JPH036181B2 - - Google Patents

Description

[Detailed description of the invention]

(Industrial Application Field) The present invention relates to a gel composition, particularly a gel composition based on silicone oil that does not use fillers such as silica and is useful as a base material for cosmetics. It is. (Prior Art) Various silicone oils are added to pastes, creams, pressed compositions, etc. for cosmetics and medical purposes, but there are few examples of the use of silicone compositions as a base material. This is because to make silicone oil into a gel, it is necessary to add thickeners such as hydrophobic silica and bentone as inorganic fillers, and the silicone oil used also has a viscosity of 100cS or more at 25℃. Because it needs to have a high viscosity, when the gel-like material obtained in this way is applied to the skin surface, it feels heavy and has a long-term sticky feeling because it has almost no volatile matter. It is said that this is because there is a disadvantage in remaining in the country over time. Therefore, there is a long-awaited need for a gel-like composition based on silicone, which has low viscosity and high volatility, and which solves these drawbacks. (Structure of the Invention) The present invention relates to a silicone-based gel composition that solves the above-mentioned disadvantages. This is equation (1) (R ¹ is a hydrogen atom or a carbon number 1 to 6
a cyclic diorganopolysiloxane represented by a valent saturated hydrocarbon group, ^R2 is a monovalent saturated hydrocarbon group having 2 to 6 carbon atoms, m is an integer of 1 to 6, n is an integer of 0 to 5, and m+n=3 to 6) 15 to 95 parts by weight, (2) boiling point under normal pressure
0 to 75 parts by weight of one or more organopolysiloxanes or organopolysiloxane mixtures selected from dimethylpolysiloxane or methylphenylpolysiloxane having a temperature of 300°C or less;
(3) It is characterized by comprising 5 to 30 parts by weight of dextrin fatty acid ester. That is, the present inventors have conducted various studies on gel-like compositions based on silicone oil, which are particularly useful for cosmetics and medical purposes, and have found that the silicone oil is a cyclic diorganopolysiloxane represented by the above formula. If necessary, use a mixture of dimethylpolysiloxane or methylphenylpolysiloxane with a boiling point of 300℃ or less at normal pressure, and use dextrin fatty acid ester as a gelling agent to achieve the desired gel-like composition. This gel-like composition does not contain any inorganic fillers, so when applied to the skin, it has light extensibility and provides a refreshing feel, and it is non-toxic. The present invention was completed by confirming that it is useful as a solid or semi-solid base suitable for cosmetics and medical applications because of its extremely low content. The silicone oil as the first component constituting the gel composition of the present invention has the formula , R ¹ is a hydrogen atom or a monovalent saturated hydrocarbon group having 1 to 6 carbon atoms selected from methyl group, ethyl group, propyl group, butyl group, pentyl group, hexyl group, etc., and R ² is ethyl group, propyl group,
A saturated monovalent hydrocarbon group having 2 to 6 carbon atoms selected from butyl group, pentyl group, hexyl group, etc., m is an integer of 1 to 6, n is an integer of 0 to 5, and m+n = 3 to 6. Ru. In addition, this product may be used alone or in a mixture of two or more types, but the organic groups represented by R ¹ and R ² described above have a carbon number of 7 or more. When this composition is applied to the skin, it feels sticky, so it needs to have 6 or less carbon atoms. In addition, the organic group content of this first component (organic groups R ¹ , R ² ,
Total weight of ₃ CH groups ÷ Total weight x 100) That is 42% by weight
If it is less than 60% by weight, it will be difficult to gel, and if it is more than 60% by weight, the composition will feel sticky when applied to the skin, etc., and this composition will become less volatile and the sticky feeling will remain for a long time. However, since this results in an unfavorable feel during use, it is preferable that the content is in the range of 42 to 60% by weight. In addition,
The amount of this first component to be used is 15% or less based on 100 parts by weight of the gel composition, and if it is more than 95 parts by weight, it will not gel.
Parts by weight are required. Further, as mentioned above, the second component used as necessary in this composition has a boiling point under normal pressure.
Dimethylpolysiloxane or methylphenylpolysiloxane with a temperature below 300℃, including hexamethylcyclotrisiloxane, octamethylcyclotetrasiloxane, decamethylcyclopentasiloxane, dodecamethylcyclohexasiloxane, hexamethyldisiloxane, octamethyl Examples include trisiloxane, decamethyltetrasiloxane, dodecamethylpentasiloxane, tetradecamethylhexasiloxane, phenyltris(trimethylsiloxa)silane, diphenylbis(trimethylsiloxy)silane, and these are one type of organopolysiloxane. The siloxane may be a mixture of two or more of these siloxanes. In addition, the boiling point of this substance under normal pressure is
If the temperature is higher than 300℃, the composition will not volatilize for a long time after being applied to the skin, and it will remain on the skin and leave a sticky feeling, making the feeling of use undesirable. However, if the amount used is 75 parts by weight or more in 100 parts by weight of the gel composition,
Since this composition will not gel, the amount needs to be 75 parts by weight or less. Next, the dextrin fatty acid ester as the third component in this gel composition has, for example, the following structural formula: A is a hydrogen atom or an acyl group having 8 to 20 carbon atoms, and more than 50% of the total A moles are acyl groups, and l is 20 to 30, but the amount used is This third in 100 parts by weight of the gel composition
If the amount of the component is less than 5 parts by weight, the gelation of the silicone oil will not proceed, and if it is more than 30 parts by weight, the resulting composition will be too hard and have poor extensibility, so it should be in the range of 5 to 30 parts by weight. That is required. The gel composition of the present invention can be obtained by uniformly mixing predetermined amounts of the first to third components described above, but this mixing is preferably carried out at 50 to 100°C, for example, at 100°C. The cyclic organopolysiloxane as the first component, the methylpolysiloxane or methylphenylpolysiloxane as the second component, and the dextrin fatty acid ester as the third component are uniformly dissolved by heating and stirring at a temperature below ℃. By cooling after that, the desired homogeneous gel-like composition can be obtained. It should be noted that various oily agents, fragrances, medicinal ingredients, antioxidants, pigments, dyes, etc. may be added to this composition as long as they do not significantly deviate from the physical properties of the composition of the present invention. Next, examples of the present invention will be given, and the viscosity in the examples is a value measured at 25°C. Examples 1 to 3 200 g of concentrated hydrochloric acid and 32 g of water were placed in a hard glass flask, and while stirring while keeping the temperature at 25 to 45°C, 286 g (2 moles) of ethylmethyldichlorosilane was added dropwise over 30 minutes. After finishing stirring at 60-70℃ for 2 hours and discarding the lower aqueous layer,
500 ml of 3% heavy tank water was added thereto, and the mixture was stirred at room temperature for 2 hours to neutralize the oil layer. Next, this product was dehydrated and subjected to simple distillation, and 91g (yield 61%) of a 119-124℃ fraction at a reduced pressure of 13mmHg was collected.
It is a colorless, transparent, odorless liquid of 4.6 cS, and gas chromatograph analysis shows that it is composed of 1.4% trimer, 91.7% tetramer, 6.6% pentamer, and 0.3% hexamer.
It was confirmed that the mixture was a cyclic ethylmethylpolysiloxane mixture (hereinafter abbreviated as cyclic ethylmethylpolysiloxane) with an organic group content of 50% by weight. Next, dextrin fatty ester Leopard KL (trade name manufactured by Chiba Flour Milling Co., Ltd.) in the amount also shown in Table 1 was added to the cyclic ethylmethylpolysiloxane in the amount shown in Table 1. Stir at ℃ and confirm that it has become a homogeneous solution, then stop stirring.
When rapidly cooled in an ice water bath, a uniform gel-like composition was obtained, and the consistency of this composition was determined by JIS.
When the volatile content was measured in accordance with K2220, the results shown in Table 1 were obtained.

[Table] Examples 4 to 5 Cyclic ethylmethylpolysiloxane produced in Examples 1 to 3 above and decamethylcyclopentasiloxane KF96L (trade name manufactured by Shin-Etsu Chemical Co., Ltd.) with a viscosity of 2 cS or a viscosity of 2.3 cS octamethylcyclotetrasiloxane KF994 [product name manufactured by the company] and dextrin fatty ester Leopard KL
[mentioned above] in the weight shown in Table 2, 60 ~
When the solution was stirred at 70℃ to form a homogeneous solution and then rapidly cooled in an ice water bath, a white to pale yellow homogeneous gel-like composition was obtained.The consistency and volatile content of these were examined and they are also listed in Table 2. The exact results were obtained.

[Table] Examples 6 to 9 Ethylmethyldichlorosilane was used instead of ethylmethyldichlorosilane used in the production of cyclic ethylmethylpolysiloxane in Examples 1 to 3.
143g (1 mole) and 129g dimethyldichlorosilane
95 g (yield: 59%) of a colorless, transparent, and odorless liquid with a viscosity of 3.4 cS was prepared in the same manner as in Examples 1 to 3, except that a silane mixture consisting of (1 mol) was used. As a result of analysis, it was confirmed that it was a cyclic ethylmethylpolysiloxane mixture (hereinafter abbreviated as cyclic ethylmethylpolysiloxane) with an organic group content of 45% by weight. Next, dextrin fatty ester Leopard KL [mentioned above] was added to the cyclic ethylmethylpolysiloxane in the amount shown in Table 3 and treated in the same manner as in Examples 1 to 3. A uniform white to pale yellow gel-like composition was obtained,
This product exhibited gel properties as listed in Table 3. In addition, for this cyclic ethylmethylpolysiloxane, phenyltolus (trimethylsiloxy) silane KF58 [trade name manufactured by Shin-Etsu Chemical Co., Ltd.] and dextrin fatty ester Leopard are used.
When KL [mentioned above] was mixed with the weight shown in Table 3 and treated in the same manner as in Examples 1 to 3, the color was white.
A pale yellow, uniform gel-like composition was obtained, which exhibited gel properties as listed in Table 3.

[Table] Examples 10 to 11 1,3,5,7-tetramethyl-1,5-dipropylcyclotetrasiloxane (organic group content 46% by weight) in the amount shown in Table 4 was added to When the amount of dextrin fatty acid ester Leopard KL [mentioned above] shown in the table was added and treated in the same manner as in Examples 1 to 3, a white to pale yellow uniform gel-like composition was obtained. The gel properties were shown as listed in Table 4.

[Table] Comparative example Octamethylcyclotetrasiloxane/KF-
To 90 g of 994 (organic group content 40% by weight) [see above], 10 g of dextrin fatty acid ester Leopard KL [see above] was added and stirred at 60 to 70°C, but Leopard KL did not dissolve uniformly. After stirring for 2 hours, the mixture was rapidly cooled in an ice water bath, and Rheopar precipitated.
The composition did not gel and remained liquid.

Claims (1)

[Claims] 1 (1) Formula (Here, R ¹ is a hydrogen atom or a monovalent saturated hydrocarbon group having 1 to 6 carbon atoms, and R ² is a monovalent saturated hydrocarbon group having 2 to 6 carbon atoms.
Cyclic diorganopolysiloxane represented by a valent saturated hydrocarbon group, m is an integer of 1 to 6, n is an integer of 0 to 5, and m+n = 3 to 6)
15-95 parts by weight, (2) One or more organopolysiloxanes or organopolysiloxane mixtures selected from dimethylpolysiloxane or methylphenylpolysiloxane whose boiling point under normal pressure is 300°C or less 0-75 (3) 5 to 30 parts by weight of dextrin fatty acid ester.