KR102072370B1 - Method for preparation of MQ-T silicone resin using polyhedral oligomeric silsesquioxanes(POSS) - Google Patents

Abstract

This invention relates to the silicone type film formation composition used for cosmetics. MQ-T silicone resin of the present invention is obtained through a systemic reaction using a polyhedral oligomeric silsesquioxane (POSS) combined with a silicone MQ resin and a hydrocarbon compound, the advantage of not using a solvent that cannot be used in cosmetics There is this. In addition, the resin obtained in this way has its own stability at high temperatures, oxidation stability by ultraviolet rays, breathability and adhesion, properties that do not appear when applied to cosmetics, compatibility with oils used in cosmetics, adhesion and spreading It has excellent properties of flexibility, durability and durability.

Description

Method for preparation of MQ-T silicone resin using polyhedral oligomeric silsesquioxanes (POSS)}

The present invention synthesizes a polyhedral oligomeric silsesquioxane (compound A) and a silicone MQ resin compound (compound B), each of which is a hydrocarbon compound, is prepared through a body reaction by mixing them with a solvent and a catalyst. Silicon MQ-T resin.

Silicone resins are widely used in cosmetics because of their film-forming, long lasting, and non-sticking properties. These silicone resins are developed in various types such as MQ resins, MTQ resins, T resins and polyacrylates (US Pat. No. 2,814,601, 2,857,356, 8,614,278, 4,972,037 3,973,298), and the disadvantages of these resins are sticky and unfolded. It may not feel good, and when applied to cosmetics may feel dry and foreign matters such as the pulling phenomenon in the skin, there is a lot of difficulties in applying to cosmetics because of poor compatibility with the oil used in cosmetics.

Cosmetics to which the MQ resin is applied have a disadvantage in that drying and pulling occurs, and a method of mixing silicone MQ resin and T resin (or propylsilsesquioxane resin including T resin) is proposed (Korean Patent No. 10). -1158690, Published Patent Publication No. 10-2016-0117362), and also a method for obtaining a MQ-T resin composition by reacting the T-resin in which the hydrocarbon compound is bonded to the silicone MQ resin in a systemic reaction (US Pat. 8,742,051), but in this case, in order to dissolve MQ resins and T resins, which are incompatible with solvents, organic solvents that are limited to cosmetics such as benzene, toluene, and xylene should be used. There are many difficulties in completely removing the solvent.

Therefore, by synthesizing silicone resin and applying it to cosmetics without using organic solvents that are limited in cosmetics, it increases the compatibility with oils used in cosmetics, safety, stability, adhesion, spreadability, flexibility, durability and cosmetics It is required to develop a silicone MQ-T resin which has a property of not being easily adhered to after application.

On the other hand, polyhedral oligomeric silsesquioxanes (Polysedral oligomeric silsesquioxane, POSS) has been developed for the purpose of coatings, adhesives, polymer precursors (U.S. Pat. No. 2005/0010012, 6,972,312, 5,484,867, 6,933,345).

KR 10-1158690 B KR 10-2016-0117362 A

The present invention aims to ensure safety by synthesizing silicone MQ-T resins without the use of organic solvents that are limited to cosmetics, and when applied to cosmetics, stability, compatibility, adhesion, spreadability, flexibility It is another object of the present invention to provide a method for synthesizing a silicone MQ-T resin having a long-lasting property and a non-bleeding property.

As a solution of the present invention, a polyhedral oligomeric silsesquioxane compound (Compound A) in which a hydrocarbon compound is bonded through a hydrolysis and condensation reaction, and a silicone MQ resin compound (Compound B) made through a hydrolysis and condensation reaction are prepared. To solve the above problems by synthesizing MQ-T resin through hydrolysis and condensation reaction in the presence of a catalyst, using a solvent that is not limited to use in cosmetics.

The silicone MQ-T resin compound of the present invention is prepared through the above method and has a chemical formula of (R ¹ _a Si _a O _(1.5) ) _x ((R ⁴ ₃ SiO _0.5 ) _c (SiO ₂ ) _d ) _y ( I) R ¹ is an alkyl group or aryl group having 1 to 8 carbon atoms, and R ⁴ is an alkyl group or aryl group having 1 to 8 carbon atoms; ii) a is 1 to 20 as an integer; iii) the weight of '(R ⁴ ₃ SiO _0.5 ) _c / The weight 'of (SiO ₂ ) _d is 0.5 to 2; And iv) the weight of (R ¹ _a Si _a O _(1.5) ) _x / (the weight of (R ⁴ ₃ SiO _0.5 ) _c (SiO ₂ ) _d ) _y is 6-19).

The moiety designated R ¹ _a Si _a O _(1.5) in the formula of the silicone MQ-T resin compound of the present invention is obtained from R ¹ _a Si _a O _(1.5a-0.5b) R ² _b (where i) R ¹ is an alkyl group or an aryl group having 1 to 8 carbon atoms, and R ² is a hydroxy or alkoxy (methoxy, ethoxy, propoxy, etc.) group; And ii) a is 1-20 as an integer and b is 0-18 as an integer. Where b is less than or equal to a + 2 and a + b must always be 2n as an integer).

Further, in the formula of the silicone resin MQ-T compounds of this invention ^{_{(R 4 3 SiO 0.5) c}} (SiO 2) portions are denoted by _{d ^{(R 4 3 SiO 0. 5}} ) c (SiO (2-0.5e) R ² _e ) obtained from _d (where i) R ⁴ is an alkyl group or aryl group having 1 to 8 carbon atoms, and R ² is a hydroxy or alkoxy (methoxy, ethoxy, propoxy, etc.) group; And ii) e is 0 to 2 as an integer).

The present invention relates to a silicone-based film-forming composition for use in cosmetics, and it is possible to ensure safety for cosmetic use by synthesizing silicone MQ-T resin without using a solvent which cannot be used in cosmetics. In addition, the resin obtained according to the present invention is synthesized through a systemic reaction under catalytic conditions, and thus has high temperature stability, oxidation stability by ultraviolet rays, breathability and adhesiveness, and is not used when applied to cosmetics, which is used in cosmetics. It has excellent compatibility with oils, adhesion, spreadability, flexibility and durability.

The present invention relates to a silicone-based film forming composition used in cosmetics and a method for producing the same. The composition of the present invention is obtained by a systemic reaction using a polyhedral oligomeric silsesquioxane (POSS) in which silicone MQ resin and a hydrocarbon compound are bonded, without using a solvent for which cosmetics are limited, and polyhedral oligomeric silsesquioxane By applying the compound, it is possible to increase the compatibility of the MQ resin and to have high temperature stability in air, adhesion, oxidation stability by ultraviolet rays, and high tensile strength.

Specifically, the present invention synthesizes a polyhedral oligomeric silsesquioxane (POSS) compound and a silicone MQ resin to which a relatively low molecular liquid hydrocarbon compound is bound, and the POSS and MQ resins are mixed with a solvent. Systemic reactions under catalytic conditions can yield MQ-T resin more effectively. According to this method, it is not necessary to use a solvent that cannot be used in cosmetics, and silicone MQ-T resin itself has stability at high temperature, oxidation stability by ultraviolet rays, breathability and adhesiveness, and after application to cosmetics It has properties that are hard to get off, compatibility with oils used in cosmetics, adhesion, spreadability, flexibility, glossiness and durability.

In order to achieve the object of the present invention, a polyhedral oligomeric silsesquioxane (compound A) and a silicone MQ resin compound (compound B) to which a hydrocarbon compound is bound are synthesized, respectively, and by using the systemic reaction, a silicone MQ-T resin is used. To prepare. Specifically, compound A, compound B, and silicone MQ-T resin will be described below.

1.Compound A

A polyhedral oligomeric silsesquioxane compound with a hydrocarbon compound is composed of a combination of T units, a solvent, a catalyst and a neutralizing agent, where T units are RSiO ₃ containing three oxygen atoms in silicon, where R is Reactive substituents, R generally means a monomer in the form of Alkyl group, Phenyl, Hydrogen, Hydroxyl group, Chlorine or Alkoxy group). Compound A has an oligomer form in which 2 to 20 T units are bonded.

2. Compound B

The silicone MQ resin compound consists of a combination of M units, Q units, solvents, catalysts, neutralizers and diluting solvents. Here, M unit is a monomer in the form of R ₃ SiO containing only one oxygen atom in silicon, Q unit is a monomer in the form of SiO ₄ containing four oxygen atoms in the silicon atom (where R is Non-reactive substituents, R is typically an Alkyl group, Phenyl, Hydrogen, Hydroxyl group, Chlorine or Alkoxy group).

3.silicone MQ -T resin

In the final compound of the present invention, the compound A and the compound B consist of a combination of a solvent and a catalyst which can be used in cosmetics.

Hereinafter, a method of synthesizing Compound A and Compound B and a method of preparing silicon MQ-T resin using the same will be described below.

1. Compound A: Hydrocarbon compound Combined  Polyhedral oligomer Silsesquioxane  compound

The polyhedral oligomeric silsesquioxane compounds of the present invention can be broadly classified into two types, and can be divided into a complete compound in cage form as shown in FIG. 1 and a polyhedral oligomeric silsesquioxane compound in incomplete form as shown in FIG.

[Figure 1]

[Figure 2]

Complete compounds in cage form (Figure 1) may have low reactivity but high stability, and incomplete compounds (Figure 2) have low stability and high reactivity, making them suitable as intermediates for the preparation of the compounds of the present invention. .

As an intermediate of the systemic reaction of the present invention, a polyhedral oligomeric silsesquioxane compound (i.e. compound A) having a hydrocarbon compound bonded thereto is composed of a combination of a T unit, a solvent, and a catalyst, wherein the T unit is bound to 2 to 20 units. Has an oligomeric form.

Hydrocarbon compounds Combined  Polyhedral oligomer Silsesquioxane  Chemical formula of compound (compound A): R ^One _a Si _a O _(1.5a-0.5b) (R ² ) _b

In the above formula, R ¹ is an aryl group such as an alkyl group having 1 to 8 carbon atoms or a phenyl group, and R ² is a hydroxy or alkoxy (methoxy, ethoxy, propoxy, etc.) group, preferably hydroxy or ethoxy. to be. In the case of alkoxy having more than 3 carbon atoms, the release of R ² is difficult, and it is difficult to separate when a solvent is added later.

a is 1-20 as an integer, Preferably it is 4-10. b is 0-18 as an integer, Preferably it is 0-8. In addition, b is less than or equal to a + 2, and a + b must always be 2n (n is a natural number) as an integer. If the length of the chain is long, i.e. if a and / or b exceed the above range, the viscosity may increase due to the attraction and may form into a solid phase.

Silicon is relatively easy to exist in the liquid phase because of its intrinsic bond length and flexibility due to its inherent nature compared to hydrocarbons. In particular, the polyhedral oligomer form in which a is an integer of 1 to 20 is spherical or ladder-like, and thus, it is easy to dissolve the M / Q resin of the present invention, but the polymer form other than the oligomer form is gel or It tends to become a solid phase and is not suitable for dissolving the M / Q resin of the present invention.

The polyhedral oligomeric silsesquioxane compound to which a hydrocarbon compound is bonded consists of the following reactions and combinations of i), ii), iii) and iv).

i) R ¹ SiR ³ ₃

ii) solvent

iii) hydrolysis and condensation catalysts

iv) neutralizing agent

Hereinafter, the reactants i), ii), iii) and iv) will be described in detail.

i) R ^One SiR ³ ₃

R ¹ SiR ³ ₃ may be used to form R ¹ _a Si _a O _(1.5a-0.5b) (R ² ) _b , which is Compound A, and R ¹ is an aryl such as an alkyl group having 1 to 8 carbon atoms or a phenyl group. Group. When R ¹ is a substituent such as hydrogen or methyl, steric hindrance does not occur, making it easier to form a full-form polyhedral oligomeric silsesquioxane, while R ¹ has many steric effects such as cyclohexyl, cyclopentyl and aryl groups. In the case of the receiving substituent, the formation of incomplete polyhedral oligomeric silsesquioxane occurs. Therefore, when applied to cosmetics can increase the compatibility with the oil used in cosmetics, relatively three-dimensional obstacles may occur It is preferable that it is a C3 or more alkyl group.

In addition, R ³ may be a hydroxy, halide (fluorine, chlorine, bromine, etc.) or alkoxy (methoxy, ethoxy, propoxy, etc.) group as a hydrolyzable group, but a halide is used. If the salt is generated in the result can cause problems such as skin irritation, it is not preferable for the use of cosmetics. Hydrolysis of R ³ occurs relatively quickly in the hydrolysis condensation reaction. Especially, in the case of halides, it is difficult to control the molecular weight because it is easily formed into a polymer other than an oligomer form due to the property of causing hydrolysis faster than alkoxy. Follow. Therefore, alkoxy is suitable for easy molecular weight control.

ii) solvent

The solvent is at least one selected from the group consisting of aliphatic alcohols having 2 or more carbon atoms, such as ethanol, isopropanol, butanol, water, and hexamethyldisiloxane, without being limited thereto.

As aliphatic alcohols, solvents such as methanol have a problem of rapid hydrolysis and cannot be used as harmful ingredients in cosmetics. Therefore, alcohols having 2 or more carbon atoms are suitable, but if the carbon number is too long, the process of separating the solvent and the catalyst is difficult. It takes a long time or is not easy to volatilize when drying under reduced pressure at high temperature.

The solvent does not have a harmful effect on the skin. The choice of solvent is a very important factor in the formation of polyhedral oligomeric silsesquioxanes, and the hydrogen of water leaves many hydroxyl groups of the silanol groups, which favors the formation of incomplete polyhedral oligomeric silsesquioxanes. In addition, when the content of the polar solvent in the synthesis process is high, it inhibits the formation of silsesquioxane of the polymer, thereby enabling the formation of polyhedral oligomeric silsesquioxane. Therefore, the solvent is more preferably water or ethanol.

At this time, it is more preferable to mix water and other polar solvents other than water, and it is most preferable to mix water and ethanol. In this case, the water and the polar solvent may be added in a mixed form at the same time, but of course also includes the case in the mixed form.

The ratio of water and ethanol is very important in the mixed use, and the weight ratio of water / ethanol is 2 to 5, which is advantageous for the formation of the compound A in oligomeric form. If the weight ratio of water / ethanol exceeds 5 it can be easily gelled due to the high reactivity during hydrolysis, if less than 2 has a disadvantage that the hydrolysis is not easy due to the low polarity.

iii) hydrolysis and Condensation  catalyst

As the hydrolysis and condensation catalyst, a base catalyst or an acid catalyst can be used. As the base catalyst, one or more of the group consisting of potassium hydroxide, sodium hydroxide, ammonia, carbonate, and the like can be used. As the acidic catalyst, trifluoromethylsulphonic acid, acetic acid, methylsulphonic acid, hydro One or more may be used in the group consisting of collic acid, sulfonic acid, sulfuric acid, and the like. In the formation of the polyhedral oligomeric silsesquioxanes of the present invention, the catalyst has a very high effect, the high pH catalyst facilitates the formation in polymer form, and the low pH catalyst forms the polyhedral oligomeric silsesquioxane. To facilitate. Therefore, the acid catalyst is more preferably used in the preparation of Compound A of the present invention.

iv) neutralizing agent

As a neutralizing agent used for the purpose of stopping the reaction, a basic neutralizing agent may be used potassium hydroxide, sodium hydroxide, sodium bicarbonate or a combination thereof, and as an acid neutralizing agent, citric acid, acetic acid, Lactic acid, hydrocholic acid, sulfonic acid, sulfuric acid or a combination thereof may be used, and in the present invention, it is preferable to use a basic neutralizing agent.

Specifically, R ¹ SiR ² ₃ composed of the main component of the polyhedral oligomeric silsesquioxane (Compound A) to which the hydrocarbon compound is bonded is 1 to 50 parts by weight, preferably 5 to 20 parts by weight. The solvent is 30 to 98 parts by weight, preferably 60 to 95 parts by weight.

The catalyst is 0.001 to 10 parts by weight, preferably 0.01 to 5 parts by weight is suitable, the higher the acidity and content of the catalyst may be a phenomenon of polymerizing, the lower the acidity and content may not proceed the reaction.

In addition to the above mentioned properties of R ^1, the properties of R ³ , the solvent and the pH of the catalyst, the temperature and reaction time also have important influences. After the reaction mixture is mixed, the reaction is carried out at 30 to 100 ° C. for 4 to 24 hours, and a reaction stop reagent is added to stop the reaction. 6-8 is suitable for stopping the reaction. In addition, the higher the temperature of the reaction or the longer the reaction time, the greater the possibility of obtaining in the form of a polymer, which is not preferable for the formation of Compound A.

After the reaction is stopped, the solvent and catalyst layer are separated by standing for 24 to 48 hours, dried under reduced pressure and filtered at 80 to 150 ° C. for 1 to 5 hours to remove unreacted products, secondary products and solvents. Through this process, a polyhedral oligomeric silsesquioxane (Compound A) to which the final liquid hydrocarbon compound is bound is obtained.

2. Compound B: Silicone MQ  Resin

Silicon MQ resin, compound B of the present invention, is an intermediate of systemic reaction, two kinds of M units and Q units are used, where M unit contains only one oxygen atom in silicon and Q unit is used in silicon atom. It contains four oxygen atoms.

Any individual M, Q siloxane unit in the silicone MQ resin may contain a hydroxy group or an alkoxy group. Such siloxane units containing hydroxy or alkoxy groups are commonly found in silicone resins. When alkoxy silane precursors in these silicone resins are used, the product is obtained by reacting hydrolyzable groups with water. Alkoxy groups in the alkoxy silane precursors are obtained from complete hydrolysis or from interchange of alcohols with hydrolyzable groups.

Typically, the weight percent of the total hydroxy groups present in the silicone MQ resin is 1 to 3 weight percent based on the total weight of compound B and the weight percent of the alkoxy groups is less than or equal to 10 weight percent, such that polyhedral oligomeric silsesquioxanes Systemic reaction with a hydroxyl group or an alkoxy group is carried out. Silicone MQ resins have an average molecular weight of 1,000 to 10,000.

silicon MQ  Chemical formula of resin (Compound B): ( R ⁴ ₃ SiO _{0 . 5} ) _c (SiO _(2-0.5e) R ² _e ) _d

In said formula, R <^4> is an aryl group like a C1-C8 alkyl group or a phenyl group, Preferably a methyl group is suitable. R ² here is a hydroxy or alkoxy (methoxy, ethoxy, propoxy etc.) group, preferably hydroxy or ethoxy. And the MQ resin has T resin and reaction when R ² is and leaving the condensation reaction, R ² is a leaving '(R ⁴ ₃ SiO _{0.5) c} in weight / (SiO _{2) d} weight of' is 0.5 to 2.0, preferably Is 0.8 ~ 1.5.

The silicone MQ resin compound consists of the following reactions and combinations of i), ii), iii), iv), v) and vi).

i) R ⁴ ₃ SiO _{0 .5}

ii) SiO _(2-0.5e) R ² _e

iii) solvent

iv) hydrolysis and condensation catalysts

v) neutralizer

vi) diluent solvent

Hereinafter, the reactants i), ii), iii), iv), v) and vi) will be described in detail.

i) R ⁴ ₃ SiO _{0 .5}

R ⁴ to form a ₃ SiO _{0 .5,} SiR ₃ R ⁴ can be used to ^5, R ⁴ is an aryl group such as alkyl group or a phenyl group having 1 to 8 carbon atoms, preferably methyl, R ⁵ is artists As the degradable group, halides (fluorine, chlorine, bromine, etc.), alkoxy (methoxy, ethoxy, propoxy, etc.) or R ⁴ ₃ Si- may be used. In the case where the halide is used as R ⁵ here, salts may occur in the resultant, which may cause problems such as skin irritation, which is not preferable for use in cosmetics. R ⁵ is preferably hexamethyldisiloxane.

ii) SiO _(2-0.5e) R ² _e

To construct SiO _(2-0.5e) R ² _e , (R ⁶ O) ₄ Si can be used. Wherein R ⁶ is an alkyl group having 1 to 8 carbon atoms (e.g., tetramethoxysilane, tetraethoxysilane, etc.), or a liquid polyalkyl silicate (e.g., methyl silicate, ethyl silicate, etc.), of which tetraethoxy Preference is given to silanes or ethylpolysilicates.

iii) solvent

The solvent is at least one selected from the group consisting of aliphatic alcohols having 2 or more carbon atoms, such as ethanol, isopropanol, butanol, water, and hexamethyldisiloxane, without being limited thereto.

As aliphatic alcohols, solvents such as methanol are fast to hydrolyze and are not available as harmful components in cosmetics. Therefore, alcohols having 2 or more carbon atoms are suitable. It takes a long time or is not easy to volatilize when drying under reduced pressure at high temperature.

The solvent does not adversely affect the skin, and the solvent is more preferably water or ethanol. At this time, it is more preferable to mix water and other polar solvents other than water, and it is most preferable to mix water and ethanol. In this case, the water and the polar solvent may be added in a mixed form at the same time, but of course also includes the case in the mixed form.

The ratio of water and ethanol is very important when mixed, and the weight ratio of water / ethanol is 0.5 to 2, which is advantageous for the formation of Compound B. If the weight ratio of water / ethanol exceeds 2 it can be easily gelled due to the high reactivity during hydrolysis, if less than 0.5 has a disadvantage that the hydrolysis is not easy due to the low polarity.

Additionally, hexamethylcyclotrisiloxane (D ₃ ), octamethylcyclotetrasiloxane (D ₄ ), decamethylcyclopentasiloxane (D ₅ ), dodecamethylcyclohexasiloxane (D ₆ ) in the form of cyclic siloxanes for flexibility purposes. Or more in the group consisting of.

iv) hydrolysis and Condensation  catalyst

As the hydrolysis and condensation catalyst, a base catalyst or an acid catalyst can be used. As the base catalyst, one or more of the group consisting of potassium hydroxide, sodium hydroxide, ammonia, carbonate, and the like can be used. As the acidic catalyst, trifluoromethylsulphonic acid, acetic acid, methylsulphonic acid, hydro One or more may be used in the group consisting of collic acid, sulfonic acid, sulfuric acid, and the like. In the preparation of Compound B of the present invention, the catalyst is more preferably an acidic catalyst.

v) neutralizer

As the neutralizing agent used for the purpose of stopping the reaction, potassium hydroxide, sodium hydroxide, sodium bicarbonate or a combination thereof can be used as the basic neutralizing agent, and citric acid, acetic acid, lactic acid as acidic neutralizing agent. , Hydrocolic acid, sulfonic acid, sulfuric acid or a combination thereof may be used, and it is preferable to use a basic neutralizing agent.

vi) diluent solvent

In the case of the dilution solvent, any inert solvent which does not significantly affect the hydrolysis and condensation reaction can be used without particular limitation. For example, solvents containing groups having hydrolytic and condensation reactivity such as hydroxy groups, alkoxy groups, etc., limit their use. Suitable diluent solvents for use on the skin include volatile silicone oils, nonvolatile silicone oils, alcohols, hydrocarbons, esters and ethers, and preferably low molecular linear volatile siloxanes (I) and low molecular cyclic volatility. Siloxane (II), or low molecular branched volatile siloxane (III). Specifically, the linear volatile siloxane (I) is hexamethyldisiloxane (MM) octamethyltrisiloxane (MDM), decamethyltetrasiloxane (MD2M), dodecamethylpentasiloxane (MD3M), tetramethylhexasiloxane (MD4M), And hexadecamethylheptasiloxane (MD5M), wherein the cyclic volatile siloxane (II) is hexamethylcyclotrisiloxane (D ₃ ), octamethylcyclotetrasiloxane (D ₄ ), decamethylcyclopenta At least one selected from the group consisting of siloxane (D ₅ ), and dodecamethylcyclohexasiloxane (D ₆ ), wherein the branched volatile siloxane (III) is heptamethyl-3-((trimethylsilyl) oxy) trisiloxane ( M ₃ T), and / or hexamethyl-3,3, bis ((trimethylsilyl) oxy) trisiloxane (M ₄ T). Among these, it is especially preferable to use one or more selected from the group consisting of hexamethyldisiloxane, octamethyltrisiloxane, octamethylcyclotrisiloxane, decamethylcyclopentasiloxane, and dodecamethylcyclohexasiloxane.

Looking specifically at the method of obtaining a silicone MQ resin through the reaction and combination of i) to vi), R ⁴ ₃ SiR ⁵ composed of the main component of the silicone MQ resin is 1 to 30 parts by weight, preferably 5 to 25 Parts by weight. Further, (R ⁶ O) ₄ Si is 1 to 60 parts by weight, preferably 10 to 50 parts by weight.

The formula of the silicone MQ resin ^{_{(R 4 3 SiO 0. 5}} ) c (SiO 2) from the ^{_{d '(R 4 3 SiO 0}} . 5) c weight / (SiO _{2) d} weight of a' is 0.5 to 2.0, preferably Preferably 0.8-1.5. The c can vary the characteristics of the resins according to the ratio of the group and d ^{_{groups, '(R 4 3 SiO 0}} . 5) c weight / (SiO ₂₎ of _d parts by weight of' the higher the value of which the molecular weight is low, While it tends to have a liquid form, while the value is low, the molecular weight tends to be high and has a solid form.

The solvent is 10 to 50 parts by weight, preferably 20 to 40 parts by weight. The catalyst is 0.001 to 10 parts by weight, preferably 0.1 to 5 parts by weight. When the content of the catalyst exceeds 10 parts by weight, the acidity is increased to cause a lot of gelation phenomenon, which is not suitable for use in the cosmetic composition of the present invention, when the content is less than 0.001 parts by weight, the acidity may not proceed.

After the reaction mixture was mixed, the reaction was carried out at 30 to 100 ° C. for 1 to 8 hours, and the reaction was stopped by adding a reaction stop reagent. 6-8 is suitable for stopping the reaction. In addition, the higher the temperature of the reaction or the longer the reaction time, the same phenomenon as the above may occur, which is not preferable for the formation of Compound B.

In order to separate the reactant, the solvent and the catalyst, a diluent solvent is added at 5 to 60 parts by weight, preferably 10 to 50 parts by weight to separate the solvent and the catalyst layer after standing, and to remove the unreacted product, the secondary product and the solvent. In order to dry under reduced pressure for 1 to 5 hours at 80 ~ 150 ℃. Through this process, the final silicone MQ resin (Compound B) is obtained.

3.silicone MQ -T resin compound

As the final compound of the present invention, a compound and a compound B and a solvent usable in cosmetics are added to the mixture of the compound.

silicon MQ Chemical formula of -T resin: (R ^One _a Si _a O _(1.5) ) _x ( ( R ⁴ ₃ SiO _{0 . 5} ) _c (SiO ₂ ) _d ) _y

In the above formula, R ¹ is an alkyl group having 1 to 8 carbon atoms or an aryl group such as a phenyl group, and an alkyl group having 3 to 8 carbon atoms that may cause relatively steric hindrance is suitable.

R ⁴ is an aryl group such as an alkyl group having 1 to 8 carbon atoms or a phenyl group, preferably methyl. a is 1-20 as an integer, Preferably it is 4-10.

^{_{Furthermore, '(R 4 3 SiO 0}} . 5) c w / w of the ((SiO _{2) d) y} parts by weight of a "is 0.5 to 2.0, preferably from 0.8 to 1.5 is suitable. ^{_{Furthermore, '(R 1 a Si a}} O (1.5)) x weight / of ^{_{((R 4 3 SiO 0.}} 5) c (SiO 2) d) y parts by weight of a' is 6 to 19, preferably 7 to 18.

The silicone MQ-T resin compound consists of the following reactions and combinations of i), ii), iii), iv), v) and vi).

i) Compound A [R ¹ _a Si _a O _(1.5a-0.5b) R ² _b ]

ii) Compound ^{_{B [(R 4 3 SiO 0}} . 5) c (SiO (2-0.5e) R 2 e) d]

iii) solvent

iv) hydrolysis and condensation catalysts

v) neutralizer

vi) diluent solvent

Hereinafter, the reactants i), ii), iii), iv), v) and vi) will be described in detail.

i) Compound A [ R ^One _a Si _a O _(1.5a-0.5b) R ² _b ]

In compound A [R ¹ _a Si _a O _(1.5a-0.5b) R ² _b ], R ¹ is an alkyl group having 1 to 8 carbon atoms or an aryl group such as a phenyl group, preferably having a relatively steric hindrance Alkyl groups of 3 to 8 are suitable.

R ² is a hydroxy or alkoxy (methoxy, ethoxy, propoxy, etc.) group, preferably hydroxy or ethoxy. a is 1-20 as an integer, Preferably it is 4-10. b is 0-18 as an integer, Preferably it is 0-8. Also, b is less than or equal to a + 2, and a + b must always be 2n (n is a natural number) as an integer.

ii) Compound B [( R ⁴ ₃ SiO _{0 . 5} ) _c (SiO _(2-0.5e) R ² _e ) _d ]

Compound ^{_{B [(R 4 3 SiO 0}} . 5) c (SiO (2-0.5e) R 2 e) d] in, R ⁴ is an aryl group such as alkyl group or a phenyl group having 1 to 8 carbon atoms, preferably Methyl is suitable. R ² is a hydroxy or alkoxy (methoxy, ethoxy, propoxy, etc.) group, preferably hydroxy or ethoxy. Wherein in the equation (R ⁴ ₃ SiO _{0.5) c} and ^{_{(SiO (2- 0.5e) R 2}} e) a MQ resin which is formed from the reaction of ^{_{d '(R 4 3 SiO 0}} . 5) c weight of / (SiO ₂ The weight of _d ) is 0.5 to 2.0, preferably 0.8 to 1.5. In addition, e is 0-2 as an integer.

iii) solvent

The solvent is at least one selected from the group consisting of aliphatic alcohols having 2 or more carbon atoms, such as ethanol, isopropanol, butanol, water, and hexamethyldisiloxane, without being limited thereto.

As aliphatic alcohols, solvents such as methanol can not be used as a harmful component in cosmetics as well as a fast hydrolysis process, so alcohols of 2 or more carbon atoms are suitable, but if the carbon number is too long, the process of separating the solvent and catalyst is difficult It may not be easy to volatilize when it is long or under reduced pressure at high temperature.

The solvent does not adversely affect the skin, and the solvent is more preferably water or ethanol. At this time, it is more preferable to mix water and other polar solvents other than water, and it is most preferable to mix water and ethanol. In this case, the water and the polar solvent may be added in a mixed form at the same time, but of course also includes the case in the mixed form.

The ratio of water and ethanol is very important when mixed, and the weight ratio of water / ethanol is 0.5 to 2, which is advantageous for the formation of the MQ-T silicone resin of the present invention. If the weight ratio of water / ethanol exceeds 2, the reactivity may be easily gelled during hydrolysis. Therefore, it is preferable to use a polar solvent other than water to reduce the reactivity to prevent gelation. There is a disadvantage that is not easy.

iv) hydrolysis and Condensation  catalyst

As the hydrolysis and condensation catalyst, a base catalyst or an acid catalyst can be used. As the base catalyst, one or more selected from the group consisting of potassium hydroxide, sodium hydroxide, ammonia, carbonate and the like can be used, and as the acidic catalyst, trifluoromethylsulphonic acid, acetic acid, methylsulphonic acid It may be used one or more selected from the group consisting of, hydrocolic acid, sulfonic acid, sulfuric acid and the like. It is preferable to use a basic catalyst for manufacture of the silicone MQ-T resin compound of this invention.

v) neutralizer

As the neutralizing agent used for the purpose of stopping the reaction, potassium hydroxide, sodium hydroxide, sodium bicarbonate or a combination thereof can be used as the basic neutralizing agent, and citric acid, acetic acid, lactic acid as acidic neutralizing agent. , Hydrocolic acid, sulfonic acid, sulfuric acid or a combination thereof may be used. It is preferable to use an acid neutralizing agent for manufacture of the silicone MQ-T resin compound of this invention.

vi) diluent solvent

In the case of the dilution solvent, any inert solvent which does not significantly affect the hydrolysis and condensation reaction can be used without particular limitation. For example, solvents containing groups having hydrolytic and condensation reactivity such as hydroxy groups, alkoxy groups, etc., limit their use. Suitable diluent solvents for use on the skin include volatile silicone oils, nonvolatile silicone oils, alcohols, hydrocarbons, esters and ethers, and preferably low molecular linear volatile siloxanes (I) and low molecular cyclic volatility. Siloxane (II), or low molecular branched volatile siloxane (III). Specifically, the linear volatile siloxane (I) is hexamethyldisiloxane (MM) octamethyltrisiloxane (MDM), decamethyltetrasiloxane (MD2M), dodecamethylpentasiloxane (MD3M), tetramethylhexasiloxane (MD4M), And hexadecamethylheptasiloxane (MD5M), wherein the cyclic volatile siloxane (II) is hexamethylcyclotrisiloxane (D ₃ ), octamethylcyclotetrasiloxane (D ₄ ), decamethylcyclopenta At least one selected from the group consisting of siloxane (D ₅ ), dodecamethylcyclohexasiloxane (D ₆ ), and the branched volatile siloxane (III) is heptamethyl-3-((trimethylsilyl) oxy) trisiloxane (M ₃ T), and / or hexamethyl-3,3, bis ((trimethylsilyl) oxy) trisiloxane (M ₄ T). Among these, it is especially preferable to use one or more selected from the group consisting of hexamethyldisiloxane, octamethyltrisiloxane, octamethylcyclotrisiloxane, decamethylcyclopentasiloxane, and dodecamethylcyclohexasiloxane.

Wherein i) to a silicone MQ-T resin, and finally the present invention produced by the reaction and combination of ^{_{vi) (R 1 a Si a}} O (1.5)) x ((R 4 3 SiO 0. 5) c ( SiO ₂ ) _d ) _y .

The method for preparing MQ-T is largely compound A [R ¹ _a Si _a O _(1.5a-0.5b) R ² _b ] and compound B [(R ⁴ ₃ SiO _0.5 ) _c (SiO _{(2-0.5e )} R ² _e ) _d ] is mixed, the solvent and the catalyst is added and reacted, and then the neutralizing agent and diluent solvent are purified. The final result is in the form of powder, liquid and gel.

Looking at the manufacturing method of the silicone MQ-T resin in detail, Compound A [R ¹ _a Si _a O _(1.5a-0.5b) R ² _b ] as the main component of the silicone MQ-T resin is 83 to 95 parts by weight, Preferably it is 85-94 weight part.

In addition, the compound ^{_{B [(R 4 3 SiO 0}} . 5) c (SiO (2-0.5e) R 2 e) d] may be 4 to 17 parts by weight, preferably from 5 to 14.5 parts by weight.

When R ¹ _a Si _a O _(1.5a-0.5b) R ² _b is lower than 83 parts by weight, _{^{(R 4 3 SiO 0. 5}} ) c (SiO (2-0.5e) R 2 e) the reaction difficult due to high viscosity during the reaction _d, does not have the flexibility required by the present invention in an amount of high MQ resin , R ¹ _a Si _a O _{(1.5a-0.5b) When} R ² _b is higher than 96 parts by weight, it is a simple liquid form, which has a property of film formation, which is a characteristic of resin, and is persistent and does not adhere to other substrates. It is not suitable for the silicone resin of the present invention.

In addition, the solvent is 10 to 80 parts by weight, preferably 30 to 70 parts by weight, when the solvent content is lower than 10 parts by weight shows a high polymerization degree and a fast reaction rate, it is difficult to control the molecular weight than 80 parts by weight If it is high, there is a problem that the reaction is not shown due to the low degree of polymerization.

The hydrolysis and condensation catalyst is 0.001 to 10 parts by weight, preferably 0.01 to 3 parts by weight, and may be gelated as the basicity and content of the catalyst increase, and the reaction does not proceed as the acidity and content decrease. You may not.

After the reaction mixture was mixed, the reaction was carried out at 80 to 150 ° C. for 1 to 8 hours, and the reaction stopped reagent was added to stop the reaction. 6-8 is suitable for stopping the reaction. In addition, the higher the temperature of the reaction or the longer the reaction time, the same phenomenon may occur as the above form, which is not preferable for the formation of MQ-T resin.

In order to separate the reactant, the solvent and the catalyst, a diluent solvent is added at 20 to 80 parts by weight, preferably 30 to 50 parts by weight to separate the solvent and the catalyst layer after standing, and to remove the unreacted product, the secondary product and the solvent. In order to dry under reduced pressure for 1 to 5 hours at 80 ~ 150 ℃. Through this process, the final silicon MQ-T resin is obtained.

Hereinafter, the present invention will be described in detail through Examples and Comparative Examples. However, the following Examples and Comparative Examples are merely illustrative of the present invention, can be implemented in various different forms and the content of the present invention is not limited by the Examples and Comparative Examples described below.

[ Example ]

Example  One

Hydrocarbon compounds Combined  Polyhedral oligomer Silsesquioxane  Preparation of Compound (Compound A)

50 parts by weight of propyltriethoxysilane and 15 parts by weight of ethanol were added to a round bottom flask equipped with a condenser and stirred at 25 ° C for 10 minutes. Thereafter, 0.3 parts by weight of sulfuric acid and 40 parts by weight of water were slowly added at 40 to 60 ° C, followed by stirring for 4 hours. An appropriate amount of a 10% by weight sodium bicarbonate solution was added at 30 to 40 ° C. so as to have a pH of 7 and stirred for 50 minutes. Then, after sufficiently stirring at room temperature, the mixture was left for 36 hours to separate the lower layer, and the remaining solution was concentrated under reduced pressure at 120 to 150 ° C. for 1 hour, and then cooled and a high pressure filter. Through this process, a polyhedral oligomeric silsesquioxane compound having a liquid hydrocarbon compound bonded thereto was obtained.

Example  2

silicon MQ  Preparation of Resin Compound (Compound B)

In a round bottom flask equipped with a condenser, 50 parts by weight of hexamethyldisiloxane, 45 parts by weight of ethanol, and 100 parts by weight of ethyl silicate-40 were added and stirred at 25 ° C for 10 minutes. Thereafter, 1.5 parts by weight of sulfuric acid was added thereto, and then maintained at 70 to 80 ° C., 60 parts by weight of water was slowly added thereto, followed by stirring for 4 hours. An appropriate amount of a 10% by weight sodium bicarbonate solution was added at 30 to 40 ° C. so that the pH was 7 and then stirred for 30 minutes. Then, 130 parts by weight of decamethylcyclopentasiloxane was added to the mixture at room temperature, and after sufficient stirring, the mixture was left for 24 to 48 hours to separate the lower layer, and the remaining solution was concentrated under reduced pressure at 120 to 150 ° C for 3 hours to obtain a high viscosity silicone MQ resin. Got it.

Example  3

silicon MQ -T Resin Compound Preparation

86 parts by weight of Compound A prepared in Example 1 and 14 parts by weight of Compound B prepared in Example 2 were placed in the same device as in Example 1, and stirred at 70 ° C. for 30 minutes to dissolve. Next, 1 part by weight of a solution of 30 parts by weight of ethanol, 20 parts by weight of water and 5% by weight of potassium hydroxide was added and reacted at 120 to 150 ° C for 3 hours, followed by 10 weights of citric acid at 30 to 40 ° C. An appropriate amount of a solution of% concentration was added to make the pH 7, followed by stirring for 30 minutes. The mixture was left for 24 to 48 hours to separate the lower layer, and the remaining solution was concentrated under reduced pressure at 120 to 150 ° C. for 3 hours to obtain a high viscosity silicone MQ-T resin.

Example  4

silicon MQ -T resin compound Produce

90 parts by weight of Compound A prepared in Example 1 and 10 parts by weight of Compound B prepared in Example 2 were placed in the same device as Example 1, and stirred at 70 ° C. for 30 minutes to dissolve. Then, 1 part by weight of a solution of 30 parts by weight of ethanol, 20 parts by weight of water and 5% by weight of potassium hydroxide, and reacted at 120 to 150 ° C for 3 hours, followed by 10 weights of citric acid at 30 to 40 ° C An appropriate amount of a solution of% concentration was added to make the pH 7, followed by stirring for 30 minutes. The mixture was allowed to stand for 24 to 48 hours to separate the lower layer, and the remaining solution was concentrated under reduced pressure at 120 to 150 ° C for 3 hours to obtain a silicone MQ-T resin having a viscosity.

Example  5

silicon MQ -T resin compound Produce

95 parts by weight of Compound A prepared in Example 1 and 5 parts by weight of Compound B prepared in Example 2 were placed in the same device as Example 1, stirred at 70 ° C. for 30 minutes, and dissolved. Next, 1 part by weight of a solution of 30 parts by weight of ethanol, 20 parts by weight of water and 5% by weight of potassium hydroxide was added and reacted at 120 to 150 ° C for 3 hours, followed by 10 weights of citric acid at 30 to 40 ° C. An appropriate amount of a solution of% concentration was added to make the pH 7, followed by stirring for 30 minutes. The mixture was left for 24 to 48 hours to separate the lower layer, and the remaining solution was concentrated under reduced pressure at 120 to 150 ° C. for 3 hours to obtain a low viscosity silicone MQ-T resin.

Comparative example  One

Hydrocarbon compounds Combined  Polyhedral oligomer Silsesquioxane  Preparation of Compound (Compound A ")

80 parts by weight of propyltriethoxysilane and 10 parts by weight of ethanol were added to the same device as Example 1, followed by stirring at 25 ° C for 10 minutes. Thereafter, 0.3 parts by weight of sulfuric acid and 15 parts by weight of water were slowly added at 40 to 60 ° C, followed by stirring for 4 hours. An appropriate amount of a 10% by weight sodium bicarbonate solution was added at 30 to 40 ° C. so as to have a pH of 7 and stirred for 50 minutes. Then, after sufficiently stirring at room temperature, the mixture was left for 36 hours to separate the lower layer, and the remaining solution was concentrated under reduced pressure at 120 to 150 ° C. for 1 hour, and then cooled and a high pressure filter. Through this process, unlike the oligomeric silsesquioxane compound of Example 1, a polymer type silsesquioxane compound having a hydrocarbon compound bonded to a solid was obtained.

Comparative example  2

silicon MQ -T resin compound Produce

50 parts by weight of Compound A prepared in Example 1 and 50 parts by weight of Compound B prepared in Example 2 were placed in the same apparatus as in Example 1, and stirred at 70 ° C. for 30 minutes to dissolve. Through this process, a high viscosity liquid gel was obtained, but it was impossible to proceed later due to the high viscosity.

Comparative example  3

silicon MQ -T resin compound Produce

65 parts by weight of Compound A prepared in Example 1 and 35 parts by weight of Compound B prepared in Example 2 were placed in the same device as in Example 1, and stirred at 70 ° C. for 30 minutes to dissolve. Next, 1 part by weight of a solution of 30 parts by weight of ethanol, 20 parts by weight of water and 5% by weight of potassium hydroxide was added and reacted at 120 to 150 ° C for 3 hours, followed by 10 weights of citric acid at 30 to 40 ° C. An appropriate amount of a solution of% concentration was added to make the pH 7, followed by stirring for 30 minutes. This was allowed to stand for 24 to 48 hours to separate the lower layer, and the remaining solution was concentrated under reduced pressure at 120 to 150 ° C. for 3 hours to obtain a gel-like silicone MQ-T resin. However, due to the high MQ resin content, it was dissolved in a volatile solvent. The film forming ability when applied to the skin is high, but due to shrinkage and high hardness is not suitable for the result of the resin having the flexibility required by the present invention.

Comparative example  4

silicon MQ -T resin compound Produce

98 parts by weight of Compound A prepared in Example 1 and 2 parts by weight of Compound B prepared in Example 2 were placed in the same apparatus as in Example 1, and stirred at 70 ° C. for 30 minutes to dissolve. Next, 1 part by weight of a solution of 30 parts by weight of ethanol, 20 parts by weight of water and 5% by weight of potassium hydroxide was added and reacted at 120 to 150 ° C for 3 hours, followed by 10 weights of citric acid at 30 to 40 ° C. An appropriate amount of a solution of% concentration was added to make the pH 7, and then stirred for 30 minutes. This was allowed to stand for 24 to 48 hours to separate the lower layer, and the remaining solution was concentrated under reduced pressure at 120 to 150 ° C. for 3 hours to obtain a liquid silicone MQ-T resin. Apart from this, it is not suitable for the result of resin having the property of persistence and other substrates required by the present invention.

Comparative example  5

silicon MQ -T Resin Compound Preparation

90 parts by weight of Compound A prepared in Example 1 and 10 parts by weight of Compound B prepared in Example 2 were placed in the same device as Example 1, and stirred at 70 ° C. for 30 minutes to dissolve. Then, 15 parts by weight of ethanol, 35 parts by weight of water, and 1 part by weight of a solution of 5% by weight of potassium hydroxide were added and reacted at 120 to 150 ° C for 3 hours, followed by 10 weights of citric acid at 30 to 40 ° C. An appropriate amount of a solution of% concentration was added to make the pH 7, and stirred for 30 minutes. This was allowed to stand for 24 to 48 hours to separate the lower layer, and the remaining solution was concentrated under reduced pressure at 120 to 150 ° C. for 3 hours to obtain a high viscosity gel-like silicone MQ-T resin. When it is dissolved in a volatile solvent and applied to the skin, the film forming ability is high, but the condensation reaction occurs very well, and thus the elastic force is decreased due to the high shrinkage and hardness, and thus it is not suitable for the resultant resin having the flexibility required by the present invention.

Comparative example  6

silicon MQ -T resin compound Produce

50 parts by weight of polymer polypropylsilsesquioxane in powder form, 50 parts by weight of compound B prepared in Example 2 and 200 parts by weight of xylene were added to the same device as Example 1, and stirred at 50 ° C. for 1 hour. It was dissolved. Next, 1 part by weight of a solution of 30 parts by weight of ethanol, 20 parts by weight of water and 5% by weight of potassium hydroxide was added and reacted at 120 to 150 ° C for 3 hours, followed by 10 weights of citric acid at 30 to 40 ° C. An appropriate amount of a solution of% concentration was added to make the pH 7, and then stirred for 30 minutes. This was allowed to stand for 24 to 48 hours to separate the lower layer, and the remaining solution was concentrated under reduced pressure at 120 to 150 ° C for 3 hours to obtain a gel-like silicone MQ-T resin, but a slight amount of xylene solvent appeared.

In the production of silicone MQ-T resin, the weight ratio of solvent water / ethanol is suitably 0.5 to 2, and when it is more than 2, the reactivity during hydrolysis may be easily gelled. Therefore, in Comparative Example 5 in which the weight ratio of solvent water / ethanol exceeds 2, as shown in Table 2, a high-viscosity gel-like silicone MQ-T resin is formed. The disadvantage is very low flexibility.

Claims (15)

A silicone MQ-T resin compound according to the following [Formula 1], prepared by adding a solvent and a catalyst to a polyhedral oligomeric silsesquioxane compound and a silicone MQ resin compound having a hydrocarbon compound bonded thereto.
[Formula 1]
(R ¹ _a Si _a O _(1.5a) ) _x ((R ⁴ ₃ SiO _0.5 ) _c (SiO ₂ ) _d ) _y
(However, in the above [Formula 1],
i) R ¹ is an alkyl group having 3 to 8 carbon atoms and R ⁴ is methyl;
ii) a is 4 to 10 as an integer;
iii) the weight of '(R ⁴ ₃ SiO _0.5 ) _c / The weight 'of (SiO ₂ ) _d is 0.5 to 2; And
iv) 'Weight of (R ¹ _a Si _a O _(1.5) ) _x / ((R ⁴ ₃ SiO _0.5 ) _c (SiO ₂ ) _d ) _y is 6 to 19')
The method of claim 1,
Said R ¹ _a Si _a O _(1.5) in the material of Formula 1 is obtained from the following [Formula 2], silicone MQ-T resin compound.
[Formula 2]
R ¹ _a Si _a O _(1.5a-0.5b) R ² _b
(However, in the above [Formula 2],
i) R ² is hydroxy or alkoxy; And
ii) a is 1-20 as an integer and b is 0-18 as an integer. Where b is less than a + 2 and a + b is always an integer 2n.)
The method of claim 1,
In the material of Formula 1, (R ⁴ ₃ SiO _0.5 ) _c (SiO ₂ ) _d is obtained from the following [Formula 3]: Silicone MQ-T resin compound.
[Formula 3]
(R ⁴ ₃ SiO _0.5 ) _c (SiO _(2-0.5e) R ² _e ) _d
(However, in the above [Formula 3],
i) R ² is hydroxy or alkoxy; And
ii) e is an integer of 0 to 2)
The method of claim 1,
In the above [Formula 1],
i) the weight of '(R ⁴ ₃ SiO _0.5 ) _c / The weight of (SiO ₂ ) _d 'is 0.8-1.5,
ii) the weight of (R ¹ _a Si _a O _(1.5a) ) _x / ((R ⁴ ₃ SiO _0.5 ) _c (SiO ₂ ) _d ) _y 'is 6-18, characterized in that the silicon MQ -T resin compound.
The method of claim 2,
In the R ¹ _a Si _a O _(1.5a-0.5b) R ² _b , R ² is hydroxy or ethoxy, silicone MQ-T resin compound.
The method of claim 2,
Wherein _{^{R 1 a Si a O (1.5a}} -0.5b) R 2 b of the b is 0 to 8, a silicone MQ resin T-compound, characterized in that, as an integer.
The method of claim 3,
_Wherein said R ² in said (R ⁴ ₃ SiO _0.5 ) _c (SiO _(2-0.5e) R ² _e ) _d is hydroxy or ethoxy, silicone MQ-T resin compound.
The method of claim 1,
The solvent is silicone MQ-T resin compound, characterized in that any one or more selected from the group consisting of water, aliphatic alcohols having 4 or less carbon atoms, and hexamethyldisiloxane.
The method of claim 8,
The solvent is used by mixing water and aliphatic alcohol,
The aliphatic alcohol is ethanol,
Silicone MQ-T resin compound having a weight ratio of 'water / ethanol' of 0.5 to 2.
The method of claim 1,
The catalyst is silicon MQ-T resin compound, characterized in that at least one selected from the group consisting of potassium hydroxide, sodium hydroxide, ammonia, and carbonate as a base catalyst.
A cosmetic composition comprising the silicone MQ-T resin compound according to any one of claims 1 to 10.
Preparing a polyhedral oligomeric silsesquioxane compound and a silicone MQ resin compound to which a hydrocarbon compound is bound, respectively;
Mixing a polyhedral oligomeric silsesquioxane compound and the silicone MQ resin compound to which the hydrocarbon compound is bonded together with a solvent to obtain a mixed solution; And
Adding a catalyst to the mixed solution to prepare a silicone MQ-T resin compound corresponding to [Formula 1]; comprising, a method for producing a silicone MQ-T resin compound.
[Formula 1]
(R ¹ _a Si _a O _(1.5a) ) _x ((R ⁴ ₃ SiO _0.5 ) _c (SiO ₂ ) _d ) _y
(However, in the above [Formula 1],
i) R ¹ is an alkyl group having 3 to 8 carbon atoms and R ⁴ is methyl;
ii) a is 4 to 10 as an integer;
iii) the weight of '(R ⁴ ₃ SiO _0.5 ) _c / The weight 'of (SiO ₂ ) _d is 0.5 to 2; And
iv) 'Weight of (R ¹ _a Si _a O _(1.5) ) _x / ((R ⁴ ₃ SiO _0.5 ) _c (SiO ₂ ) _d ) _y is 6 to 19')
The method of claim 12,
In the above [Formula 1],
i) the weight of '(R ⁴ ₃ SiO _0.5 ) _c / The weight of (SiO ₂ ) _d 'is 0.8-1.5,
ii) the weight of (R ¹ _a Si _a O _(1.5a) ) _x / ((R ⁴ ₃ SiO _0.5 ) _c (SiO ₂ ) _d ) _y 'is 6-18, characterized in that the silicon MQ Process for the preparation of -T resin compound.
The method of claim 12,
The solvent is water, C4 or less aliphatic alcohol, and hexamethyldisiloxane, characterized in that any one or more selected from the group consisting of, the method of producing a silicone MQ-T resin compound.
The method of claim 13,
The solvent is used by mixing water and aliphatic alcohol,
The aliphatic alcohol is ethanol,
A method for producing a silicone MQ-T resin compound, wherein the weight ratio of 'water / ethanol' is 0.5 to 2.