JPS601259A - Aqueous resin emulsion - Google Patents

Abstract

(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.

Description

DETAILED DESCRIPTION OF THE INVENTION This invention relates to aqueous emulsions of organopolysiloxane resins which are preferred and useful in agricultural applications over conventional solvent systems.

The present invention describes both an aqueous silicone emulsion and a method for making the composition.

Silicone resins are often selected for applications requiring superior properties. These organopolysiloxane resins are known to exhibit remarkable durability against weather and environmental conditions such as extreme heat and cold. Silicone resins are useful in many applications such as pressure sensitive adhesives and release coatings. Furthermore, they have been found to be particularly useful in the coatings industry, where coating formulations are produced which exhibit consistently excellent properties.

Silicone resin solutions have been used in the paint coating industry as vehicles and binders, an essential part of quality paint formulations.

Hitherto, silicone resins have typically been supplied to formulators in the form of solutions, ie, resins containing a high proportion (by weight) of silicone solids in an organic solvent such as xylene or toluene. However, the use of such organic solvents has recently been curtailed due to increasing concerns about the cost and environmental aspects of organic materials. (Solvent-based silicone resins are expensive and require troublesome contamination prevention measures and equipment [7].)As such, there has recently been a trend toward silicone resin systems that are water-based and therefore do not rely on organic solvents. Be looked at.

However, these silicone resins, which are particularly useful in coatings and other coatings, are often immiscible or incompatible with aqueous coating systems. The present invention first provides a silicone resin that can be readily dispersed in aqueous emulsion compositions to impart the advantageous properties of silicone resins without the need for stirring or large amounts of organic solvents.

As mentioned above, silicone resins are used in high temperature resistant coating agents and are commonly used in similar applications as high performance coating vehicles that outperform traditional silicone resins. Those skilled in the art will appreciate that there are many silicone resins available for '$r* applications.

U.S. Patent Nos. 4,028,339 and 4.056.4
The silicone resins shown in No. 92 (Merrll) are examples of resins that can be part of the aqueous emulsion compositions of the present invention.

Although previously known silica-based emulsions have been commonly used for coating glass fabrics, this acidic acid requires the use of an ionic emulsifier such as alkylphenoxyethanol. This system generally requires about 1 part emulsifier for every 7 parts resin solids. This weight emulsion technique can be applied to the fat coatings (“C”) discussed here as required by formulation formulators.
When tried in formulations for
At high temperatures, the film is severely affected. Silicone resins based on a combination of nonionic and anionic emulsifiers are also known, and these can be compared with acid thickeners based on N-high molecular weight carboxyvinyl polymers' (DumO
u]. In U.S. Pat. No. 4,052,55
1, No. 6, line 58). Compositions containing a small amount of polyvinyl alcohol of fairly high saponification value have also been disclosed. This composition can be applied, for example, to a person's skin.
Buddha can be added to freeze, but acid thickeners are not allowed to freeze. The use of unmarked kraft paper as a coating is also indicated.

On the other hand, the present invention utilizes an emulsion system based on a combination of nonionic and/or anionic emulsifiers and certain neutral vinyl addition polymer compositions. Total required 11 ft of emulsifier for the emulsion of the present invention:
ul generally about 05-5 based on silicone resin solid weight
There is a range of 0.0%. Furthermore, when a neutral vinyl compound is used as a cooperative reagent, 1
The aqueous composition can be coated more uniformly than the emulsions using nonionic emulsifiers, which tend to cause "fish eyes".

Accordingly, a first object of the present invention is to provide organopolysiloxanes 4f1. useful in coating formulations. The objective is to obtain an aqueous emulsion of fat.

Another object is to obtain an emulsifier system consisting of a mixture of nonionic and/or anionic and neutral polymeric emulsifiers effective for dispersing silicone resins in aqueous coatings.

It is another object to provide a method for producing aqueous silicone resin emulsions.

These and other objects will be apparent to those skilled in the art upon consideration of the following description and claims.

Summary of the Invention The aqueous silicone emulsion of the present invention has the following general formula:
, S 10 o,s about 0 50 percent, trifunctional units of the formula Re I O ts 0 to 100
double-lobed par-shaped needles, and a tetrafunctional unit of general formula 810, 0
100 parts by weight of at least one organopolysiloxane resin consisting of ~60 weight percent.

In the above formula, R represents a directly substituted or unsubstituted side-legged hydrogen group, usually independently selected from the group consisting of methyl and phenyl. The organoborisiloxane resin has 1.0 to 1.99 R groups per silicon atom. In the present invention,
In addition to using one type of resin in each emulsion, blends of different organoborisiloxane resins may be used.

Book B [Organopolysiloxanes useful in emulsions of
Approximately 5 to 40 small. R. %C) T3S I
O 15 units, 0-55% by weight (a1■3),
s s o Jl- position, 15-65 weight- (Ose
s) B I O ts year unit unit n-1 [1 ¥K (fN-related (c6u5), consisting of sto units, and there are about 1.0 to 1.8 plugged groups per silicon atom) Chiru.

These Olga and Novolisiloxane oils are emulsified in water by the method described in the present invention. 2'1. In the field of silicone resins, a certain weight percent of silicone (1%
It is usually supplied in a solution consisting of an eye oil serum. For example, silicone resins may be mixed with organic solvents such as toluene or xylene, which, if present, are not a critical component of the present invention and are generally unsuitable for the useful properties of these aqueous silicone emulsions. There is nothing that can lower it. In fact, the presence of a small amount of organic solvent in an emulsion often imparts some other beneficial properties to the emulsion.

Aqueous emulsions of the silicone resins mentioned above may be obtained by utilizing mixtures of emulsifiers.

The amount of emulsifier required to emulsify the resin homogeneous 100-fold gold emulsion varies widely depending on the process conditions and the selection of components in the emulsion. Those skilled in the art will be able to prepare a variety of aqueous silicone resin emulsions according to the method presented herein and still be able to reduce the amount of emulsifier according to the method presented here, and further adjust the amount of emulsifier according to individual requirements. The amount of emulsifier can be adjusted.

Although not intended to limit the scope of the present invention, it should be noted that approximately 0.0
25 to 50 parts by weight of emulsifier mixture may be required.
This is 1 letter. It has been discovered by the present invention that certain combinations of emulsifiers are effective in dispersing these silicone resins to provide aqueous emulsions. Emulsifier Mixture Emulsifier consisting of a vinyl polymer having pendant hydroxyl groups or pendant neutralized carboxyl groups or a mixture of these groups. Anionic surfactant or emulsifier 95~
Consisting of 5% by weight. For example 70-757Jj
'M percent of beer-containing polymeric emulsifier and 25%
It is known that ~30 parts by weight of nonionic and/or anionic surfactants can produce satisfactory emulsions according to the present invention. Specific examples of each of these types of emulsifiers are given below. An effective amount of such an emulsifier mixture is mixed with an organopolysiloxane resin in the presence of water. Aqueous silicone resin emulsions are obtained by use of well-known emulsification techniques such as colloid milling. The amount of water is not limited and usually depends on the use of the resulting emulsion. Add water and mix to bring the resulting emulsion to a preselected silicone resin solids content.

The method of the present invention provides the aqueous silicone resin emulsion composition described above by mixing certain components and then using well-known emulsification techniques.

DESCRIPTION OF THE INVENTION The silicone resins used in the compositions of the present invention are organohalosilanes whose composition can be varied by a number of well-known methods, for example by varying the proportion of the organohalosilane component that is hydrolyzed. Fake 1JI'J is amazing compared to the hydrolysis of the mixture. Assuming a typical resin, then,
In the presence of water, acetone and a water-immiscible organic solvent,
about 6 n mole percent methyltrichlorosilane, about 3
5 mole percent phenyltrichlorosilane and ca.
Starting from a mole percent dimethyldichlorosilane mixture. Generally, the hydrolysis solution can contain about 1.7 to 10 parts of water, 0.2 to 5 parts of acetone, and 0.3 to 5 parts of a water-immiscible organic solvent per part by weight of the silane mixture. .

The various components of the hydrolysis mixture may be added separately in the desired order. Generally, the organohalosilane is added to a mixture of water, acetone, and an organic solvent. Preferably, when this method is used, 2 to 6 parts of water, about 3 to 2 parts of acetone, and about 0.0 parts of organic solvent are used per part of the total weight of the organohalosilane mixture. It is used in a proportion of 6 to about 2 parts. Adding the organohalosilane to the hydrolyzed Pr'F medium is preferable to suppressing the hydrochloric acid formation during the hydrolysis reaction than vice versa. Strong hydrochloric acid solutions are not preferred in this example. This is because salts ["'"', 1: 7] cause the acid concentration of the setone to form polymerization products that impart an undesirable color to the product and have an adverse effect on the physical properties of the product. It's for a reason.

The preferred method for preparing the organoborisiloxane 1.4 fat used in this invention is a dual feed method, which consists of an organohalosilane mixture and a ca.
It consists of feeding another 7 parts, preferably 0.9 to 1.2 parts, of acetone from the vessel through separate tubes and then premixing them just before hydrolysis. The presence of water causes hydrolysis of Or7j Tubaronran,
Polymerize acetone 11. ``, 0 is generated, so when it comes into contact with the acetate or organohalosilane, filter 5.>'
Since water may be present in the air even at sunset, it is necessary to limit the contact time. The initial hydrolysis medium before introduction of the silane blend-acetone mixture is about 0 to 41
parts of acetone, preferably 0.9 to 1.2 parts of acetone. The amounts of water and organic solvent are as indicated above, preferably about 3 to 55 parts of water and 0.9 to 1.2 parts of organic solvent per part of total organohalosilane blend weight. 2.

Temperature of the hydrolysis mixture (-1, addition series jVj of trials 4 and 5
; or by heating or, if desired, cooling.

Temperatures between about 0°C and about 40°C are preferred during hydrolysis. After all of the reagents have been added, 1 the mixture is generally agitated for an additional period of time, such as 15 to 30 minutes or more, to effect complete decomposition of the organohalosilane. The mixture is then allowed to stand and the aqueous (low) acid layer is allowed to drain from the organic layer. The organic layer is then freed from the solvent to reach a solids content of up to 100%, depending on each individual's wishes. Organic solvents are removed under reduced pressure or atmospheric pressure. At this point, the desired viscosity is achieved by condensing and crosslinking the silanol units with the aid of M11, such as iron octoate or celite or mixtures thereof, under complete reflux. 15-12 cpn at 25℃ for Sushikake 20% solids by weight
The resin thickens, ie, its zero molecular weight increases, until . In addition, resin impurities can be treated by analogy (Fushichi Light 545 [ke (0), Jeans Man Building (Johnr 3 Man Building)
It can be removed by filtration using filter aids such as Vfile'), Fuller's earth (calcium montmorillonite), and mixtures thereof, or simply by centrifugation. Obtained silanol-containing Olga 1. /The polysiloxane resin has a ratio of atom groups to silicon groups of approximately 1.05 to 1.
It is.

Water-immiscible solvents used in the above method for obtaining silicone resins include benzene, l-luene, xylene, etc. There are esters such as butyl acetate and ethyl acetate, and ethers such as diethyl ether.Toluene is the most suitable solvent as it is a good solvent and has a low boiling point.
(+l) Generally, an organic solvent that is inert to the hydrolyzed reactants during hydrolysis, can dissolve the hydrolysis products, can be separated from the aqueous layer, and is immiscible with water. Any one can be used.

Of course, it is possible to disperse these water-immiscible resins in an aqueous medium by the method presented by the present invention.

One of the necessary emulsifiers for the aqueous silicone resin emulsions of the present invention is a vinyl addition polymerization product, such as polyvinyl alcohol and/or carboxyvinyl polymer.

This fpO fluid formulation (e.g. Monzant Plastics & Resins Co., St. Louis, Missouri, USZ)
Trade name of GKLVATOL
and Carbobol (trade name) of B. F. Gutdridge Chemical Co., Creepland, Ohio, tJ8A.
CARBOPOL) can be used respectively. Polyvinyl alcohol is one type of commercially available product. It is produced by hydrolyzing polyvinyl esters, usually acetic esters, with acids or bases. The degree of hydrolysis depends on various conditions. 1 Fully hydrolyzed 'polyvinyl alcohol usually has about 5% residual pendant acetate groups. In the present invention, the extent of residual pendant acetate groups varies over a fairly wide range, such as from about 5% to about 80%, preferably from about 5% to about 60%, with a pendant hydroxyl content of about 20% to about 95%, preferably It means that it varies in the range of about 40 to about 95%.

Carboxy-substituted vinyl addition polymers are also commercially available varieties. This polymer is typically a white powder with a slight acetic acid odor (17) and when dispersed in water (e.g. hydroxylated).
When mixed with IJum or other 53 groups described below, the viscosity becomes 1f1M. Three materials are suitable for the purposes of this invention: Carbobol 934, 940 and 941. When these are neutralized and made into a 0.2% solution,
Viscosity changes depending on the molecular weight. When the Brookfield test apparatus is operated at 25° C. and 20 rpm according to well-known methods, ? 34 is generally 2.050 ~
5,450cp range, 940 is 15,000-55
．． 00 mouth CP range, 941 is 1.950-7. OO
Ocp 17) Range FIIt. Carbo Ball 941
It appears that the class of substances known as are particularly suitable for the purposes of the present invention. Acidic components are neutralized before use by reaction with bases such as alkali metal or alkaline earth hydroxides, carbonates, bicarbonates or monoamines (primary, secondary, tertiary) or ammonia. Ru.

Other types of necessary emulsifiers used in conjunction with the above polymerized vinyl products include sodium lauryl sulfate, sodium linear alkylbenzene sulfonate, triethanolamine linear alkylbenzene sulfonate, sodium alpha olefin sulfonate, alkylphenol ethoxy Anionic emulsifiers such as ammonium laurate sulfate, ammonium lauryl ether sulfate, ammonium alkyl ether sulfate, dialkyl ester of sodium sulfosuccinate, sodium cumene sulfonate, ammonium xylene sulfonate and ammonium oleate, morpholinium stearate, and dimethyl ammonium linoleate.

Examples of nonionic emulsifiers are well known and include alkylphenoxypoly(ethyleneoxyethanol), trinotylnonylpolyethylene glycol, and generally any n
- Contains alkyl monoethers, which have been commercially available for many years. (See U.S. Pat. No. 4,052,231, supra.) The aqueous silicone resin emulsions of the present invention may be prepared in any of several ways.

Usually, the order of addition of the components is not limited. One suitable method involves dispersing the vinyl addition polymer additive in water by stirring and heat until the solids dissolve. The aqueous phase of the emulsion product optionally comprises:
2. It can also be added in portions. Shudori, silicone resin solids per 100 executive parts, 0
5-10 claw group vinyl polymer polymer and 0.1-50v
The nonionic and/or anionic emulsifier in the hoe part is (
Effective for emulsifying T4 fat in aqueous systems. Those of ordinary skill in the art will be able to vary the proportions of the ingredients to obtain the desired resin emulsion formulation.

Optional ingredients such as K, formalin, etc. can be added to these emulsions depending on the desired end use without appreciably reducing the properties of the aqueous emulsions. Examples of typical silicone resins used in the emulsions and methods of the present invention include General Elec's IJ
It is EIR-141 commercially available from Tsuku Corporation.

The composition to be emulsified is then mixed until homogeneous;
The composition is then emulsified in a colloid mill or homogenized into a single formulation.

A useful colloid mill for producing these aqueous resin emulsions on a laboratory scale is the Manton-Gorlin (M+!).
, nton-aaul, tn 5 colloid mill, type 2A. This mill has a fQi of 40 which can be adjusted from 1 to 40 mills.
mil spacing, at atmospheric pressure or (5 to 40
1” of p[+1gN2: Can operate under G'r pressure.

Of course, any person skilled in the art will appreciate the advantages of the method of the present invention in order to produce these water-based silicone emulsions in an industrial manner. It is possible to enlarge the model.

The viscosity of the resulting emulsion can be determined by changing the amount of water contained in the blend! I can do 71 verses. This is best accomplished by first forming a premix consisting of the vinyl polymer and silicone resin and some water. This premix can be emulsified by mixing a nonionic and/or anionic emulsifier and the remainder water. The following example shows that it is also possible to add the water in three parts.

The organopolysiloxane resins used in the following examples are mainly of the formula 0n3SIO1,5 (T unit) and the formula ((!6
1'15) 81015 (TI units) consists of chisel functional units and difunctional units of formula %).

In the description of each resin, silane (parts by weight) refers to the number of parts by weight of the organohalosilane required for the functional units of the resin. Approximate trade and mole percentages of silanes are given for convenience by those skilled in the art. Approximate numbers are shown. R vs. s
The ratio of 1 to 1 is an expression used by those skilled in the art to indicate the approximate number of radicals bonded to silicon, and is a useful measure of the degree of tri- and di-functionality in silicone resins. It is.

T 149.5 24.2 30 17.7D I29
14.0 20 15. IT' 211.5 54.
4 30 34.23D' 255 27.4 20
54.97R to Sl ratio: 1.40 to 1 1) 129 27.9 40 24.56T' 21
1.5 22.9 2 0 21.24D' 255
41 30 4a89 R vs. S! Ratio: 1.7 to 1 DESCRIPTION OF THE PREFERRED SIZE ELJ All prices are based on weight (January 1).

Example 1 An emulsified silicone resin is made of a viscous compound consisting of approximately 35.1% methyltrichlorosilane, 15.2% dimethyldichlorosilane, and 49.7% phenyltrichlorosilane (by weight). 1. It is a product of hydrolysis of solid resin.

x 7-7 Tarat I! +1 A- 150 g of solid silicone resin in a 2 liter stainless steel beaker,
Anatomy of nonionic surfactants [! 'iQ: 5o alkylphenoxypoly('1,000, 'C jetanol)-trimethylnonylpolyethylene glycol ether] 85%
Mix 5 oz of aqueous solution, 5 oz of water, 100 ml of mineral spirit, 10 ml of xylene and 10 tl) and then run in a colloid mill (4 mil spacing, under atmospheric pressure). The resulting emulsion has a viscosity of 142 D cp
s, the solid content is 24.7%, and the appearance is homogeneous milky white. 40 copies of sample fd,! After centrifugation at 1o00 RPM for 30 minutes, no separation is visible on the top or bottom. When this composition is coated on an aluminum panel, a uniform coating is obtained with no creep, although in the blend of this example only the nonionic component exhibits emulsification and, in some cases, creep.

Implementation P'02 Polynato 2 Fluoroethylene Powder [Modern Industrial Plastics, Inc., Deton, Ohio, US, Lyloupe (n+1ube) N[L b 5 ) 21
2, titanium dioxide pigment 45f and silicone 1f described in Example 1 (J fat powder bed 451 blend t, 2
Ball mill for 4 hours and prepare into a homogeneous powder. This was added to a 5% aqueous dispersion of colloidal magnesium silicate (R, T, Panderbilt, Ves
gum) HV) 100 f, 100 t of a 10% aqueous polyvinyl alcohol solution, 20 g of an 85 g aqueous solution of an active nonionic emulsifier mixture (Example 1) and 0.5 f of iron octoate catalyst are added. The mixture is poll milled for 48 hours. This 1. The pigmented resin-emulsified composition obtained in step 1 was applied to an aluminum panel. ．． Cure for 1 hour at 1°C. A good cured film with no uniform voids can be obtained.

Example 5 Dry and ground silicone resin powder 18 as described in Example 1
7F, titanium dioxide 60f1 nonionic emulsifier (Example 1) 19F, polyvinyl alcohol 10% solution 85v1
Wed 282f, Park o.

Ethylene solvent 372 and N-proboxyglopanol 941 are mixed uniformly. Add the resin water (premixture of polyvinyl alcohol 10% solution 1002 and odorless mineral grit) to 1001F.

Next, 10f of methylphenyl silicone oil and 1 part of iron octoate catalyst are added. The premix is mixed in a stainless steel beaker with an air-driven stirrer until homogeneous. This is then run through a colloid mill set at 4 mil intervals. The resulting paint containing emulsified silicone resin was found to have a solids content of 2a6h and a viscosity of 10540pe. 40ml sample at 3000 rp
After centrifugation at m for 30 minutes, no separation at the bottom of the upper boundary can be seen with the naked eye. 4rl aluminum panel with paint
(q) and cured at 105°C for 1 hour to obtain a uniform coating with few voids.

Example 4 Carboxylated high molecular weight vinyl polymer (B, ?,
Gudrich, Carbobol 941) 2F is dispersed in deionized water 9401 at 50° C. by vigorous stirring. Next, a 6-acetoxy-2,4-dimethyl-m-dioxane anti-dust agent [Gsyanaan' Co., Ltd.,
Clifton, 2s, -S'r)-1USA, GibgardDXN] 2.89 and sodium hydroxide 10%
Add aqueous solution a5f. Then 10q of sodium hydroxide
6 Add aqueous solution 811F. Then 85% active nonionic emulsifier blend 81f and silicone resin solution 1757
Add F.

The silicone resin has a silicone resin solid content of 80% dissolved in VM&P naphtha solvent, mainly methyltrichlorosilane &1%, dimethyldichlorosilane 27.9%,
It consists of a hydrolysis product of 22.9% phenyltrichlorosilane and 41.1% diphenyldichlorosilane.

(Silicone resin - B1 above) Disperse the mixture by stirring at high speed. Next, add an additional 8o1 of the nonionic emulsifier mixture (Example 1) and 100f of water.
Add. The premix is mixed and colloid milled at 5 mil intervals under atmospheric pressure. The resulting milky white emulsion had a viscosity of 1573 cps and a solids content of 51.6.
% and the pH is 5.8). 40me 30110
Centrifuge for 30 minutes at rpm.
Separation below me was observed.

Example 5 Preservative (GIBANDAN, GIBGUARD DXN) 0.52
, carboxylated polymer 1, vinyl addition polymer (Carbobol 941), 3 f of 10% sodium hydroxide aqueous solution and 566.89 g of water were mixed and dispersed for 1 hour in 6 (IIc) to neutralize the carboxy vinyl polymer. Add 600.f of silicone resin solution to 85% solution of active nonionic emulsifier (
Example 1) Mixing with sor.

The silicone resin solution is a toluene solution with a resin solids content of 50 parts and consists primarily of a 10 part methyltrichlorosilane product (Silicone Resin-A1 supra).

After uniformly mixing #, the laminated liquid and the emulsifier, the neutralized carboxyvinyl-combination solution is added.

The premixes were mixed and then passed through a colloid mill for 5 mils under atmospheric pressure. The solids content of the silicone resin emulsion was 56.1%, the pH was 16, and the viscosity was 5 n OOcpe.4o- sample is 3
At nOOrpm! Even after centrifugation for 10 minutes, no separation was observed in the white of the eye. It was found that the emulsion had good storage stability when aged for 1 ton at 50° C. in an open air circulation environment.

Example 6 Add 1 (MlF) of polyvinyl alcohol solution (Example 1) to 600 t of the silicone resin solution of Example 5. Mix the premix, and add 5 r of sodium lauryl sulfate (one ionic surfactant) to water. The pre-4M mixture was mixed for 11 hours and then colloid milled at 6 mil spacing under atmospheric pressure. The emulsion had a viscosity of 1000 cps, a pH of zO, and a solids content of 3.
It turned out to be 1.8 inches. 3 samples of 40+r-
On [! Even after centrifugation at 111 rpm for 30 minutes, no minute δ1t was visible to the naked eye at the top or bottom. It was found that a sample of an emulsified silicone resin containing polyvinyl alcohol had good storage stability when stored at 50° C. for 1 t month.

Example 7 The polyvinyl alcohol solution 1001 of Example 1 is added to the silicone resin 6002 of Example 5, and the mixture is mixed. Next, add a solution of 21 parts of potassium salt of dodecylbenzenesulfonic acid (anionic type) dissolved in 298 parts of water. The mixture is mixed for 1 hour and colloid milled at 6 mil intervals under atmospheric pressure. The emulsion has a viscosity of 4100 cpe, a pH of 6.3, and a solids content of 3t 2 %. 3 samples of 4ntrte [)
When eccentrically separated for 50 minutes at OQ rpm, f□ with the naked eye:
l: No Pif is observed, only a skin phenomenon on the surface due to dryness is observed.

Even if the sample was kept open for 1 ton and 11 months at 50°C, it remained in good condition.

Example 8 Real Ni (3': l 5 silicone resin 600 fi
Add jτ, oleic acid 14.1f and mix the mixture well. Next, a solution consisting of 11.2 grams of carboxyl vinyl polymer (carboxyl 941), 3 grams of an aqueous solution of 28 grams of ammonium hydroxide, and 582.7 grams of water is added.

The premix is stirred for 1 hour and then colloid milled at 6 mil intervals under atmospheric pressure. The resulting delusion has a viscosity of 2900 cpe, a pH of 88 and a solids content of 31.9 cpe. 40m sample at 500 orpm
Even after centrifugation for 30 minutes, no separation is visible to the naked eye. The sample was kept at 50° C. for 1 t month, and Kokichi was found to have good storage stability.

Silicone resins of the type used herein are suitable and can be used in the preparation of a variety of coatings and skin thinners.

Because of environmental limitations, seedlings must either be equipped with expensive solvent recovery systems or be cheaply cut into solvent-based systems that are compatible with the environment. Introducing resin solutions into aqueous systems is effective in meeting the political need to reduce pollution. Emulsifying current silicone resin compositions in aqueous systems has not been very easy on this scale, but can be easily accomplished with the present invention. The vinyl compound as used herein is a form of ``1'' and creeping that occurs with the use of only nonionic surfactant systems.

The blended emulsion can be dried without causing any damage.

In light of the above detailed description, many modifications may occur to those skilled in the art. Such obvious modifications are included within the scope of the claims of this application.

Claims (1)

[Claims] 1. (a) 2R,S to O,s (7J) J,I
'-Sensory unit 0 to 5011 percent, formula 11'l
, 0-60 weight percent difunctional units of l5IO, 0-100 weight percent trifunctional units of formula R8l01.5 heavy bone per old bone percent S 10. At least one organopolysiloxane resin qualitatively consisting of 0 to 60 percent tetrafunctional units of
Alternatively, the organopolysiloxane resin has an R group of about 1.0 to 1.0 to 1.0 to 1.
(b) an emulsifier consisting of a vinyl addition polymer having a pendant hydroxyl group or a pendant neutralized carboxyl group, and a nonionic and anionic interface. An emulsifier mixture comprising 95 to 5 weight percent of activator and 0.25 to 50. An aqueous silicone resin emulsion consisting of 4 parts (per 100 parts of the organopolysiloxane resin) and Cl water.2. 5. The aqueous silicone resin emulsion according to claim 1, wherein the water-based silicone resin emulsion is effective for supplying the organopolysiloxane resin 10.
3. The emulsion of claim 2, wherein the emulsion is about 25 to 400 parts by weight per 0 parts by weight. 4. ~5 parts per 100 parts by weight of organopolysiloxane
The emulsion according to claim 1, further comprising 00 parts by weight of an organic solvent. 5. The emulsion according to claim 4, wherein the organic solvent is selected from toluene, xylene and benzene. 6. The emulsion of claim 1, wherein the -valent hydrocarbon groups are independently selected from the group consisting of methyl and phenyl groups. 7. The organopolysiloxane resin has about 5 to 40 weight percent) -0)73810,5 units, about 0 to 6
5 City percent (apr,), s to unit,
Approximately 15 to 65 reprinted parts O (cs Hs) S
I Ot s units, and about υ to 50 type needle percent (0, Hs), s Io units, having about 1.0 to 1.8 4.1 groups per silicon atom. The emulsion according to claim 1. 8. The vinyl polymer emulsifier is selected from polyvinyl alcohol, neutralized carboxyvinyl polymer a, and mixtures thereof. F. Claim 9.0. Emulsion according to Item 1. 9. Claim 9, wherein the anionic surfactant is selected from the group consisting of linear sodium alkylbenzene sulfonate and ammonium oleate. The emulsion according to paragraph 1. 10, 1.(n) monofunctional units o to 5° of formula R35too5 rule f, 1%, difunctional units 0 to 6° of formula Ft2S 10 percent, formula R8I O1,
0 to 100 trifunctional units of s and 1 percent by weight, and 0 to 60* of tetrafunctional units of the formula s t O,! 100 parts by weight of at least a portion of the organopolysiloxane resin consisting essentially of (b) an emulsifier consisting of a vinyl addition polymer having an R group of about 10 to 1.99 per atom); 0.25 to 500 parts by weight of an emulsifier mixture effective to disperse said organoborisiloxane in an aqueous emulsion, comprising 95 to 5 percent by weight of a nonionic and/or anionic surfactant; (based on 100 parts of organopolysiloxane resin); and (c) mixing water; and
How to build J. 11. The method according to claim 10, wherein the emulsification step is carried out using a colloid mill. 12. Premixing the emulsifier mixture or a portion thereof with a portion of the water, and then mixing the emulsifier with the organopolysiloxane resin and the remaining water. The method described in Section 13. 14. The method according to claim 15, wherein the water content is about 25 to 400 parts by weight per 100 parts of the organopolysiloxane resin. 15. Furthermore, the method according to claim 10 includes the step of adding an organic solvent of 0 to 500 parts by weight per 100 parts of the organopolysiloxane resin. 16. The organic solvent is toluene, xylene. and benzene to j'7''-gewaru! The method described in Section 15 of the claim 1.17. Old rF claims number 1
The method described in item 0. 18, the organoborisiloxane) #1 fat is about 5
~40 weight percent OH3S'015, approximately 0 to 35 weight percent (aH3), s+o units,
(C!r) is about 1'5 to 60 weight percent (C!r)
, Hs)2 and has about 10 to 18 atoms per silicon atom.A11! the method of. 19. The method according to claim 10, wherein the vinyl addition polymer emulsifier is selected from polyvinyl alcohol and polymeric neutralized carboxyvinyl polymers and mixtures thereof. 20. The emulsion according to claim 10, wherein the ionic surfactant is selected from the group consisting of straight-aligned sodium alkylbenzene sulfonate and hyolein ri+2 ammonium. 21. (a) a step of dispersing one or more emulsifiers consisting of a vinyl phosphor polymer having a Tarumi E'F! radical, i and a neutralized carboxyl 4; (b) an organopolysiloxane resin; The previous wage is equal!+1
(c) mixing a non-ionic and/or anionic surfactant in another water; (d) adding a vinyl addition polymer/silicone fat premix to the mixture; Ionic and/or anionic surfactant/water mixture is combined with vinyl adduct/silicone resin 1
11. A method for producing an aqueous silicone resin emulsion comprising the steps of: adding the resin to the mixture and mixing until homogeneous; and (e) emulsifying the organopolysiloxane resin to obtain an aqueous silicone resin emulsion.