JPH0445154A - Silicone emulsion composition for forming protection film - Google Patents

Abstract

PURPOSE:To obtain an O/W-type silicone emulsion composition capable of forming a protection film by emulsifying a composition composed of a high- molecular weight organopolysiloxane and a low-boiling oil with an anionic surfactant, a polyhydric alcohol and water. CONSTITUTION:The objective composition is produced by emulsifying (A) 100pts. wt. of a composition composed of (A1) 1-50pts.wt. of an organopolysiloxane of formula [R<1> is (substituted)univalent hydrocarbon group; R<2> is H, methyl, vinyl, phenyl, etc.; (m) is integer of 2,300-20,000] and (A2) 99-50pts.wt. of a low- boiling oil capable of dissolving the component A1 (e.g. siloxane having low molecular weight), (B) 1-30pts.wt. of an anionic surfactant composed of a polyoxyethylene alkyl ether carboxylic acid (salt), (C) 1-100pts.wt. of a polyhydric alcohol and (D) >=10pts.wt. of water based on 100pts.wt. of A+B+C or >=20pts.wt. of water and <=25% (based on the total composition) of a lower alcohol.

Description

[Detailed Description of the Invention] [Industrial Application Field] The present invention provides a protective film-forming silicone emulsion composition,
In particular, when water, low-boiling point oils, and lower alcohols are volatilized, a silicone rubber film is formed on the container, so it is useful as a mold release agent, polishing agent, fiber treatment agent, and cosmetic agent when coated on a base material. The present invention relates to a protective film-forming silicone emulsion composition.

[Prior art] Silicone emulsions include those obtained by emulsifying and dispersing organopolysiloxane oil using a surfactant.
It is applied in many fields such as antifoaming agents, fiber treatment agents, mold release agents, polishing agents, and cosmetics.

However, since this organopolysiloxane oil is mainly composed of dimethylpolysiloxane, it has a low surface tension and strong hydrophobicity, making it difficult to emulsify and disperse it. During phase inversion from O/W type to O/W type, a stable emulsion cannot be obtained unless emulsification and dispersion is performed using a physical energy imparting machine such as a colloid mill, homomixer or homogenizer.
Organopolysiloxanes that can be emulsified and dispersed using this method can only be emulsified and phase-inverted within the range of viscosity that is within the range of physical energy that is possible due to the structure of the equipment. Even if you use a combination mix or a sand grinder, which is said to be able to emulsify by applying cutting energy, the viscosity is at most 500,000 ml.
It is said to be up to 000cS (Japanese Patent Application Laid-Open No. 1092-1092)
No. 27, JP-A No. 63125530).

On the other hand, methods for emulsifying and dispersing high molecular weight organopolysiloxanes include emulsifying and dispersing low molecular weight organopolysiloxanes and then adding a strong acid or strong alkali catalyst to polymerize them (see Japanese Patent Publication No. 34-2041);
A method in which low molecular weight organopolysiloxane is emulsified and dispersed using a catalytically active surfactant, and then polymerized (
(see Japanese Patent Publication No. 18800/1982), and a method of diluting a high molecular weight organopolysiloxane with an aromatic organic solvent such as benzene, toluene, or coconut, and then emulsifying and dispersing it (see Japanese Patent Publication No. 1258/1989). 1986-12
No. 59, Japanese Patent Publication No. 63-45748) is known, which is a method for making cosmetics by mixing a high molecular weight organopolysiloxane with a degree of polymerization of 3,000 or more with a low boiling point oil and emulsifying the mixture. (Unexamined Japanese Patent Publication No. 183515/1983,
JP-A No. 63-183516), and a method for producing a stable solubilized product of a highly viscous silicone compound such as a raw rubber region consisting of an organopolysiloxane, a cyclic organopolysiloxane, a surfactant, and water (see JP-A-63-183516). (See Japanese Patent Publication No. 63-37154) has also been proposed.

[Problem to be solved by the invention] However, in the production of silicone emulsions based on high molecular weight organopolysiloxanes, the method of emulsifying low molecular weight siloxanes and then polymerizing them involves an equilibration reaction. The disadvantage is that siloxane remains, and the method of diluting high molecular weight organopolysiloxane with an aromatic organic solvent and then emulsifying it has problems with solvent odor and flammability. The degree of polymerization is up to 2,200, and the method of adding a low-boiling oil to a high molecular weight organopolysiloxane does not indicate a composition or method for obtaining a highly stable emulsion. A compound consisting of polysiloxane, cyclic siloxane, surfactant, and water has the disadvantage that it cannot provide a stable 0/W type emulsion that is compatible with lower alcohols.

[Means for Solving the Problems] The present invention relates to a protective film-forming silicone emulsion composition that solves the above-mentioned disadvantages. substitution or replacement 1
a valent hydrocarbon group, R2 is a hydrogen atom or a group selected from a methyl group, an ethyl group, a vinyl group, a phenyl group, a hydroxyl group,
Organopolysiloxane composition 100 consisting of 1 to 50 parts by weight of an organopolysiloxane represented by (m is an integer of 2,300 to 20,000), b) 99 to 50 parts by weight of a low-boiling oil capable of dissolving component a) parts by weight, B) 1 to 30 parts by weight of a surfactant consisting of polyoxyethylene alkyl ether carboxylic acid or its salt, C) polyhydric alcohol 1
~100 parts by weight, D) Total amount of A), B), and C) 1
It is characterized by emulsifying and dispersing at least 10 parts by weight of water per 00 parts by weight.

That is, as a result of various studies in order to develop an emulsion composition of high molecular weight organopolysiloxane that has good alcohol resistance and forms a stable O/W type emulsion, the inventors of the present invention have developed a composition represented by the above general formula (1). A high molecular weight organopolysiloxane that exhibits soft rubber-like properties at room temperature is mixed with a low boiling point oil, and this is mixed with an anionic surfactant as component B, a polyhydric alcohol as component C), and a polyhydric alcohol as component D.
) It was discovered that when emulsified and dispersed using an emulsifying and dispersing device in the presence of water as a component, a stable ○/W type silicone emulsion was obtained. When the seafood is evaporated, a protective film made of rubber-like organopolysiloxane is formed on the surface of the base material, and this protective film provides the base material with properties such as mold releasability, polishing properties, luster, flexibility, lubricity, and repulsion. After confirming that it imparts elasticity, water repellency, etc., the present invention was completed by conducting research on the types and amounts of each component used.

This will be explained in further detail below.

[Function] The present invention relates to a protective film-forming silicone emulsion composition containing a high molecular weight organopolysiloxane as a main material.

Component A) constituting the composition of the present invention consists of the following components a) and b).

The orcappolysiloxane as component a) is represented by a general formula, where R1 is an alkyl group such as a methyl group, an ethyl group, a propyl group, a butyl group, a cycloalkyl group such as a cyclohexyl group, or an alkenyl group such as a vinyl group or an allyl group. 3.3.3 aryl groups such as phenyl groups, tolyl groups, or chloromethyl groups in which some or all of the hydrogen atoms bonded to the carbon atoms of these groups are substituted with halogen atoms, cyano groups, etc. - at least 90% selected from trifluoropropyl groups, cyanoethyl groups, etc.
is the same or different unsubstituted or substituted monovalent hydrocarbon as a methyl group, R2 is a hydrogen atom or a group selected from a methyl group, an ethyl group, a vinyl group, a phenyl group, a hydroxyl group, m is 2,300 to With an integer of 20,000, it is said to exhibit soft rubber-like properties at room temperature, and this includes dimethylpolysiloxane whose molecule end is blocked with a trimethylsilyl group, and dimethylpolysiloxane whose molecule end is blocked with a hydroxyl group. Siloxane, a copolymer of dimethylsiloxane and diphenylsiloxane whose molecular end is capped with a trimethylsilyl group, a copolymer of dimethylsiloxane and methylvinylsiloxane whose molecular end is capped with a hydroxyl group,
Examples include a copolymer of dimethylsiloxane and methyl-3,3,3-trifluoropropylsiloxane containing a vinyl group at the terminal end of the molecule.

In addition, component b) is a low boiling point oil that can dissolve the organopolysiloxane as component a), which includes low molecular weight chain or cyclic siloxane,
Examples include isoparaffinic hydrocarbons having 1 to 30 carbon atoms.

This low molecular weight chain siloxane is represented by the general formula, where R3 is a hydrogen atom or the same monovalent hydrocarbon as R1 above, and R4 is the same hydrogen atom as R2 above, or a methyl group, ethyl group, or vinyl group. , phenyl group, and hydroxyl group, where n is an integer of 0 to 7, including hexamethyldisiloxane, octamethyltrisiloxane, decamethyltetrasiloxane, hexadecamethylheptasiloxane. , hexaethyldisiloxane, tetramethyldiethyldisiloxane, detramethyldivinyldisiloxane, and the like.

In addition, this cyclic siloxane is represented by the general formula, R5 is a hydrogen atom or the same monovalent hydrocarbon as R1, and k is an integer of 3 to 8 on average,
These include hexamethylcyclotrisiloxane, octamethylcyclotetrasiloxane, decamethylcyclopentasiloxane, 1,1-diethylhexamethylcyclotetrasiloxane, phenylhebutamethylcyclotetrasiloxane, 1.1 diphenylhexamethylcyclo Tetrasiloxane, 1,2,3.4-tetravinyl-1,2,3
, 4-tetramethylcyclotetrasiloxane, 1,2,
Examples include 3.4-tetramethylcyclotetrasiloxane and dodecamethylcyclohexasiloxane.

Note that this isoparaffinic hydrocarbon has a boiling point of 60 to 80°C at normal pressure and has a carbon atom number of 1.
~30 is required, but this requires Aitzba-A1 Isopar C1 Isopar D1 Isopar E1 Isopar G1 Isopar H1 Isopar to 1 Isopar-L1 Isopar M [all trade names manufactured by Exxon Corporation in the United States], Isosol 200, Isosol 300, Isosol 400, Isosol 500 [all are Nippon Petrochemical's split product names], Shellsol 71 [product name manufactured by Shell, Inc., USA], Tsurutol 100 [product name manufactured by Phillips, Inc., USA], Mineral Spirit [Showa Sekiyu Co., Ltd.] Chemistry■Cracked product name].

These low boiling point oils may be any one or two of these.
After applying the composition of the present invention to a substrate, these low boiling point oils are volatilized together with water to form a protective film of high molecular weight organopolysiloxane on the surface of the substrate. At least 16mmHg as required
It is required that the boiling point at reduced pressure is 200°C or less, and the blending amount is 99 parts by weight per 1 to 50 parts by weight of the organopolysiloxane as component a).
If it exceeds 50 parts by weight, the content of the high molecular weight organopolysiloxane becomes too low and the performance when used as a protective film cannot be exhibited, and if it is less than 50 parts by weight, the viscosity of the composition as component A) becomes too high. Since this makes emulsification and dispersion difficult, it is necessary to set the amount in the range of 99 to 50 parts by weight.

In addition, the surfactant as component B) constituting the composition of the present invention is considered to be an essential component for emulsifying and dispersing the organopolysiloxane composition as component A), but the dough is The anionic surfactant is selected from oxyethylene alkyl ether carboxylic acids or salts thereof. This includes polyoxyethylene (4)
Sodium octyl ether acetate, polyoxyethylene (4) sodium lauryl ether acetate, polyoxyethylene (4) sodium tridecyl ether acetate, polyoxyethylene (4) sodium cetyl ether acetate, polyoxyethylene (4) sodium stearyl ether acetate , polyoxyethylene (8) sodium tridecyl ether acetate, polyoxyethylene (8) sodium stearyl ether acetate, polyoxyethylene (4)
Octyl ether potassium acetate, polyoxyethylene (
4) Tridecyl ether calcium acetate, polyoxyethylene (4) tridecyl ether ammonium acetate, polyoxyethylene (4) cetyl ether ammonium acetate, polyoxyethylene (2) octyl ether acetate,
Polyoxyethylene (4) lauryl ether acetic acid, polyoxyethylene (4) tridecyl ether acetic acid, polyoxyethylene (8) stearyl ether acetic acid, polyoxyethylene (8) cystyl ether acetic acid (in examples)
2), (4), and (8) (the numerical values indicate the number of moles of polyoxyethylene groups), but these have a HLB of 8 or higher in terms of their emulsifying performance and the stability of the resulting emulsion. - It would be better if it belonged to Hi.

However, regarding this surfactant, alkyl sulfates such as sodium lauryl sulfate, triethanolamine lauryl sulfate, ammonium lauryl sulfate, polyoxyethylene (4) sodium lauryl ether sulfate, polyoxyethylene (13) Sodium cetyl ether sulfate, polyoxyethylene (6) sodium stearyl ether sulfate, polyoxyethylene (4) ammonium lauryl ether sulfate, polyoxyethylene (
6) Polyoxyethylene alkyl ether sulfates such as stearyl ether sulfate triethanolamine, polyoxyethylene alkylphenyl such as polyoxyethylene (6) sodium nonylphenyl ether sulfate, polyoxyethylene (9) octylphenyl ether sulfate triethanolamine, etc. Organopolysiloxane composition 1 as component A) containing an anionic surfactant selected from ether sulfate or alkyl sulfocarboxylic acid salts such as sodium lauryl sulfocarboxylate.
If necessary, polyoxyethylene such as polyoxyethylene (9) nonylphenyl ether or polyoxyethylene (9) octylphenyl ether may be used in combination with 00 parts by weight. Alkyl phenyl ether, polyoxyethylene alkyl ether such as polyoxyethylene (13) cetyl ether, polyoxyethylene (12) stearyl ether, polyoxyethylene such as polyoxyethylene (14) monostearate, polyoxyethylene (20) monomaleate, etc. Ethylene alkyl ester, polyoxyethylene (20)
Sorbitan monostearate, polyoxyethylene (2
0) A nonionic surfactant selected from polyoxyethylene sorbitan fatty acid esters such as turbitan sesquioleate, etc. as described above. Its properties as a surfactant cannot be fully exhibited, and if the amount exceeds 30 parts by weight, it is too much and the properties of the organopolysiloxane composition are impaired, so it may be used in combination in the range of 1 to 30 parts by weight.

Next, the polyhydric alcohol as component C) constituting the composition of the present invention acts as a causer factant when the organopolysiloxane composition as component 8) is emulsified and dispersed with the surfactant as component B). It is added to maintain the stability of the emulsion produced, and these include glycerin, diglycerin, polyglycerin, pentaerythritol, ethylene glycol, polyethylene glycol, ethylene-propylene copolymer, trimethylene glycol , triethylene glycol, 1,2-butylene glycol,
1.3-butylene glycol, 1.4-butylene glycol, tetramethylene glycol, 2.3-butylene glycol, pentamethylene glycol, hexylene glycol, trimethylolpropane, 1.2.6-hexaglycerin, xylitol, sorbitol , mannitol, diethylene glycol, dipropylene glycol, tetraethylene glycol, triglycerin, tetraglycerin, ethylene glycol monooleyl ether, hexaglycerin, octaglycerin, decaglycerin, decaglycerin monolaurate, decaglycerin dioleate, etc. . If the blending amount of the polyhydric alcohol as component C) is less than 1 part by weight based on 100 parts by weight of the organopolysiloxane composition as component A), the action as a causer factant will be insufficient; Even if the amount is more than 1 part by weight, there is no change in the performance as a causer factant, and if it is added more than this, it will be economically disadvantageous and furthermore, there is a risk that the protective film forming ability of component A) will be impaired, so 1 to 100 parts by weight. The preferred range is 5 to 5.
The amount is 60 parts by weight.

In addition, whether water as component D) constituting the composition of the present invention is required to make the composition of the present invention into an O/W type emulsion, and its blending amount is determined in the above-mentioned A).
, B), 10 per 100 parts by weight of the total amount of components
If the amount is less than 10 parts by weight, it is difficult to form the composition into an O/W type emulsion, and the composition becomes soluble in W2O type, so it is necessary to use at least 10 parts by weight.

The composition of the present invention includes the above-mentioned A), B), C), and D.
) can be obtained by homogeneously mixing predetermined amounts of A) organopolysiloxane as a) component and A) b) a low boiling point oil as component. Mix uniformly and dissolve in component b) a.
Component A) is prepared, and a predetermined amount of the organopolysiloxane as the A) component, a surfactant as the B) component, and a polyhydric alcohol as the C) component are blended, and the mixture is stirred and mixed to form a uniform mixture. By adding a predetermined amount of water as component D) little by little, the phase of this composition is inverted from W2O type to O/W type and emulsified. According to this, the desired O/W type can be obtained. An emulsion can be easily obtained by blending the above-mentioned components A) and B), stirring and mixing them uniformly, and then adding a mixture of component C) dissolved in component D) to this mixture. Similarly, phase inversion and emulsification may be carried out, and when performing phase inversion and emulsification from W2O type to O/W type, an emulsifying and dispersing device selected from a colloid mill, homomixer, homogenizer, Combimix, or sand grinder may be used. , more uniform and finer particle size O/
A W-type emulsion composition can be obtained.

In addition, when preparing the composition of the present invention, part of the water as component b) may be replaced with a lower alcohol, which includes methanol, ethanol, isopropanol, n-
Examples include alcohols having 1 to 8 carbon atoms, such as butanol, inbutanol, n-pentanol, and hexanol, but ethanol is preferred from the viewpoint of volatility, safety, and odor. When the composition of the present invention to which this lower alcohol is added is used, for example, as a mold release agent or a hair cosmetic, it has the effect of improving wettability and controlling volatility.

Generally speaking, such lower alcohols act as emulsion-destroying agents, but the composition of the present invention has excellent compatibility and resistance to these lower alcohols, so the emulsion will not be destroyed, and this lower alcohol will not destroy the emulsion. The amount of alcohol to be added is 25% or less, preferably 2% or less, since if the amount exceeds 25% of the total amount of the emulsion composition of the present invention, the stability of the emulsion may be impaired.
It should be less than 0%.

The emulsion composition of the present invention is applied to a substrate and dried at room temperature, or optionally heated at 60 to 200°C for several seconds to several hours to volatilize the low boiling point seafood. A protective film mainly composed of
This product can be used as a mold release agent, polishing agent, fiber treatment agent, and cosmetic agent.

When using this emulsion composition as a mold release agent, mica, talc,
Inorganic fillers such as zinc oxide and calcium carbonate, stabilizers such as carboxymethyl cellulose, polyvinyl alcohol, and sodium polyacrylate, as well as silanes containing epoxy groups, silanes containing mercapto groups, silanes containing acrylic groups, and carboxyl groups. Silanes such as silanes containing vinyl groups, silanes containing vinyl groups, organoxime silanes,
Pigments, preservatives, bactericides, etc. may be added. When using this as a mold release agent, dilute it with water and spray it uniformly with an air blower or brush on the surface to be released. The resins to be released from the mold include phenyl resins, epoxy resins, thermosetting resins such as polyester resins, thermoplastic resins such as polyvinyl chloride, polyethylene, and polypropylene, natural rubber, isoprene, chlorobrene, and styrene. - Rubbers such as butadiene rubber are exemplified.

In addition, when using this emulsion composition as a fiber treatment agent, it is diluted with water so that the amount of adhesion to the fiber material is 0.0 as a high molecular weight organopolysiloxane component.
Is it okay to adjust the coating to a range of 5 to 5.0% by weight, preferably 0.1 to 1.0% by weight? In this case, if necessary, add glyoxal resin, melamine resin,
Add resin processing agents such as urea resin, polyester resin or acrylic resin, organopitrodiene polysiloxane, epoxy group-containing organopolysiloxane, amino group-containing organopolysiloxane emulsion, surfactants, preservatives, colorants, etc. This is optional, and examples of this fiber material include natural fibers such as wool, silk, cotton, and linen, recycled fibers such as rayon and bemberb, polyester, polyacrylonitrile, vinylon, polyvinyl chloride, nylon, and tetron. Examples include inorganic fibers such as synthetic fibers, glass fibers, and carbon fibers.

In addition, when using this emulsion composition as a hair cosmetic, the paste may be mixed with water, lower alcohol, or a water-lower alcohol mixture in an appropriate ratio, but when using this as a setting lotion, These mixtures may be used as a hairspray as they are, or in the case of forming a foam hair styling product, these mixtures may be used as an aerosol prepared by mixing an appropriate liquefied gas with a propellant.

[Example] Next, examples and application examples of the present invention will be given. Parts in the examples are parts by weight, viscosity is a value measured at 25°C, and storage stability of the obtained emulsion is shown. , centrifugation test, and average particle size measurement are shown below.

[Storage Stability] 100 g of a sample was collected in a glass bottle, left in a constant temperature bath at 40° C. for one week, and the appearance was observed, and the stability was evaluated using the following criteria.

○...The oil component is not separated and is stable, △～○...The oil component is slightly separated or is in a very stable state, △...A part of the lower layer is Separated, ×: Half or more of the lower layer is separated, or creaming is observed in the upper layer.

[After weighing the centrifuged Testco sample into a 20zP glass container,
The mixture was centrifuged at 00 rpm for 15 minutes, and in order to examine phase separation, 2 g of the upper and lower samples were weighed into an aluminum dish, heated at 105°C for 3 hours, and the nonvolatile content was measured.
Stability was evaluated based on the ratio, and the closer this ratio was to 1.0, the more stable the product was.

[Measurement of average particle size] Measure the particle size of the sample using a light scattering particle size measuring device / Nanosizer N4
(trade name, manufactured by Coulter, Inc., USA).

Examples 1 to 4 Dimethylpolysiloxane crude rubber 10 with a degree of polymerization of 3,500, in which the terminal end of the molecule is blocked with a trimethylsilyl group
1 part was dissolved in 90 parts of octamethylcyclotetrasiloxane to prepare oil A having a viscosity of 1.630 cS.

Next, to 100 parts of this oil-A, a boxoxyethylene ether carboxylate surfactant and a polyhydric alcohol of the type and amount shown in Table 1 were added, and the mixture was well stirred and mixed. The amount of phase inversion water shown in Table 1 was added to emulsify and disperse, and the amount of dilution water shown in Table 1 was added to make emulsions A-D, and the storage stability and average particle size of these emulsions were evaluated. When a centrifugation test was performed along with the measurement, the results shown in Table 1 were obtained.

Table Examples 5 to 7. Comparative Examples 1 to 3 Anionic surfactants, nonionic surfactants, and polyhydric alcohols of the types and amounts shown in Table 2 were added to 100 parts of oil-A prepared in Example 1, and the mixture was thoroughly stirred. After that, the amount of phase inversion water shown in Table 2 was added to this while stirring to emulsify and disperse, and then the amount of water/water shown in Table 2 was added.
Diluted with ethanol mixture, then 316 kg/cm”
Emulsions E to G were homogenized through a Galarin homogenizer at a pressure of .

Also, for comparison, oil made in Example 1-A 1
00 parts of surfactant of the type and amount shown in Table 2 (for Comparative Example 2, glycerin was also added) and emulsified and dispersed in the same manner as above to prepare emulsions H to J.

Next, we measured the storage stability and particle size of emulsions E to J obtained in this way, and also conducted a centrifugation test on dough, and the results shown in Table 2 were obtained. It was done.

Table Examples 8 to 11 Dimethylpolysiloxane crude rubber 12 with a degree of polymerization of 3,000, which is blocked at the molecular terminal with a trimethylsilyl group
Part of isoparaffinic organic solvent / Isosol 400 [
Oil-B having a viscosity of 1.270 cS was prepared by dissolving and mixing 88 parts of Nippon Petrochemical Co., Ltd. [Cracked product name].

Next, to 100 parts of this oil-B, surfactants and polyhydric alcohols of the types and amounts shown in Table 3 were added, and emulsified and dispersed in the same manner as in Examples 1 to 4 to form an emulsion.
The storage stability and particle size of this emulsion composition were measured, and a centrifugation test was conducted, and the results shown in Table 3 were obtained.

Fruit surface Examples 12-14. Comparative Examples 4 to 6 Anionic surfactants, nonionic surfactants, and polyhydric alcohols of the types and amounts shown in Table 4 were added to 8100 parts of the oil prepared in Example 8, and the mixture was thoroughly stirred. After mixing, add phase inversion water in the amount shown in Table 4 while stirring to emulsify and disperse, and then add water/water in the amount shown in Table 4.
Diluted with ethanol mixture, then 316 kg/cm2
Emulsion O-Q was made by homogenizing through a Galarin homogenizer at a pressure of .

In addition, for comparison, 8100 parts of this oil was added with the type and amount of surfactant shown in Table 4 (in Comparative Example 4, glycerin was also added), and emulsified and dispersed in the same manner as in Examples 12 to 14. I made emulsions R to T.

Next, the storage stability and particle size of the emulsion composition 0-T thus obtained were measured, and a centrifugation test was performed on the emulsion composition 0-T, and the results shown in Table 4 were obtained.

Table Application Example 1 Emulsion A obtained in Examples 1, 2, 8.10 above
, B, M is the concentration of high molecular weight silicone rubber or 0,
A fiber treatment agent was prepared by diluting it with water to a concentration of 5%, and a mixture of 65% by weight of polyester and 35% by weight of cotton (T
/C) After soaking the broadcloth, squeeze it with a squeezing roller,
Pre-drying at a temperature of 110'C followed by 3 at 150 t
Heat treated for minutes.

For comparison, a 20% emulsion of dimethylpolysiloxane with a viscosity of 1,000 cS and whose molecule end is blocked with a trimethylsilyl group was prepared with a silicone concentration of 1.
The same polyester-pure mixed broad as above was treated in the same manner as above using a commercially available emulsion solution which was adjusted to have a treatment solution of 0%.

Finally, the smoothness, repellency, flexibility, and water repellency of the silicone-treated broad obtained in this manner were examined by touch, and the water repellency was examined using the AATCC spray test method. The results shown in the table were obtained.

Table 5 Application Example 2 40.0 parts of the emulsion A obtained in Example 1 was mixed with 0.1 part of carboxydimethylcellulose Selgen F [Daiichi Kogyo Seiyaku Aji-cleavage product name] and 20 parts of water, and mixed with a stirrer. Then, 40.0 parts of 300 mesh mica was added and stirred for 2 hours to make a tire Oze molding agent, which was then sprayed into an unvulcanized butyl rubber tire liner (
A butyl rubber plate (15 x 15 x 0.5 cm) was sprayed onto a rubber plate (5 x 5 x 0.5 cm) and then vulcanized.
5cm), place the release agent coated surface on top of the surface and heat at 50℃.
10 at a pressure of 20 kg/cm2 by a press molding machine.
After the unvulcanized butyl rubber was vulcanized by applying pressure for a minute, it was taken out and its releasability was examined, and it was found to have good releasability.

Application Example 3 When the emulsion E obtained in Example 5 was filled into a sprayer and sprayed onto the hair in a dew-like manner, it was found that this product had good sprayability and gave the hair excellent gloss and smooth feel. However, the hair treated in this manner also had good set retention properties.

[Effects of the Invention] The present invention relates to a silicone emulsion composition capable of forming a protective film of a high molecular weight silicone rubber on an object to be treated. b) Emulsification of A) organopolysiloxane composition dissolved and mixed in low boiling point oil, B) blush active agent consisting of polyoxyethylene alkyl ether carboxylic acid or its salt, C) polyhydric alcohol, and D) water. The gist of this is a silicone emulsion composition obtained by dispersing a silicone emulsion composition in which the high molecular weight organopolysiloxane raw rubber as component 8) is easily emulsified by adding component B), component C), and component D). However, when this silicone emulsion is applied to a substrate and the low boiling point seafood is volatilized, a protective film made of rubber-like organopolysiloxane is formed on the surface of the substrate. This emulsion composition has industrial properties such as being useful as a mold release agent, fiber treatment agent, polishing agent, and cosmetic agent because it imparts mold release properties, polishing properties, luster, water repellency, etc. An advantage is given.

Patent applicant: Shin-Etsu Chemical Co., Ltd.

Claims (1)

[Claims] 1. A) a) General formula▲ Numerical formula, chemical formula, table, etc.▼ (Here, R^1 is the same or different unsubstituted or substituted monovalent hydrocarbon group, R^2 is 1 to 50 parts by weight of an organopolysiloxane represented by a hydrogen atom or a group selected from a methyl group, an ethyl group, a vinyl group, a phenyl group, and a hydroxyl group, m being an integer of 2,300 to 20,000, b) a) 100 parts by weight of an organopolysiloxane composition consisting of 99 to 50 parts by weight of a low-boiling oil capable of dissolving the components; B) 1 to 30 parts by weight of a surfactant consisting of polyoxyethylene alkyl ether carboxylic acid or a salt thereof; C) ) 1 to 100 parts by weight of polyhydric alcohol; D) A protective film-forming silicone obtained by emulsifying and dispersing at least 10 parts by weight of water per 100 parts by weight of the total amount of A), B), and C). Emulsion composition. 2. Component D) consists of at least 20 parts by weight of water based on 100 parts by weight of the total amount of components A), B), and C), and 25% or less of lower alcohol based on the total weight of the composition. The protective film-forming silicone emulsion composition according to claim 1.