JP3410618B2 - Silicone aqueous emulsion composition - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

FIELD OF THE INVENTION The present invention relates to an aqueous silicone emulsion composition, particularly a rubber film which is easily cured without generating hydrogen gas, has excellent strength and flexibility, and has good adhesion to various substrates. The present invention relates to a silicone aqueous emulsion composition which is useful as a coating agent or the like.

[0002]

2. Description of the Related Art As a silicone aqueous emulsion composition which cures to form a rubber film, those having various compositions have hitherto been known. For example, a silicone emulsion composition comprising an anionically stabilized hydroxylated diorganopolysiloxane, colloidal silica and an organic tin compound or an organic amine compound and having a pH in the range of 9 to 11.5 (JP-A-56-16553) However, this composition has problems in that it has poor adhesion to various substrates and is subjected to various restrictions in use due to strong alkalinity.

[0003] Therefore, in order to improve the adhesiveness of this kind of composition, for example, a cyclic organosiloxane and a functional group-containing organotrialkoxysilane such as aminoalkyltrialkoxysilane are mixed with a sulfonic acid or a sulfonic acid type. An organopolysiloxane latex composition obtained by emulsion polymerization in the presence of a quaternary ammonium salt-based surfactant (see JP-A-54-131661), a siloxane block copolymer comprising dimethylsiloxane units and monophenylsiloxane units, Silicone latex composition comprising water, cationic surfactant, nonionic surfactant, filler and aminofunctional silane (see US Pat. No. 3,817,894), hydroxyl group-containing organopolysiloxane emulsion, aminofunctional silane When The reaction product of an anhydride, a silicone aqueous emulsion composition comprising colloidal silica and a curing catalyst (see JP-A-58-101153) have been proposed.

[0004]

However, although all of them have some effect of improving the adhesiveness,
It is not always sufficient for use in severe conditions such as insufficient seam strength and partial application of large force including weak film strength, for example, sealing seams of concrete, or increasing the strength of sewing parts of fibers. At present it is not enough. Therefore, this silicone aqueous emulsion composition has excellent strength and flexibility,
In addition, there is a demand for providing a rubber film having good adhesion to various substrates.

[0005]

SUMMARY OF THE INVENTION The present invention is directed to a silicone aqueous emulsion composition which solves such disadvantages, problems and problems, and comprises (A) an organopolysiloxane containing at least two or more alkenyl groups. Siloxane 100 parts by weight (B) Organohydrogenpolysiloxane containing at least two or more Si-H bonds 0.05 to 20 parts by weight (C) Colloidal silica and / or polysilsesquioxane 1 to 100 parts by weight (D) Reaction product of aminofunctional organosilane and acid anhydride 0.5 to 20 parts by weight (E) Addition reaction catalyst 0.0001 to 1 part by weight (F) Epoxy group-containing organosilane and / or partial hydrolyzate thereof 0 to 20 parts by weight As a main component.

The present invention relates to an aqueous silicone emulsion composition comprising (A) an organopolysiloxane containing at least two or more alkenyl groups, and (B) at least two or more Si-H as described above. An organohydrogenpolysiloxane containing a bond,
(C) colloidal silica and / or polysilsesquioxane, (D) a reaction product of an aminofunctional organosilane and an acid anhydride, (E) an addition reaction catalyst,
(F) It consists of a predetermined amount of an epoxy group-containing organosilane and / or a partial hydrolyzate thereof, which is easily cured by removing water to form a uniform rubber film without foaming, It was confirmed that this film had physical properties such as excellent strength and flexibility and good adhesion to various substrates. Hereinafter, each component used in the present invention will be described in detail.

First, the organopolysiloxane containing at least two or more alkenyl groups, which is the component (A), has the general formula

Embedded image [Wherein, R represents the same or different alkyl group having 1 to 20 carbon atoms or aryl group having 6 to 20 carbon atoms, X represents the same or different alkyl group having 1 to 20 carbon atoms, aryl having 6 to 20 carbon atoms. A group, an alkoxy group having 1 to 20 carbon atoms, a hydroxyl group or an alkenyl group having 1 to 20 carbon atoms, Y is the same or different group represented by X or (OSiX ₂ ) _C X, a is a positive number of 0 to 1,000, b
Is a positive number of 100 to 10,000, and c is a positive number of 1 to 1,000], and is an organopolysiloxane containing at least two or more alkenyl groups in one molecule. Here, R is the same or different and is an alkyl group having 1 to 20 carbon atoms or an aryl group having 6 to 20 carbon atoms, specifically, a methyl group, an ethyl group, a propyl group, a butyl group, a pentyl group, a hexyl group. , Heptyl, octyl, decyl, tetradecyl, octadecyl, phenyl, tolyl, naphthyl and the like, with methyl being preferred. X represents the same or different alkyl group having 1 to 20 carbon atoms,
To 20 alkoxy groups, hydroxyl groups or alkenyl groups having 1 to 20 carbon atoms, specifically, a hydroxyl group, methyl group, ethyl group, propyl group, butyl group, hexyl group, heptyl group, octyl group, decyl group, Tetradecyl, octadecyl, phenyl, tolyl, naphthyl, methoxy, ethoxy, propoxy, butoxy, hexyloxy, heptyloxy, octyloxy, decyloxy, tetradecyloxy, octadecyloxy , Vinyl group, allyl group and the like. Y is the same or different group represented by X or (OSiX ₂ ) _C X;
Is larger than 1,000, the resulting rubber film has insufficient flexibility, so it is a positive number of 0 to 1,000, preferably a positive number of 0 to 100. When it is larger than 10,000, the tear strength is reduced. Therefore, it is a positive number of 100 to 10,000, preferably a positive number of 1,000 to 5,000, and c is a positive number of 1 to 1,000.

The organopolysiloxane as the component (A) contains at least two alkenyl groups in one molecule from the viewpoint of crosslinking with the Si—H bond of the organohydrogenpolysiloxane as the component (B). And this content is in the range of 1 × 10 ^-6 to 1 × 10 ^-4 mol / g. Such an organopolysiloxane has the following general formula:

Embedded image

Embedded image Can be mentioned.

[0009] Such an organopolysiloxane can be synthesized by a known method. For example, this is accomplished by adding a cyclic siloxane such as octamethylcyclotetrasiloxane and 2,4,6,8-tetramethyl- as a vinyl raw material in the presence of a catalyst such as an alkali metal hydroxide.
Vinyl group-containing siloxane oligomers such as 2,4,6,8-tetravinylcyclotetrasiloxane, 1,1,3,3-tetramethyl-1,3-divinyldisiloxane, hexavinyldisiloxane, trimethoxyvinylsilane, dimethoxy Vinyl group-containing silanes such as methylvinylsilane, and other raw materials such as hexamethyldisiloxane, α, ω-dihydroxysiloxane oligomer, dimethoxydimethylsilane, diethoxydimethylsilane,
It is obtained by equilibrating a compound selected from trimethoxymethylsilane, triethoxymethylsilane, triethoxyphenylsilane and the like.

Since the organopolysiloxane of the component (A) is preferably used in the form of an emulsion, it may be formed into an emulsion by a known emulsion polymerization method.
As necessary, after emulsifying and dispersing a vinyl group-containing siloxane oligomer or vinyl group-containing silane as a vinyl raw material and a siloxane oligomer or an alkoxysilane as another raw material in water using an anionic surfactant or a cationic surfactant. It can be easily synthesized by adding a catalyst such as an acid or an alkaline substance to carry out a polymerization reaction.

Next, the organohydrogenpolysiloxane containing at least two Si—H bonds in the molecule as the component (B) serves as the above-mentioned component (A) crosslinking agent.

Embedded image Wherein R is the same as above, Q is R or a hydrogen atom, d is a positive number of 1 to 1,000, e is a positive number of 1 to 1,000, provided that e = 0
In the above case, Q is a hydrogen atom, and when e = 1, at least one of Q is a hydrogen atom.] Is usually used. From the viewpoint of crosslinkability, it is preferable that when the organosiloxane (A) has two alkenyl groups, it contains at least three Si-H bonds in one molecule. The siloxane skeleton may contain a branch unit.

Specific examples of such an organohydrogenpolysiloxane include the following:

Embedded image Are also exemplified, but these are also similar to the organopolysiloxane of the above-mentioned component (A).
It can be synthesized by an equilibrium reaction or emulsion polymerization of an H bond-containing cyclic siloxane and hexamethyldisiloxane or 1,1,3,3-tetramethyldisiloxane. Further, it can be synthesized by a conventionally known method by a cohydrolytic condensation reaction of methyldichlorosilane, trimethylchlorosilane, dimethylchlorosilane and the like.

In the present invention, it is preferable that the organohydrogenpolysiloxane is used as the component (B) in the form of an emulsion. However, the amount of the component (B) is preferably 100 parts by weight of the component (A). If the amount is less than 0.05 parts by weight, the crosslinkability becomes insufficient and the strength of the silicone rubber film decreases, and the effect of improving the adhesiveness and flame retardancy is lost. If the amount exceeds 20 parts by weight, the film becomes too hard and flexible. Is required to be 0.05 to 20 parts by weight, but a preferable range is 0.1 to 10 parts by weight.
Si-H bond in component (B) and Si-V in component (A)
When the preferred blending amount of both components (A) and (B) is represented by the molar ratio of the i bond, Si-H / Si-Vi = 0.01 to 1.0.

[0014] Colloidal silica and / or polysilsesquioxane as the component (C) is added as a film reinforcing agent. Specifically, colloidal silica and trimethoxymethylsilane are hydrolyzed and condensed. Such as polymethylsilsesquioxane. Polymethylsilsesquioxane is prepared by adding an acid such as sulfuric acid or an alkali compound such as potassium hydroxide as a condensation catalyst to a surfactant aqueous solution, and then dropping and stirring trimethoxymethylsilane. An emulsion containing sun is obtained. At this time, in order to adjust the degree of crosslinking of the polysilsesquioxane, it is possible to add an alkoxytrialkylsilane, a dialkoxydialkylsilane, a tetraalkoxysilane, or the like. Further, in order to increase the reactivity of polysilsesquioxane, vinyl silane, epoxy silane, acrylic silane, methacryl silane, or the like may be added. The amount of the component (C) is 100%.
If the amount is less than 1 part by weight, there is no effect of improving the strength and flame retardancy of the silicone rubber film. If the amount exceeds 100 parts by weight, the film becomes hard and brittle, and elongation and flexibility are reduced. , 1 to 100 parts by weight, but a preferred range is 5 to 50 parts by weight. The average particle size of the component (C) is preferably from 5 to 200 nm.

Next, the reaction product of the aminofunctional organosilane (D) and the acid anhydride is a component for improving the adhesion between the silicone rubber film and the base material. And a dicarboxylic anhydride. The raw material amino group-containing alkoxysilane is represented by the general formula AR _g Si (OR) _3-g [wherein,
R is the same as above, A is the formula -R ¹ (NHR ¹ ) _h NHR ² (wherein, R ¹ is the same or different divalent hydrocarbon group having 1 to 6 carbon atoms, R ² is R
Or a hydrogen atom, h is an integer of 0 to 6), and g is an amino-containing group represented by 0, 1 or 2], and specific examples thereof include the following. (C ₂ H ₅ O) ₃ SiC ₃ H ₆ NH ₂ , (C ₂ H ₅ O) ₂ (CH ₃ ) SiC ₃ H ₆ NH ₂ , (CH ₃ O) ₃ SiC ₃ H ₆ NHC ₂ H ₄ NH ₂ , (CH ₃ O) ₂ (CH ₃ ) SiC ₃ H ₆ NHC ₂ H ₄ NH ₂ Examples of the dicarboxylic anhydride for reacting with the amino group-containing alkoxysilane include, for example, phthalic anhydride,
Examples include succinic anhydride, methylsuccinic anhydride, maleic anhydride, glutaric anhydride, itaconic anhydride and the like.

The ratio of the aminofunctional organosilane to the acid anhydride is preferably such that one molecule contains one or more amide groups or aminocarboxylates from the viewpoint of adhesion to the substrate. It is preferable to react at least one molecule of dicarboxylic anhydride with one NH group. These reactions are carried out at room temperature in a solvent such as alcohol.
It is sufficient to stir at a temperature of 100 ° C. for 1 to 30 hours, to form an amide bond in the reaction between the amino group and the carboxylic acid anhydride, and to react the amino group with the carboxylic acid in which the carboxylic acid anhydride is opened by the moisture in the alcohol. During this time, salt formation occurs. When each raw material is used without reaction, the stability of the composition becomes extremely unstable, and the addition reaction does not proceed, so it is necessary to use a product obtained by reacting each raw material. Become.
The amount of the component (D) is based on 100 parts by weight of the component (A).
If it is less than 0.5 part by weight, there is no effect of improving the adhesion to the base material, and if it exceeds 20 parts by weight, the flexibility is reduced,
It is required to be 0.5 to 20 parts by weight, but a preferable range is 1 to 10 parts by weight.

The addition reaction catalyst as the component (E) is
An organopolysiloxane containing an alkenyl group as the component (A) and an organohydrogenpolysiloxane containing a Si—H bond as the component (B) are added to cause an addition reaction, and include a platinum compound, a rhodium compound, and the like. It is preferred to use Platinum compounds are well known to those skilled in the art as catalysts for addition reactions, and include chloroplatinic acid, alcohol-modified chloroplatinic acid, chloroplatinic acid-vinylsiloxane complex and the like. Among these platinum compounds, a complex of a vinylsiloxane and a platinum compound, which is further preferably alcohol-modified, is particularly preferable, and in particular, chloroplatinic acid described in JP-B-33-9969 or vinylsiloxane and chloroplatinic acid is used. Are preferred. Examples of the rhodium compound include RhCl (Ph ₃ P) ₃ described in JP-A-4-352793.
And the like. In addition, these catalysts are diluted with an organopolysiloxane containing an alkenyl group in advance,
It is desirable to use a surfactant to form an emulsion emulsified and dispersed in water. If the amount of the component (E) is less than 0.0001 part by weight per 100 parts by weight of the component (A), no catalytic effect of the addition reaction will be obtained, and if it exceeds 1 part by weight, there will be no advantage and it will be uneconomical. The amount may be 1 part by weight, but a preferable range is 0.005 to 0.1 part by weight.

Further, the epoxy group-containing organosilane and / or the partial hydrolyzate thereof as the component (F) are as follows:
It is a component for improving the adhesion between the silicone rubber film and the substrate, and specific examples include the following. γ
-Glycidoxypropyltrimethoxysilane, γ-glycidoxypropyldimethoxymethylsilane, β- (3,
4-epoxycyclohexyl) ethyltrimethoxysilane, β- (3,4-epoxycyclohexyl) ethyldimethoxymethylsilane. The amount of the component (F) is (A)
If the amount is more than 20 parts by weight with respect to 100 parts by weight of the component, the flexibility is lowered. Therefore, the amount may be 0 to 20 parts by weight, but the preferable range is 0 to 10 parts by weight.

The aqueous silicone emulsion composition of the present invention is prepared by mixing the above-mentioned components (A) to (F) and forming them into an emulsion. Is often used,
The surfactant used here is not particularly limited, and examples thereof include anionic surfactants such as alkyl sulfate, alkylbenzene sulfonate, and alkyl phosphate, polyoxyethylene alkyl ether, polyoxyethylene alkyl phenyl ether, and polyoxyethylene alkyl phenyl ether. Examples thereof include nonionic surfactants such as oxyethylene fatty acid esters, cationic surfactants such as quaternary ammonium salts and alkylamine acetates, and amphoteric surfactants such as alkyl betaines and alkyl imidazolines. The composition of the present invention may contain, if necessary, an addition reaction controlling agent, a water-based paint, or a component added to the fiber treating agent, such as a thickener, an antifoaming agent, a pigment, an inorganic powder, a penetrating agent, and an antistatic agent. , Preservatives and the like may be appropriately compounded.

The silicone aqueous emulsion composition of the present invention thus produced is put to practical use by applying it to various substrates to be treated. The treatment method is not particularly limited. The coating may be performed by a known method such as brush coating, roll coating, spray coating, knife coating, dip coating, etc., and the base material thus treated is then heated and dried to form a silicone rubber film. The silicone aqueous emulsion composition can be widely applied as a paint, a fiber treatment agent, a release agent, a back surface treatment agent such as an adhesive sheet, or a binder of an inorganic or organic substance.

[0021]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS The embodiments of the present invention will be described below with reference to Examples and Comparative Examples. The methods for evaluating the physical properties of coatings and the adhesion to various substrates in these Examples and Comparative Examples, and fiber treatment The method for evaluating the properties (flexibility, tear strength of the sewn portion, combustibility) as the agent is described above. [Evaluation of film physical properties and adhesion to various substrates] The following composition was poured into a fluoroplastic casting plate, and at room temperature for 48 hours.
After standing for 1 hour, cure at 105 ° C for 1 hour, thickness about 1mm
A cured film of was prepared. The appearance of this film was observed and evaluated as follows. 〇: A uniform film without any foaming. Δ: Some foaming was observed, but it was possible to measure the film properties. X: The foaming was so severe that the physical properties of the film could not be measured. Further, the elongation and the tensile strength were measured according to JIS K-6301. Similarly, a cured film having a thickness of about 1 mm was similarly prepared using a casting plate composed of various substrates as shown in Table 1, and one end of the film was formed in a direction perpendicular to the substrate by approximately 300 mm.
/ Min, and the state of the film and the substrate at this time was observed and evaluated as follows. 〇: The adhesiveness was extremely excellent, and the film was broken without peeling off at the interface between the film and the substrate. Δ: Peeled off at the interface, but required considerable force. C: Peeled off at the interface, and almost no force was required.

[Evaluation of properties as a fiber treatment agent] To the composition prepared below, carboxymethylcellulose (Cerogen F, manufactured by Daiichi Kogyo Seiyaku Co., Ltd.) was further added as a thickener under stirring to obtain a treatment composition having a viscosity of 18,000 cP. After preparing the product, fineness
Using 420 denier 66 nylon long fiber yarn, each warp yarn 46
After the above-mentioned treatment composition was knife-coated on a woven fabric plain-woven at a book / inch density so as to have a coating amount of about 45 g / m ² ,
Heat curing was performed at 180 ° C. for 2 minutes to prepare a treated cloth for testing. The following properties were evaluated for the treated cloth. <Flexibility> Using a Uenoyama type texture meter,
(Cm width) was measured. (The smaller the value, the softer) <Tear strength of sewing part>
1 mm was sewn with a polyester thread at 5 mm from the end of the test piece shown in FIG. 1 (a), and each end on the opposite side was oriented in the direction shown in FIG. 1 (b). Pull,
The strength at which the treated cloth at the sewn portion was torn was measured. <Flammability> Evaluated by FMVSS-302 method. Burning speed of 101.2mm / min or less passed.

[0023]

【Example】

Examples 1 to 5 [Preparation of Raw Material Components] Preparation of Component (A) [1] 385.4 g of octamethylcyclotetrasiloxane, 2,4
After uniformly mixing 13.4 g of 6,8-tetramethyl-2,4,6,8-tetravinylcyclotetrasiloxane, 1.2 g of triethoxyphenylsilane, and 100 g of a 10% aqueous solution of dodecylbenzenesulfonic acid with a homomixer, 500 g was gradually added and emulsified and dispersed in water, and then subjected to secondary emulsification with a high-pressure homogenizer to obtain a stable emulsion.
This emulsion is polymerized at 50 ° C for 24 hours, aged at 25 ° C for 24 hours, and neutralized with 10% aqueous sodium carbonate solution to obtain the following composition.

Embedded image "Emulsion A1" containing 36.9% by weight of an organopolysiloxane was obtained.

Preparation of component (A) [2] Octamethylcyclotetrasiloxane 353.2 g, 2,4
After uniformly mixing 45.6 g of 6,8-tetramethyl-2,4,6,8-tetravinylcyclotetrasiloxane, 1.2 g of triethoxyphenylsilane, and 100 g of a 10% aqueous solution of dodecylbenzenesulfonic acid with a homomixer, 500 g was gradually added and emulsified and dispersed in water, and then subjected to secondary emulsification with a high-pressure homogenizer to obtain a stable emulsion.
This emulsion is polymerized at 50 ° C for 24 hours, aged at 25 ° C for 24 hours, and neutralized with 10% aqueous sodium carbonate solution to obtain the following composition.

Embedded image "Emulsion A2" containing 36.7% by weight of an organopolysiloxane was obtained.

Preparation of component (B) [1] below

Embedded image 300 g of an organopolysiloxane represented by the following formula and 50 of polyoxyethylene nonyl phenyl ether (10 mole adduct of EO)
g was uniformly mixed with a homomixer, 650 g of water was gradually added and emulsified and dispersed in water, and then mixed with a high-pressure homogenizer.
Subsequent emulsification was performed to obtain "Emulsion B1" containing 34.1% by weight of a stable solid component. Preparation of component (B) [2]

Embedded image 300 g of an organopolysiloxane represented by the following formula and 50 of polyoxyethylene nonyl phenyl ether (10 mole adduct of EO)
g was uniformly mixed with a homomixer, 650 g of water was gradually added and emulsified and dispersed in water, and then mixed with a high-pressure homogenizer.
Subsequent emulsification was performed to obtain "Emulsion B2" containing 34.3% by weight of a stable solid component.

Preparation of Component (C) 3 g of a 10% aqueous solution of dodecylbenzenesulfonic acid was dissolved in 770 g of water, 200 g of trimethoxymethylsilane was added dropwise at room temperature, and the mixture was further aged at 60 ° C. for 3 hours to give 10% sodium carbonate. The mixture was neutralized with an aqueous solution to obtain "emulsion C" which is a blue-white translucent polymethylsilsesquioxane emulsion. This emulsion had a nonvolatile content of 9.9% after drying at 105 ° C. for 3 hours. (D) Preparation of Component After dissolving 154 g of maleic anhydride in 500 g of ethanol,
346 g of 3-aminopropyltriethoxysilane at room temperature,
It was added dropwise in one hour. After the completion of the dropwise addition, the mixture was further reacted at 80 ° C. under reflux of ethanol for 24 hours to give a pale yellow transparent “solution D”.
Got. This solution had a nonvolatile content of 45.1% after drying at 105 ° C. for 3 hours, and the reaction products in the solution were IR, GC,
Approximately 60% when analyzed by NMR, GCMS, etc.
Is a mixture of those represented by the following formula, and the remaining about 40%
Were oligomers derived from them. _{(C 2 H 5 O) 3} SiC 3 H 6 -NHCO-CH = CHCOOH, (C 2 H 5 O) 3 SiC 3 H 6 N + H 3 · - OCOCH = CHCOOC 2 H 5

Preparation of Component (E) A mixture of 1 g of a complex of vinyl siloxane and chloroplatinic acid and 99 g of vinyl siloxane was uniformly mixed with 25 g of polyoxyethylene nonylphenyl ether (10 mol adduct of EO) using a homomixer. 375 g was gradually added and emulsified and dispersed in water, and then subjected to secondary emulsification with a high-pressure homogenizer to obtain a stable "emulsion E".

[Preparation of composition] First, colloidal silica (Snowtex C manufactured by Nissan Chemical Co., Ltd .: 20% active ingredient) or "emulsion C" was added as a component (C) with stirring at the compounding amount shown in Table 1 under stirring. After adding “solution D” as the component (D) and adding γ-glycidoxypropyltrimethoxysilane as the component (F), stirring was further continued for 30 minutes to obtain a uniform dispersion. Then, the obtained dispersion liquid is gradually added to “Emulsion A” as the component (A) under stirring, and then “Emulsion B” as the component (B) and “Emulsion E” as the component (E). Was added to prepare a composition. Next, the physical properties (appearance, elongation, tensile strength) of the silicone rubber film obtained from the aqueous silicone emulsion composition thus produced were examined, and when the silicone rubber film was applied to concrete, mortar, glass, copper plate, or wood. Was measured and the flexibility, tear strength, and flammability of the fabric when processed into fibers were measured. The results shown in Table 1 below were obtained.

[0029]

[Table 1]

Comparative Examples 1-4 [Preparation of condensation catalyst component] 300 g of dioctyltin dilaurate
And polyoxyethylene nonyl phenyl ether (EO10
Mol adduct) after homogeneously mixing 50g with a homomixer,
650 g of water was gradually added, emulsified and dispersed in water, and subjected to secondary emulsification with a high-pressure homogenizer to obtain a stable "emulsion G". [Preparation of Composition] First, “solution D” as a component (D) was added to colloidal silica (Snowtex C manufactured by Nissan Chemical Co., Ltd .: active ingredient 20%) as a component (C) with stirring at a blending amount shown in Table 2. ) And 3-glycidoxypropyltrimethoxysilane as the component (F), and then
Stirring was continued for 30 minutes to obtain a uniform dispersion. Then, the obtained dispersion is gradually added to “Emulsion A” as the component (A) under stirring, and then “Emulsion B” as the component (B) and “Emulsion E” as a catalyst component. Alternatively, "Emulsion G" was added to prepare a composition. Next, the physical properties of the coating, the adhesive properties, and the physical properties of the treated cloth were examined for these compositions in the same manner as in the examples. The results shown in Table 2 below were obtained.

[0031]

[Table 2]

[0032]

Industrial Applicability The present invention relates to an aqueous silicone emulsion composition, which is easily cured by removing water and forms a uniform rubber film without foaming. This film has strength and flexibility. It has the advantage of being excellent and having good adhesion to various substrates.

[Brief description of the drawings]

FIG. 1 (a) is a perspective view of a test piece for measuring the tear strength of a sewn portion of a woven fabric having a sewn portion coated with the aqueous silicone emulsion of the present invention, and (b) is a view of the test piece. It is explanatory drawing which shows a pulling direction.

────────────────────────────────────────────────── ─── Continuation of the front page (51) Int.Cl. ⁷ Identification code FI C09D 183/07 C09D 183/08 183/08 C08K 5/54 (72) Inventor Yoshinobu Takahashi 1-chome, Matsuida-cho, Usui-gun, Gunma Prefecture No. 10 Shin-Etsu Chemical Co., Ltd. Silicone Electronic Materials Research Laboratory (72) Inventor Satoshi Kuwata 1-10, Hitomi, Matsuida-cho, Usui-gun, Gunma Prefecture Shin-Etsu Chemical Co., Ltd. Silicone Electronic Materials Research Laboratory (56) References JP-A-5-202338 (JP, A) JP-A-58-101153 (JP, A) JP-A-5-59284 (JP, A) (58) Fields investigated (Int. Cl. ⁷ , DB name) C08L 83/04-83/07 C08K 3/36 C08K 5/54

Claims (1)

(57) [Claims] (A) 100 parts by weight of an organopolysiloxane containing at least two or more alkenyl groups (B) 0.05 to 20 parts by weight of an organohydrogenpolysiloxane containing at least two or more Si—H bonds ( C) 1 to 100 parts by weight of colloidal silica and / or polysilsesquioxane (D) 0.5 to 20 parts by weight of a reaction product of an aminofunctional organosilane and an acid anhydride (E) 0.0001 to 1 part by weight of an addition reaction catalyst ( F) An aqueous silicone emulsion composition comprising, as a main component, 0 to 20 parts by weight of an epoxy group-containing organosilane and / or a partial hydrolyzate thereof.