also set forth in Table 1. Working Examples Comparative Example Rotational speed of rotor, rpm 6600 9900 13,200 16,500 16,500 Volume average particle size, ⁇ m Emulsion Suspension 12.3 12.7 10.5 11.1 7.8 8.0 3.4 3.6 4.1 4.3 200 mesh remainder, wt % 0.3 0.2 0.2 0.2 0.3

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
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  • Compositions Of Macromolecular Compounds (AREA)
  • Processes Of Treating Macromolecular Substances (AREA)
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  • Silicon Polymers (AREA)
EP00309249A 1999-10-20 2000-10-20 Emulgiervorrichtung und Verfahren zur Herstellung von Silikonölemulsion oder Suspension von vernetzten Silikonpartikeln Withdrawn EP1093843A1 (de)

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JP29861799 1999-10-20
JP29861799A JP2001113147A (ja) 1999-10-20 1999-10-20 乳化機、およびシリコーンオイルエマルジョンもしくは架橋シリコーン粒子サスペンジョンの製造方法

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US7448793B2 (en) * 2007-01-26 2008-11-11 Value Supplier & Developer Corporation Emulsion production apparatus
CN109015800A (zh) * 2018-08-10 2018-12-18 芜湖维软新材料有限公司 一种硅油碾平切块装置

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20030143176A1 (en) * 2002-01-25 2003-07-31 Yihan Liu Compositions containing silicone oil-in-water emulsions, salts, alcohols and solvents
JP4749677B2 (ja) * 2004-04-13 2011-08-17 旭化成ワッカーシリコーン株式会社 シリコーンエマルション組成物
JPWO2011052695A1 (ja) 2009-11-02 2013-03-21 信越化学工業株式会社 球状炭化ケイ素粉末、その製造方法、及びそれを使用する炭化ケイ素セラミックス成形体の製造方法
JP5630333B2 (ja) 2011-03-08 2014-11-26 信越化学工業株式会社 易焼結性炭化ケイ素粉末及び炭化ケイ素セラミックス焼結体
KR20170091605A (ko) * 2014-11-25 2017-08-09 신토고교 가부시키가이샤 분산 장치 및 분산 방법
JP7053156B2 (ja) * 2017-03-17 2022-04-12 株式会社明治 起泡性水中油中水型乳化物及びその製造方法

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2742229A1 (de) * 1977-08-31 1979-03-08 Escher Wyss Gmbh Verfahren zur bestimmung von eigenschaften von in suspension befindlichen papierstoffasern sowie messvorrichtung zur ausfuehrung des verfahrens
FR2454094A1 (fr) * 1979-03-27 1980-11-07 Sredneaziat Nii Prirod Gaza Procede de controle du processus de dispersion d'une phase solide dans une phase liquide
US4380503A (en) * 1980-07-01 1983-04-19 Th. Goldschmidt Ag Process for preparing oil-in-water emulsion
GB2120565A (en) * 1982-05-29 1983-12-07 Janke & Kunkel Gmbh Co Kg Stirring apparatus
DE3221476A1 (de) * 1982-06-07 1983-12-08 Probst & Class Gmbh & Co Kg, 7550 Rastatt Kolloidmuehle
US4589598A (en) * 1984-10-12 1986-05-20 Beloit Corporation Apparatus for controlling a variable speed gearmotor
US4963778A (en) * 1986-12-13 1990-10-16 Grundfos International A/S Frequency converter for controlling a motor
JPH05123592A (ja) * 1991-11-06 1993-05-21 Topy Ind Ltd クリアランス自動調整式コロイドミル
CH683322A5 (de) * 1991-11-18 1994-02-28 Glatt Maschinen & Apparatebau Einrichtung und Verfahren zum Emulgieren eines Gutes.

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2742229A1 (de) * 1977-08-31 1979-03-08 Escher Wyss Gmbh Verfahren zur bestimmung von eigenschaften von in suspension befindlichen papierstoffasern sowie messvorrichtung zur ausfuehrung des verfahrens
FR2454094A1 (fr) * 1979-03-27 1980-11-07 Sredneaziat Nii Prirod Gaza Procede de controle du processus de dispersion d'une phase solide dans une phase liquide
US4380503A (en) * 1980-07-01 1983-04-19 Th. Goldschmidt Ag Process for preparing oil-in-water emulsion
GB2120565A (en) * 1982-05-29 1983-12-07 Janke & Kunkel Gmbh Co Kg Stirring apparatus
DE3221476A1 (de) * 1982-06-07 1983-12-08 Probst & Class Gmbh & Co Kg, 7550 Rastatt Kolloidmuehle
US4589598A (en) * 1984-10-12 1986-05-20 Beloit Corporation Apparatus for controlling a variable speed gearmotor
US4963778A (en) * 1986-12-13 1990-10-16 Grundfos International A/S Frequency converter for controlling a motor
JPH05123592A (ja) * 1991-11-06 1993-05-21 Topy Ind Ltd クリアランス自動調整式コロイドミル
CH683322A5 (de) * 1991-11-18 1994-02-28 Glatt Maschinen & Apparatebau Einrichtung und Verfahren zum Emulgieren eines Gutes.

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
PATENT ABSTRACTS OF JAPAN vol. 017, no. 489 6 September 1993 (1993-09-06) *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7448793B2 (en) * 2007-01-26 2008-11-11 Value Supplier & Developer Corporation Emulsion production apparatus
CN109015800A (zh) * 2018-08-10 2018-12-18 芜湖维软新材料有限公司 一种硅油碾平切块装置
CN109015800B (zh) * 2018-08-10 2020-07-28 芜湖维软新材料有限公司 一种硅油碾平切块装置

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