WO2016125348A1 - Procédé de production d'une composition d'émulsion d'organopolysiloxane - Google Patents

Procédé de production d'une composition d'émulsion d'organopolysiloxane Download PDF

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WO2016125348A1
WO2016125348A1 PCT/JP2015/080197 JP2015080197W WO2016125348A1 WO 2016125348 A1 WO2016125348 A1 WO 2016125348A1 JP 2015080197 W JP2015080197 W JP 2015080197W WO 2016125348 A1 WO2016125348 A1 WO 2016125348A1
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emulsion composition
parts
organopolysiloxane
emulsion
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PCT/JP2015/080197
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Japanese (ja)
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亮広 小林
拓矢 安部
有子 高田
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信越化学工業株式会社
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/04—Polysiloxanes
    • C08G77/06—Preparatory processes

Definitions

  • the present invention relates to a method for producing an organopolysiloxane emulsion composition useful in various fields such as cosmetics, household care compositions, mold release agents and the like.
  • Patent Documents 1 and 2 Japanese Patent Publication No. 34-2041, Japanese Patent Publication No. 41-13395.
  • Patent Documents 1 and 2 Japanese Patent Publication No. 34-2041, Japanese Patent Publication No. 41-13395.
  • Patent Documents 1 and 2 Japanese Patent Publication No. 34-2041, Japanese Patent Publication No. 41-13395.
  • emulsion polymerization is carried out in the presence of an acid catalyst at a temperature below 40 ° C.
  • the method of performing is known (see Patent Document 3: Japanese Patent No. 5382273), and when these methods are used, an emulsion in which the amount of octamethylcyclotetrasiloxane contained in the organopolysiloxane is 3,000 ppm or less is obtained. be able to.
  • the stability of the obtained emulsion over time may be poor.
  • an object of the present invention is to provide a method for producing an organopolysiloxane emulsion composition having a low octamethylcyclotetrasiloxane content in the organopolysiloxane and having good temporal stability.
  • the present inventors have (A) both-end hydroxy group blocking represented by the formula (1) described later and having an octamethylcyclotetrasiloxane content of 1,000 ppm or less.
  • a mixture containing diorganopolysiloxane, (B) nonionic surfactant and / or (C) anionic surfactant, and (D-1) water is emulsified to prepare a first emulsion composition. If necessary, (D-2) water is added to the obtained first emulsion composition, and (E) the cation contained in the emulsion composition is exchanged with hydrogen ions using a cation exchange resin.
  • the present invention provides the following method for producing an organopolysiloxane emulsion composition.
  • (I) (A) Both end hydroxy group-blocked diorganopolysiloxane represented by the following general formula (1) and having an octamethylcyclotetrasiloxane content of 1,000 ppm or less: 100 parts by mass HO (R 1 2 SiO) n H (1) (Wherein R 1 is independently a hydrogen atom or an unsubstituted or substituted monovalent hydrocarbon group having 1 to 20 carbon atoms, and n is the viscosity at 25 ° C. of the hydroxy-blocked diorganopolysiloxane at both ends.
  • Nonionic surfactant 0 to 100 parts by mass
  • anionic surfactant 0 to 100 parts by mass
  • the total amount of the components (B) and (C) is 0.1 parts by mass or more.
  • a method for producing an organopolysiloxane emulsion composition comprising preparing a target emulsion composition having an amount of 3,000 ppm or less.
  • an organopolysiloxane emulsion composition having a high viscosity and containing a high viscosity organopolysiloxane having a low octamethylcyclotetrasiloxane content.
  • the component (A) is a diorganopolysiloxane having both terminal hydroxy groups blocked and represented by the following general formula (1) and having an octamethylcyclotetrasiloxane content of 1,000 ppm or less.
  • HO (R 1 2 SiO) n H (1) (Wherein R 1 is independently a hydrogen atom or an unsubstituted or substituted monovalent hydrocarbon group having 1 to 20 carbon atoms, and n is the viscosity at 25 ° C. of the hydroxy-blocked diorganopolysiloxane at both ends. (The number is 20 to 20,000 mPa ⁇ s.)
  • R 1 is independently a hydrogen atom or an unsubstituted or substituted monovalent hydrocarbon group having 1 to 20 carbon atoms.
  • the unsubstituted monovalent hydrocarbon group having 1 to 20 carbon atoms include, for example, an alkyl group having 1 to 20 carbon atoms, a cycloalkyl group having 3 to 20 carbon atoms, and an alkenyl group having 2 to 20 carbon atoms.
  • alkyl groups such as methyl, ethyl, propyl, butyl, pentyl, hexyl, heptyl, octyl, nonyl, decyl, dodecyl, tetradecyl, hexadecyl, octadecyl, etc.
  • Cycloalkyl groups such as cyclopentyl group and cyclohexyl group, alkenyl groups such as vinyl group and allyl group, and aryl groups such as phenyl group, tolyl group and naphthyl group.
  • a part of the hydrogen atoms in the monovalent hydrocarbon group having 1 to 20 carbon atoms exemplified above may be a halogen atom, an amino group, or an acryloxy group. And those substituted with a methacryloxy group, an epoxy group, a mercapto group, a carboxyl group, a hydroxy group, and the like.
  • a monovalent hydrocarbon group having 1 to 6 carbon atoms is preferable, for example, a methyl group, an ethyl group, a propyl group, a butyl group, or a phenyl group. More preferably, 80 mol% or more of the total R 1 is a methyl group.
  • n is a number at which the viscosity at 25 ° C. of the hydroxy-terminated diorganopolysiloxane at 20 ° C. is 20 to 20,000 mPa ⁇ s, preferably 35 to 10,000 mPa ⁇ s, and preferably 350 to 6,000 mPa ⁇ s. Is more preferable. If the viscosity is less than 20 mPa ⁇ s, it may be necessary to increase the time of emulsion polymerization in order to obtain the desired viscosity of the organopolysiloxane contained in the target emulsion composition, or it may be a by-product during emulsion polymerization.
  • the viscosity is a value at 25 ° C. measured with a rotational viscometer (hereinafter the same).
  • the content of octamethylcyclotetrasiloxane in the (A) component-terminated hydroxy-blocked diorganopolysiloxane is 1,000 ppm (mass ppm, the same applies hereinafter) or less, more preferably 500 ppm or less.
  • the lower limit is not particularly limited, and may be 0 ppm. If the content of octamethylcyclotetrasiloxane in the both-end hydroxy-blocked diorganopolysiloxane exceeds 1,000 ppm, the amount of octamethylcyclotetrasiloxane in the resulting emulsion composition is made 3,000 ppm or less. It becomes difficult.
  • the octamethylcyclotetrasiloxane in component can be made into content of 1,000 ppm or less by removing by means, such as vacuum distillation, by a conventional method.
  • Nonionic surfactant examples include polyoxyalkylene alkyl ether, polyoxyalkylene alkyl phenyl ether, polyoxyalkylene alkyl ester, polyoxyalkylene sorbitan alkyl ester, polyethylene glycol, polypropylene glycol, diethylene glycol and the like. Alternatively, two or more kinds can be appropriately selected and used. Especially, what is represented by the following general formula (2) is preferable.
  • R 2 O (EO) p (PO) q H (2) (In the formula, R 2 is a linear or branched alkyl group having 8 to 30 carbon atoms, EO represents an ethylene oxide group, PO represents a propylene oxide group, and the arrangement thereof may be block or random. p and q are each independently an integer of 0 to 100, provided that p + q> 0.)
  • R 2 is a linear or branched alkyl group having 8 to 30 carbon atoms, preferably a linear or branched alkyl group having 8 to 13 carbon atoms, and p and q are Independently an integer of 0 to 100 and p + q> 0, preferably independently an integer of 0 to 25 and 0 ⁇ p + q ⁇ 50.
  • the amount of component (B) used is 0 to 100 parts by mass with respect to 100 parts by mass of component (A). That is, the addition of the component (B) is optional, and it is not necessary to add it. Part, more preferably 3 to 20 parts by weight. When the amount of the component (B) used is more than 100 parts by mass, the stability over time of the intended emulsion composition is deteriorated.
  • anionic surfactant of (C) component the following are mentioned, for example, 1 type can be used individually or in combination of 2 or more types.
  • Alkyl sulfate R 3 OSO 3 M represented by the following general formula (3) (3) Wherein R 3 is a linear or branched alkyl group having 6 to 30 carbon atoms, M is an alkali metal ion such as potassium, sodium or lithium, an alkaline earth metal ion such as magnesium or calcium, or ammonium An ion or a tertiary ammonium ion such as triethanolammonium.)
  • R 3 is a linear or branched alkyl group having 6 to 30 carbon atoms, and preferably a linear or branched alkyl group having 6 to 12 carbon atoms.
  • M is an alkali metal ion such as potassium, sodium or lithium; an alkaline earth metal ion such as magnesium or calcium; a tertiary ammonium ion such as ammonium ion or triethanolammonium; Ions, ammonium ions, and triethanolammonium ions are preferred.
  • alkyl sulfate represented by the general formula (3) examples include hexyl sulfate, octyl sulfate, decyl sulfate, dodecyl sulfate, tetradecyl sulfate, hexadecyl sulfate, octadecyl sulfate, icosyl sulfate lithium salt, sodium salt, potassium salt And alkaline earth metal salts such as magnesium salts and calcium salts, triethanolammonium salts and ammonium salts.
  • Alkylbenzenesulfonate represented by the following general formula (4) R 3 —C 6 H 4 —SO 3 M (4) Wherein R 3 is a linear or branched alkyl group having 6 to 30 carbon atoms as defined in the general formula (3), and M is potassium, sodium as defined in the general formula (3) And alkali metal ions such as lithium, alkaline earth metal ions such as magnesium and calcium, and ammonium ions or tertiary ammonium ions such as triethanolammonium.)
  • R 3 is as defined in the general formula (3), and is preferably a linear or branched alkyl group having 6 to 12 carbon atoms.
  • M is as defined in the above general formula (3), and sodium ion, potassium ion, ammonium ion, and triethanolammonium ion are preferable from the emulsifying effect.
  • alkylbenzenesulfonate represented by the general formula (4) examples include hexylbenzenesulfonic acid, octylbenzenesulfonic acid, decylbenzenesulfonic acid, dodecylbenzenesulfonic acid, tetradecylbenzenesulfonic acid, hexadecylbenzenesulfonic acid. And the like.
  • Higher fatty acid salt examples include lithium salts such as lauric acid, stearic acid, oleic acid, and linolenic acid, alkali metal salts such as sodium salt and potassium salt, and alkalis such as magnesium salt and calcium salt. Examples include earth metal salts, triethanolammonium salts, and ammonium salts.
  • R 3 is a linear or branched alkyl group having 6 to 30 carbon atoms as defined in the general formula (3), and M is potassium, sodium as defined in the general formula (3) , Alkali metal ions such as lithium, alkaline earth metal ions such as magnesium and calcium, ammonium ions or tertiary ammonium ions such as triethanolammonium, etc.
  • EO represents an ethylene oxide group
  • PO represents a propylene oxide group
  • the arrangement may be block or random, i and j are independently integers from 0 to 100, provided that i + j> 0.
  • R 3 is as defined in the general formula (3), and is preferably a linear or branched alkyl group having 6 to 12 carbon atoms.
  • M is as defined in the above general formula (3), and sodium ion, potassium ion, ammonium ion, and triethanolammonium ion are preferable from the emulsifying effect.
  • i and j are each independently an integer of 0 to 100, i + j> 0, preferably independently an integer of 0 to 50, and 1 ⁇ i + j ⁇ 100.
  • polyoxyethylene alkyl ether sulfate examples include polyoxyethylene hexyl ether sulfate, polyoxyethylene octyl ether sulfate, polyoxyethylene decyl ether sulfate, polyoxyethylene dodecyl ether sulfate, polyoxyethylene tetradecyl ether sulfate, Oxyethylene hexadecyl ether sulfate, polyoxyethylene octadecyl ether sulfate, polyoxyethylene icosyl ether sulfate lithium salts, alkali metal salts such as sodium salts and potassium salts, alkaline earth metal salts such as magnesium salts and calcium salts, Examples include ethanol ammonium salt and ammonium salt.
  • EO, PO, i, j are defined by the general formula (5) As described above, EO represents an ethylene oxide group, PO represents a propylene oxide group, and the arrangement thereof may be block or random, i and j are independently integers of 0 to 100, provided that i + j> 0. )
  • R 3 is as defined in the general formula (3), and is preferably a linear or branched alkyl group having 6 to 12 carbon atoms.
  • M is as defined in the above general formula (3), and sodium ion, potassium ion, ammonium ion, and triethanolammonium ion are preferable from the emulsifying effect.
  • i and j are each independently an integer of 0 to 100, i + j> 0, preferably independently an integer of 0 to 50, and 1 ⁇ i + j ⁇ 100.
  • polyoxyethylene alkyl phenyl ether sulfate ester salt examples include polyoxyethylene hexyl phenyl ether sulfate, polyoxyethylene octyl phenyl ether sulfate, polyoxyethylene decyl phenyl ether sulfate, polyoxyethylene dodecyl phenyl ether sulfate, polyoxyethylene Tetradecyl phenyl ether sulfate, polyoxyethylene hexadecyl phenyl ether sulfate lithium salt, sodium salt, potassium salt and other alkali metal salts, magnesium salt, calcium salt and other alkaline earth metal salts, triethanol ammonium salt, ammonium salt, etc. Is mentioned.
  • the amount of component (C) used is 0 to 100 parts by mass with respect to 100 parts by mass of component (A). That is, the addition of the component (C) is optional, and it is not necessary to add it. When it is added, it is added in a range of 100 parts by mass or less, preferably 0.1 to The amount is 25 parts by mass, more preferably 0.5 to 15 parts by mass. If the amount of component (C) used is more than 100 parts by mass, the stability over time of the intended emulsion composition will be poor.
  • the total amount of (B) and (C) component is 0.1 mass part or more with respect to 100 mass parts of (A) component, although an upper limit is not specifically limited, It is 200 mass parts or less.
  • the amount is preferably 0.1 to 100 parts by mass with respect to 100 parts by mass of component (A). If the total amount of the components (B) and (C) is less than 0.1 parts by mass with respect to 100 parts by mass of the component (A), the average particle size of the emulsion particles of the intended emulsion composition to be obtained is 300 nm or less. Have difficulty.
  • step (I) the amount of component (D-1) used is 1 to 10,000 parts by weight per 100 parts by weight of component (A), and an emulsifier used to reduce the size of emulsion particles It depends on the type.
  • the amount of the component (D-1) used when using an emulsifier such as a high-pressure homogenizer that reduces the particle size of the emulsion particles using pressure is 1 to 10,000 with respect to 100 parts by mass of the component (A).
  • Part by mass is preferred, more preferably 4 to 6,000 parts by mass, and still more preferably 6 to 4,000 parts by mass.
  • emulsification such as homodispers, homomixers, and colloid mills (machines that feed and emulsify each component into the gap between a high-speed rotating disk and a fixed disk) that reduce the size of emulsion particles using shear force
  • the amount of component (D-1) used when using a machine is preferably 1 to 10 parts by weight, more preferably 2 to 9 parts by weight, even more preferably 4 to 4 parts by weight per 100 parts by weight of component (A). 8 parts by mass.
  • the component (D-2) may or may not be added, but when added, it is 10,000 parts by weight or less with respect to 100 parts by weight of the component (A). 0.1 to 1,000 parts by mass is preferable. If the amount of component (D-2) exceeds 10,000 parts by mass, the stability of the target emulsion composition obtained will deteriorate with time.
  • the cation exchange resin as component (E) serves as a polymerization catalyst for emulsion polymerization and is used for exchanging cations in the emulsion composition obtained in step (I) described later to hydrogen ions.
  • a cation exchange resin By using a cation exchange resin, the effect of improving the temporal stability of the intended emulsion composition is obtained by exchanging cations in the system with hydrogen ions.
  • the cation exchange resin preferably has a sulfonic acid group or a carboxylic acid group as a functional group for performing ion exchange on the resin matrix.
  • styrene represented by the following formula (7) and the following formula ( 8) a strongly acidic cation-type exchange resin obtained by sulfonating a polymer compound obtained by copolymerization with 1,4-divinylbenzene represented by the formula (1), or a 1,4-divinylbenzene represented by the following formula (8):
  • Both are spherical synthetic resins having a diameter of 0.5 to 1 mm having a functional group for ion exchange in the resin matrix, and can exchange the cation held by itself with the cation in the emulsion composition.
  • Component (E) is used in an amount of 0.1 to 100 parts by weight, preferably 0.1 to 50 parts by weight, more preferably 0.1 to 25 parts by weight per 100 parts by weight of component (A). Part. (E) When the amount of component used is too small, it takes a long time to polymerize the organopolysiloxane contained in the desired emulsion composition to the desired viscosity, and when it is too much, the desired emulsion composition is obtained. The stability over time becomes worse.
  • a column type After the cation exchange resin is packed into the column, the emulsion composition is passed through the column at a desired flow rate.
  • a cation exchange resin is added to the emulsion composition, and after stirring for a desired time, the cation exchange resin is removed by filtration.
  • a first emulsion composition is prepared by emulsifying a mixture containing the component (A), the component (B) and / or the component (C), and the component (D). Specifically, it includes (A), (B), (C) and (D) components, (A), (B) and (D) components, or (A), (C) and (D) components.
  • the mixture is emulsified to obtain a first emulsion composition.
  • the emulsification here can be carried out using an emulsifier such as a homodisper, homomixer, colloid mill, line mixer, universal mixer, ultramixer, planetary mixer, combimix, high pressure homogenizer and the like.
  • the emulsification temperature is preferably 1 to 80 ° C.
  • the cyclization reaction also proceeds at the same time. Therefore, it is preferable to emulsify at a temperature of less than 40 ° C. If emulsification is carried out at a temperature of 40 ° C. or higher, the production of octamethylcyclotetrasiloxane may increase. Therefore, it is preferably 5 to 30 ° C, more preferably 10 to 25 ° C.
  • the average particle size of the emulsion particles of the first emulsion composition is preferably 300 nm or less, more preferably 200 nm or less, and even more preferably 150 nm or less. And mix.
  • the average particle size of the final emulsion particles obtained in the next step is also 300 nm or less.
  • a minimum is not specifically limited, It is preferable that it is 20 nm or more.
  • the average particle diameter of the emulsion particles is a median diameter value measured by a laser diffraction / scattering method (hereinafter the same).
  • (D) component when added to a 1st emulsion composition in process (II), it can further emulsify and disperse
  • emulsifiers such as a homomixer and a high-pressure homogenizer
  • the component (E) As a method of exchanging cations contained in the emulsion composition with hydrogen ions using the component (E), for example, after adding the component (E) to the emulsion composition, preferably 1 to 40 ° C. The mixture is preferably stirred at 5 to 30 ° C., preferably 5 minutes to 6 hours, more preferably 30 minutes to 3 hours. Thereafter, the cation exchange resin is removed by filtration such as mesh filtration.
  • the emulsion composition in which cations are exchanged with hydrogen ions is subjected to emulsion polymerization.
  • the polymerization step is carried out at a temperature below 40 ° C. within 48 hours.
  • a temperature of 40 ° C. or higher there is a risk that the production of octamethylcyclotetrasiloxane will increase. Therefore, 1 to 25 ° C. is preferable, and 5 to 15 ° C. is more preferable.
  • the polymerization time exceeds 48 hours, the production of octamethylcyclotetrasiloxane may increase, so 1 to 40 hours is preferable, and 5 to 30 hours is more preferable.
  • Emulsion polymerization is started from the time when the component (E) is added to the emulsion composition, and the cation contained in the emulsion composition is exchanged with hydrogen ions by the component (E). Since the polymerization reaction further proceeds, the polymerization reaction proceeds even after the component (E) is removed.
  • the viscosity at 25 ° C. of the organopolysiloxane produced by emulsion polymerization in step (II) is at least 3 times the viscosity at 25 ° C. of the component (A) used, preferably 50,000 mPa ⁇ s or more, more preferably 100,000 mPa ⁇ s or more. Although an upper limit is not specifically limited, It is preferable that it is 20 million mPa * s or less.
  • the obtained emulsion composition is usually neutralized with a basic substance.
  • the basic substance include amine compounds such as sodium hydroxide, potassium hydroxide, sodium hydrogen carbonate, triethanolamine, and triethylamine.
  • water can be added to adjust the silicone concentration, and antiseptics, antifungal agents, and the like can be added to improve the storage stability of the emulsion composition.
  • R 4 3 Si By adding alkoxysilanes such as R 4 2 Si (OR 5 ) 2 and R 4 Si (OR 5 ) 3 , it is possible to introduce branch units and various functional groups into the resulting organopolysiloxane chain. is there.
  • R 4 is independently a hydrogen atom or an unsubstituted or substituted monovalent hydrocarbon group having 1 to 20, preferably 1 to 6 carbon atoms.
  • Examples of the monovalent hydrocarbon group include: Examples thereof include a methyl group, an ethyl group, a propyl group, a butyl group, and a phenyl group.
  • R 5 is independently a hydrogen atom or an alkyl group having 1 to 20 carbon atoms, preferably 1 to 6 carbon atoms.
  • Examples of the alkyl group include a methyl group, an ethyl group, a propyl group, and a butyl group.
  • the viscosity of the organopolysiloxane in the obtained emulsion composition at 25 ° C. is at least 3 times the viscosity of the component (A) used at 25 ° C., preferably 50,000 mPa ⁇ s or more, and 100,000 mPa -More than s is more preferable.
  • an upper limit is not specifically limited, It is preferable that it is 20 million mPa * s or less, and it is more preferable that it is about 10 million mPa * s or less.
  • the polymerization step in emulsion polymerization of the emulsion composition in the above production step is performed at a temperature of less than 40 ° C. This can be achieved by carrying out within 48 hours.
  • the average particle size of the emulsion particles of the obtained target emulsion composition is preferably 300 nm or less, and more preferably 200 nm or less. Although a minimum is not specifically limited, It is preferable that it is about 20 nm or more. When the average particle diameter of the emulsion particles is larger than 300 nm, the stability of the emulsion composition obtained over time may deteriorate. According to the production method of the present invention, the average particle size of the emulsion particles of the emulsion composition is 300 nm or less, and a very fine product is obtained.
  • a mixture containing the component (A), the component (B) and / or the component (C), and the component (D) is emulsified in the production process.
  • an emulsifier such as a homodisper, a homomixer, a colloid mill, a line mixer, a universal mixer, an ultra mixer, a planetary mixer, a combination mix, a high-pressure homogenizer, and the like.
  • the content of octamethylcyclotetrasiloxane contained in the organopolysiloxane in the obtained emulsion composition is 3,000 ppm or less, preferably 2,000 ppm or less, and 1,000 ppm or less. Is more preferable.
  • the lower limit is not particularly limited and is 0 ppm or more.
  • it can achieve by performing the superposition
  • the content of decamethylcyclopentasiloxane contained in the organopolysiloxane in the obtained emulsion composition is preferably 3,000 ppm or less, more preferably 2,000 ppm or less, and 1,000 ppm. More preferably, it is as follows.
  • the lower limit is not particularly limited and is 0 ppm or more.
  • Example 1 (A) 100 parts of an organopolysiloxane having a silanol group at the molecular chain terminal with a viscosity of 5,000 mPa ⁇ s (octamethylcyclotetrasiloxane content of 50 ppm or less), (B) polyoxyethylene tridecyl ether (EO 10 mol) 10 parts, (C) 4 parts of triethanolamine dodecylbenzenesulfonate, and (D-1) 8 parts of water are added and emulsified with a homodisper at 40 ° C., and the average particle size of the emulsion particles is 130 nm. An emulsion was obtained.
  • Example 2 (A) 100 parts of an organopolysiloxane having a silanol group at the molecular chain terminal with a viscosity of 5,000 mPa ⁇ s (octamethylcyclotetrasiloxane content of 50 ppm or less), (B) polyoxyethylene tridecyl ether (EO 10 mol) 10 parts, (C) 4 parts of sodium dodecylbenzenesulfonate, and (D-1) 8 parts of water were added and emulsified at 40 ° C. by a colloid mill to give an emulsion having an average particle size of 110 nm. Obtained.
  • Example 3 (A) 100 parts of an organopolysiloxane having a viscosity of 5,000 mPa ⁇ s and having a silanol group at the molecular chain end (octamethylcyclotetrasiloxane content of 50 ppm or less), (C) 8 parts of triethanolamine dodecylbenzenesulfonate, (D-1) 6 parts of water was added and emulsified with a homodisper at 40 ° C. to obtain an emulsion having an average particle diameter of the emulsion particles of 180 nm. To the obtained emulsion, (D-2) 125.2 parts of water was added and diluted and dispersed with a homomixer.
  • Average particle size of emulsion particles The average particle diameter of the emulsion particles in the prepared emulsion composition was measured. The average particle diameter is a median diameter value measured with a laser diffraction / scattering particle size distribution analyzer LA-920 (manufactured by Horiba, Ltd.).
  • the organopolysiloxane emulsion composition obtained by the production method of the present invention is particularly useful as a cosmetic or household care product because it is excellent in stability over time and feeling in use.
  • hair care such as shampoo and rinse. Available for supplies.
  • It can also be used as protective materials for furniture and sundries, mold release agents for processing rubber products and plastic products, and fiber treatment agents for the purpose of imparting water repellency and flexibility to fibers. It is.

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Abstract

La présente invention concerne un procédé de production d'une composition d'émulsion d'organopolysiloxane qui est petite en termes de quantité d'octaméthyl cyclotétrasiloxane (D4) dans un polysiloxane et qui présente une bonne stabilité à long terme. La présente invention décrit un procédé de production d'une composition d'émulsion d'organopolysiloxane, dans lequel : (I) une composition d'émulsion est obtenue par émulsification d'un mélange qui contient (A) un organopolysiloxane représenté par HO(R1 2SiO)nH (1) (R1 représente H ou un groupe hydrocarbure monovalent et n représentant un nombre qui permet d'obtenir de 20 à 20 000 Pa·s) et ayant une quantité D4 de 1 000 ppm ou moins, (B) un tensioactif non ionique et/ou (C) un tensioactif anionique, et (D-1) de l'eau; et (II) après l'échange des cations contenus dans la composition ainsi obtenue par des ions hydrogène avec l'utilisation de (E) une résine d'échange de cations, la composition est émulsifiée et polymérisée à une température inférieure à 40°C, préparant de là une composition dans laquelle la viscosité d'un polysiloxane produit est trois fois ou plus celle du constituant (A) et la quantité D4 contenue dans le polysiloxane est de 3 000 ppm ou moins.
PCT/JP2015/080197 2015-02-05 2015-10-27 Procédé de production d'une composition d'émulsion d'organopolysiloxane WO2016125348A1 (fr)

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Cited By (1)

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Publication number Priority date Publication date Assignee Title
JPWO2021132057A1 (fr) * 2019-12-24 2021-07-01

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