阅读说明：本技术 制备有机聚硅氧烷凝胶的方法 (Process for preparing organopolysiloxane gels ) 是由 F·桑德迈尔 C·朔塞尔 于 2017-06-12 设计创作，主要内容包括：本发明描述了一种制备有机聚硅氧烷凝胶的方法,其中使用(1a)由式SiO<Sub>2</Sub>(Q单元)和R<Sub>3</Sub>SiO<Sub>1/2</Sub>和R<Sub>2</Sub>R<Sup>1</Sup>SiO<Sub>1/2</Sub>(M单元)组成的不饱和有机聚硅氧烷树脂,其中,R和R<Sup>1</Sup>是具有权利要求1中所限定的定义,以及任选存在的(1b)具有极性有机基团和可氢化硅烷化端基的化合物,与(2)两种具有不同的平均链长和下式(R<Sup>2</Sup><Sub>3-x</Sub>H<Sub>x</Sub>SiO<Sub>1/2</Sub>)(R<Sup>2</Sup><Sub>2</Sub>SiO<Sub>2/2</Sub>)<Sub>a</Sub>(R<Sup>2</Sup>HSiO<Sub>2/2</Sub>)<Sub>b</Sub>(R<Sup>2</Sup><Sub>3-x</Sub>H<Sub>x</Sub>SiO<Sub>1/2</Sub>)(I)的含Si-H的有机聚硅氧烷的混合物在(3)促进Si-键合氢加成到脂族多键的催化剂的存在下进行反应,其中R<Sup>2</Sup>具有权利要求1中所限定的定义,x是0或1,a和b各自为≥0的整数,条件是总和a+b≥30,所述有机聚硅氧烷平均含有至少2个Si-键合的氢原子,优选至少3个Si-键合的氢原子,并且所述两种有机聚硅氧烷的长链的链长(a+b)是短链有机聚硅氧烷的链长(a+b)的至少3倍,其中(1a),任选存在的(1b)和(2)分散在(4)稀释剂中,并且该反应在加入(5)用作催化剂毒物的终止剂化合物而终止。(The invention relates to a method for producing organopolysiloxane gels, wherein (1a) is used 2 (Q unit) and R 3 SiO 1/2 And R 2 R 1 SiO 1/2 (M units) of an unsaturated organopolysiloxane resin of which R and R 1 Is a compound having the definition as defined in claim 1, and optionally present (1b) a compound having a polar organic group and a hydrosilylatable end group, and (2) two compounds having different average chain lengths and the formula (R) 2 3‑x H x SiO 1/2 )(R 2 2 SiO 2/2 ) a (R 2 HSiO 2/2 ) b (R 2 3‑x H x SiO 1/2 ) (ii) a mixture of Si-H containing organopolysiloxanes of formula (I) in which R is reacted in the presence of (3) a catalyst which promotes the addition of Si-bonded hydrogen to aliphatic multiple bonds 2 Having the definitions defined in claim 1X is 0 or 1, a and b are each integers > 0, with the proviso that the sum a + b > 30, the organopolysiloxanes containing on average at least 2 Si-bonded hydrogen atoms, preferably at least 3 Si-bonded hydrogen atoms, and the chain length of the long chains (a + b) of the two organopolysiloxanes being at least 3 times the chain length (a + b) of the short-chain organopolysiloxanes, wherein (1a), optionally (1b) and (2) are dispersed in (4) diluents and the reaction is terminated by addition of (5) terminator compounds which act as catalyst poisons.)

1. A process for preparing an organopolysiloxane gel by reacting

(1a) An unsaturated organopolysiloxane resin consisting of units of the formula:

SiO ₂(Q unit) and

R ₃SiO _1/2and R ₂R ¹SiO _1/2(M unit) of the unit,

wherein the content of the first and second substances,

r may be identical or different and is a monovalent, optionally substituted hydrocarbon radical having from 1 to 18 carbon atoms per radical,

R ¹is a monovalent hydrocarbon radical onto which Si-H groups, preferably omega-alkenyl groups having 2 to 12 carbon atoms, preferably vinyl groups, can be added in a hydrosilylation reaction,

with the proviso that the organopolysiloxane resin contains at least 2R ¹Radical, preferably at least 3R ¹And the molar ratio of M units to Q units is from 0.5 to 4.0, preferably from 0.5 to 2.0, the organopolysiloxane resin may contain small amounts of RSiO in addition to the M and Q units _3/2(T) units or R ₂SiO _2/2(D) Units, preferably in an amount of from 0.01 to 20 mol%, based on the total amount of all siloxane units, and the organopolysiloxane resin may contain up to 10% by weight of free Si-bonded hydroxyl or alkoxy groups,

and optionally (1b) a compound having a polar organic group, preferably a glycoside group, such as an oligosaccharide or polysaccharide group, a polyoxyalkyl group, such as a polyoxyethylene or polyoxypropylene group, a hydroxyl, amide or carboxyl group and a hydrosilylatable terminal group, with

(2) A mixture of two Si-H-containing organopolysiloxanes having different average chain lengths and of the formula (I) below is reacted in the presence of (3) a catalyst which promotes the addition of Si-bonded hydrogen to aliphatic multiple bonds,

(R ² _3-xH _xSiO _1/2)(R ² ₂SiO _2/2) _a(R ²HSiO _2/2) _b(R ² _3-xH _xSiO _1/2) (I)

wherein R is ²Identical or different and are unsubstituted or optionally heteroatom-substituted aliphatic, cycloaliphatic or aromatic, optionally polycyclic C ₁-C ₁₈A hydrocarbon group,

x is a number of 0 or 1,

a and b are each an integer of 0 or more,

provided that the sum a + b is equal to or greater than 30,

the organopolysiloxanes containing on average at least 2 Si-bonded hydrogen atoms, preferably at least 3 Si-bonded hydrogen atoms, and the chain length (a + b) of the long chains of the two organopolysiloxanes being at least 3 times the chain length (a + b) of the short-chain organopolysiloxanes,

wherein (1a), optionally (1b) and (2) are dispersed in (4) a diluent which is preferably an organopolysiloxane having from 2 to 200 silicon atoms, preferably from 2 to 50 silicon atoms, or an organic diluent or a mixture of an organopolysiloxane having from 2 to 200 silicon atoms, preferably from 2 to 50 silicon atoms and an organic diluent, and

the reaction is terminated by the addition of (5) a terminator compound which acts as a catalyst poison.

2. The method of claim 1, wherein x in formula (I) is 0.

3. The process as claimed in claim 1 or 2, wherein the sum a + b ≧ 55 in the formula (I).

4. A process as claimed in claim 1,2 or 3, characterized in that the catalyst (3) used is a metal catalyst, preferably a platinum catalyst, in an amount of from 1 to 100ppm by weight (parts by weight per million parts by weight), calculated in each case as elemental metal, preferably elemental platinum, based in each case on the total weight of the components (1a), optionally present (1b) and (2).

5. A process as claimed in any of claims 1 to 4, characterized in that the diluent (4) used is a polydimethylsiloxane having from 2 to 50 silicon atoms, an aliphatic or cycloaliphatic hydrocarbon having from 4 to 30 carbon atoms, or an ester of a carboxylic acid having from 2 to 30 carbon atoms.

6. The process according to any of claims 1 to 5, characterized in that the terminator compound (5) used is a compound having a functional group which acts as a catalyst poison, the terminator compound (5) used preferably being an organic compound having a mercapto group (SH) or an organopolysiloxane having a mercaptoalkyl group, preferably an organopolysiloxane having a 3-mercaptopropyl group.

7. The process according to any one of claims 1 to 6, wherein the terminator compound (5) is used in an amount of at least 1.1 mole of a functional group causing termination, preferably a mercapto group, per mole of elemental metal, in particular elemental platinum, in the catalyst (3).

8. The process according to any one of claims 1 to 7, wherein the organopolysiloxane gel obtained after the reaction is homogenized to give a storage-stable organopolysiloxane gel, "storage-stable" meaning that the organopolysiloxane gel formed does not separate into two or more phases during storage at room temperature (20 ℃) for 6 months.

9. The process according to any one of claims 1 to 8, wherein the organopolysiloxane gel thus obtained is diluted with a further diluent (4) and/or an active ingredient for personal care or health care, and then optionally homogenized.

10. Use of the organopolysiloxane gel prepared according to any of claims 1 to 9 in cosmetic compositions.

Example (b):

the following examples serve to further illustrate the invention and to describe its function and use in practice. In this regard, they are to be regarded as illustrative rather than restrictive.

These examples illustrate physical parameters determined by the test methods described below. If no detailed information about the exact traceability of the measurements is available in the embodiment text, these are already given in the description of the test method herein. In other words, at this point, further details are considered to be those given in the text of the test method.

The analysis method comprises the following steps:

the viscosity of the organopolysiloxane gels is determined at 25 ℃ at a shear rate of 1/s in accordance with DIN EN ISO 3219.

The viscosity of the organopolysiloxanes, for example of Si-H-containing crosslinkers, organopolysiloxane resins and polydimethylsiloxanes is determined in the linear range at 25 ℃ in accordance with DIN 53019.

The iodine number is determined by the method according to Wijs in accordance with DIN 53241-1.

Gel permeation chromatography was performed according to ISO 16014-1 and ISO 16014-3 to determine the weight average molecular weight Mw.

The organopolysiloxane gels of the present invention give sensory advantages in cosmetic applications, since they improve the dispersibility of the product on the skin and impart a silky smooth feel to the product. Organopolysiloxane gels are comparable in performance only when they are adjusted to a uniform viscosity for sensory testing. A particularly advantageous viscosity for this purpose has been found to be 75000-120,000mPas at 25 ℃. The criterion for successful production of organopolysiloxane gels is therefore the possibility of establishing this viscosity channel. If this is not possible, there is no comparability with other organopolysiloxane gels. One particular feature of the method of the invention is that it allows the establishment of a target viscosity, for example 75000-. This is demonstrated in the examples below, and this property is separated from the rest of the prior art.

The sensory properties of the organopolysiloxane gels described in the following examples were evaluated by 5 trained testers (panelists).

In the case of each product, the panelists applied 0.05g to the clean lower arm over a circular area of 20cm2 and the dispensability of the organopolysiloxane gels relative to each other was compared. Administration was performed with the index or middle finger at a rotation rate of two rotations per second. A total of 30 revolutions were performed. After a waiting time of 60 seconds, the silkiness of the residues of the organopolysiloxane gels relative to one another was compared.

Here, the relatively direct comparability is possessed only by organopolysiloxane gels produced using the same or at least the same diluent, i.e. more particularly volatile or nonvolatile diluents. Since different diluents lead to different behavior in terms of application and residue, products with different diluents in each case have to be evaluated separately from one another.