CN106236608B - Composition for forming in-situ polymerized film, in-situ polymerized film and application thereof - Google Patents
Composition for forming in-situ polymerized film, in-situ polymerized film and application thereof Download PDFInfo
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- CN106236608B CN106236608B CN201610674270.XA CN201610674270A CN106236608B CN 106236608 B CN106236608 B CN 106236608B CN 201610674270 A CN201610674270 A CN 201610674270A CN 106236608 B CN106236608 B CN 106236608B
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/84—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
- A61K8/89—Polysiloxanes
- A61K8/895—Polysiloxanes containing silicon bound to unsaturated aliphatic groups, e.g. vinyl dimethicone
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/84—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
- A61K8/89—Polysiloxanes
- A61K8/891—Polysiloxanes saturated, e.g. dimethicone, phenyl trimethicone, C24-C28 methicone or stearyl dimethicone
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q1/00—Make-up preparations; Body powders; Preparations for removing make-up
- A61Q1/02—Preparations containing skin colorants, e.g. pigments
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q17/00—Barrier preparations; Preparations brought into direct contact with the skin for affording protection against external influences, e.g. sunlight, X-rays or other harmful rays, corrosive materials, bacteria or insect stings
- A61Q17/04—Topical preparations for affording protection against sunlight or other radiation; Topical sun tanning preparations
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
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Abstract
The invention relates to the field of composite materials, in particular to a composition for forming an in-situ polymerized film, the in-situ polymerized film and application of the composition and the film. The composition for forming an in-situ polymerization film comprises a base component and a catalyst component, wherein the base component contains first vinyl silicone oil and hydrogen-containing silicone oil, and the content of the hydrogen-containing silicone oil is 1-40 parts by weight based on 100 parts by weight of the first vinyl silicone oil; the catalyst component contains Pt; the catalyst component is used in an amount of 0.001 to 0.1 parts by weight based on the weight of Pt therein, relative to 100 parts by weight of the first vinyl silicone oil. The composition for forming the in-situ polymerized film can be used for forming the in-situ polymerized film on the surface of skin, so that the appearance of slack or wrinkles of the skin is effectively improved, the skin looks firmer, the in-situ polymerized film has strong air permeability, the health of the skin is not influenced, and the functions of sun protection, antibiosis, spot covering, flaw covering and the like can be realized.
Description
Technical Field
The invention relates to the field of composite materials, in particular to a composition for forming an in-situ polymerized film, the in-situ polymerized film obtained by carrying out in-situ polymerization on the composition for forming the in-situ polymerized film, and the composition for forming the in-situ polymerized film and/or the application of the in-situ polymerized film on the surface of skin.
Background
The skin is the primary medium for the human body to contact the external environment and is also the natural first physical barrier, so that the invasion of external pollutants is effectively blocked. However, the barrier function of the skin gradually deteriorates due to the effects of skin aging, skin diseases, environmental pollution, and the like. Meanwhile, as people pay more and more attention to the fields of daily life related to skin health, color and moisture content, such as beauty treatment, sun protection and the like, a thin film material which has the function similar to natural skin, does not influence the health of the natural skin, and provides special functions (such as sun protection, antibiosis, spot covering and the like) which are not possessed by the natural skin and is used for the similar skin needs urgent research and wide application. At present, no film material which has weather resistance and has the similar function of natural skin exists in research or market. Wherein the weather resistance is a key property, and only the development of a composition with low temperature resistance, high temperature resistance and ultraviolet resistance can provide practical possibility for the actual industrial production, use and storage of products.
Disclosure of Invention
The invention aims to provide a composition for forming an in-situ polymerized film, the in-situ polymerized film obtained by carrying out in-situ polymerization on the composition for forming the in-situ polymerized film, and the composition for forming the in-situ polymerized film and/or the application of the in-situ polymerized film on the surface of skin. The composition for forming the in-situ polymerized film can be used for forming the in-situ polymerized film on the surface of skin, so that the appearance of slack or wrinkles of the skin is effectively improved, the skin looks firmer, the in-situ polymerized film has strong air permeability, the health of the skin is not influenced, and the functions of sun protection, antibiosis, spot covering, flaw covering and the like can be realized.
The inventors of the present invention have found that a thin film having skin-like properties can be formed on the skin surface by separately storing a base component having a vinyl silicone oil as a main component and a catalyst component having platinum as a main catalyst in specific components and ratios and performing in situ polymerization on the skin surface. According to a preferred embodiment of the present invention, the present inventors have also found that specific additives (stabilizers, functional materials, etc.) can be combined with the composition for forming an in-situ polymerized film of the present invention to achieve better effects. According to another preferred embodiment of the invention, the catalyst component contains, in addition to Pt, a vinyl silicone oil and a vinyl MQ resin.
The first aspect of the present invention provides a composition for forming an in-situ polymerized film, wherein the composition for forming an in-situ polymerized film comprises a base component and a catalyst component, the base component comprises a first vinyl silicone oil and a hydrogen-containing silicone oil, wherein the content of the hydrogen-containing silicone oil is 1 to 40 parts by weight based on 100 parts by weight of the first vinyl silicone oil; the catalyst component contains Pt; the catalyst component is used in an amount of 0.001 to 0.1 parts by weight based on the weight of Pt therein, relative to 100 parts by weight of the first vinyl silicone oil.
The second aspect of the present invention provides an in-situ polymerized film, wherein the in-situ polymerized film is prepared by applying the matrix component and the catalyst component of the first aspect of the present invention to the surface of an object in sequence or mixing them and then applying the mixture to the surface of the object, and waiting for at least 30 seconds.
In a third aspect, the present invention provides a composition for forming an in situ polymerized film according to the first aspect of the invention and/or the use of an in situ polymerized film according to the second aspect of the invention on a skin surface.
The composition for forming an in-situ polymerized film and the in-situ polymerized film of the present invention have advantages over existing cosmetics in at least:
(1) the in-situ polymerized film can be completely transparent on the surface of the skin, and simultaneously, can smooth slack and wrinkles to a great extent, so that the skin looks firmer and smoother;
(2) the in-situ polymerized film has strong air permeability, the performance of the in-situ polymerized film is similar to that of real skin, and the normal function of the skin is not influenced completely;
(3) the in-situ polymerized film of the invention does not influence the use of other cosmetics and color cosmetics;
(4) the in-situ polymerized film can realize different additional functions by adding different functional materials, and can be even used for treating skin diseases, scalds and the like.
Additional features and advantages of the invention will be set forth in the detailed description which follows.
Detailed Description
The following describes in detail specific embodiments of the present invention. It should be understood that the detailed description and specific examples, while indicating the present invention, are given by way of illustration and explanation only, not limitation.
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
The first aspect of the present invention provides a composition for forming an in-situ polymerized film, wherein the composition for forming an in-situ polymerized film comprises a base component and a catalyst component, the base component comprises a first vinyl silicone oil and a hydrogen-containing silicone oil, wherein the content of the hydrogen-containing silicone oil is 1 to 40 parts by weight based on 100 parts by weight of the first vinyl silicone oil; the catalyst component contains Pt; the catalyst component is used in an amount of 0.001 to 0.1 parts by weight based on the weight of Pt therein, relative to 100 parts by weight of the first vinyl silicone oil.
In the present invention, since the matrix component and the catalyst component are liable to react, they are preferably stored independently of each other.
In the present invention, the hydrogen-containing silicone oil is contained in an amount of preferably 5 to 30 parts by weight, more preferably 12 to 22 parts by weight, based on 100 parts by weight of the first vinyl silicone oil.
In the present invention, the viscosity of the first vinyl silicone oil may be 2000-30000 mPas, preferably 2000-15000 mPas, more preferably 2000-7000 mPas; the vinyl group content may be 0.1 to 7.5 mol%, preferably 0.1 to 5 mol%, more preferably 1 to 4 mol%.
In the present invention, the first vinyl silicone oil may be selected from one or more of monovinyl-terminated polymethylvinylsiloxane, polyvinyl-terminated polymethylvinylsiloxane, monovinyl-terminated polydimethylsiloxane, and polyvinyl-terminated polydimethylsiloxane, and is preferably monovinyl-terminated polydimethylsiloxane and/or polyvinyl-terminated polydimethylsiloxane. When the first vinyl silicone oil is a mixture of monovinyl-terminated polydimethylsiloxane and polyvinyl-terminated polydimethylsiloxane, the mass ratio of the monovinyl-terminated polydimethylsiloxane to the polyvinyl-terminated polydimethylsiloxane is preferably 1: 0.5-2, more preferably 1: 0.8-1.2. Wherein the polyvinyl terminated polydimethylsiloxane is preferably divinyl terminated polydimethylsiloxane and/or trivinyl terminated polydimethylsiloxane, most preferably trivinyl terminated polydimethylsiloxane. In addition, the first vinyl silicone oil of the present invention may be used together with a polydimethylsiloxane, which is preferably used in an amount of not more than 5% by weight (based on the total weight of the first vinyl silicone oil and the polydimethylsiloxane).
In the present invention, the terms "monovinyl-terminated polydimethylsiloxane" and "polyvinyl-terminated polydimethylsiloxane" follow the definitions customary in the art, i.e., the term "monovinyl-terminated polydimethylsiloxane" refers to a molecule in which one of the three methyl groups attached to the silicon atoms at both ends of the polydimethylsiloxane molecular chain is replaced by one vinyl group; the term "polyvinyl-terminated polydimethylsiloxane" refers to a molecule in which a plurality of (two or three) of three methyl groups bonded to silicon atoms at both ends of a polydimethylsiloxane molecular chain are substituted with a plurality of (two or three) vinyl groups. The terms "monovinyl-terminated polymethylvinylsiloxane" and "polyvinyl-terminated polymethylvinylsiloxane" can be defined by replacing "polydimethylsiloxane" with "polymethylvinylsiloxane" with reference to the above definition. By way of example of molecular structural formula, the molecular structural formula of the polydimethylsiloxane is shown as the following formula (1), and the molecular structural formulas of the monovinyl-terminated polydimethylsiloxane, the divinyl-terminated polydimethylsiloxane and the trivinyl-terminated polydimethylsiloxane are respectively shown as the following formula (2), formula (3) and formula (4),
in the present invention, the hydrogen-containing silicone oil may have a viscosity of 5 to 7000 mPas, preferably 5 to 1500 mPas, more preferably 5 to 500 mPas, and still more preferably 10 to 50 mPas.
In the present invention, the hydrogen content in the hydrogen-containing silicone oil may be 0.01 to 1.5% by weight, preferably 0.1 to 0.8% by weight, more preferably 0.1 to 0.4% by weight.
In the present invention, the base component may further contain a thixotropic material, which may be contained in an amount of 1 to 30 parts by weight, preferably 5 to 25 parts by weight, and more preferably 8 to 22 parts by weight, based on 100 parts by weight of the first vinyl silicone oil; the thixotropic material may be selected from one or more of silica, zinc oxide and titanium dioxide, preferably silica. The thixotropic material is in a nanometer scale, and the average particle diameter of the thixotropic material can be 5 to 50 nanometers, and preferably 5 to 25 nanometers.
In the present invention, the matrix component may further contain a stabilizer and/or a functional material.
In the present invention, preferably, the stabilizer is selected from one or more of ethynl cyclohexanol, methyl butynol, and silicone-modified alkynol; the stabilizer may be contained in an amount of 0.001 to 5 parts by weight, preferably 0.001 to 0.1 part by weight, more preferably 0.001 to 0.01 part by weight, based on 100 parts by weight of the first vinyl silicone oil.
In the present invention, preferably, the functional material may be various functional materials used in the art for addition to cosmetics, for example, may be selected from one or more of an ultraviolet ray resistant functional material, a medicinal functional material, and a concealer functional material. The content of the ultraviolet resistant functional material can be 1 to 30 parts by weight, preferably 10 to 30 parts by weight, based on 100 parts by weight of the first vinyl silicone oil; the content of the medicinal functional material is 0.01-1 weight part, preferably 0.1-0.5 weight part; the content of the spot-concealing and flaw-concealing functional material is 0.1-2 parts by weight, preferably 0.5-1.2 parts by weight.
The inventor of the invention finds that better effects can be achieved by using several specific functional materials, wherein the ultraviolet-resistant functional materials are preferably one or more of titanium dioxide, zinc dioxide, silicon dioxide, isooctyl p-dimethylaminobenzoate and avobenzone, and are more preferably silicon dioxide and/or titanium dioxide. The medicinal functional material is preferably one or more of nitrofurazone, benzalkonium chloride and dexamethasone acetate. The spot-covering and flaw-covering functional material is preferably one or more of talcum powder, calcium carbonate and magnesium carbonate, the talcum powder can be 0.5-5 parts by weight, preferably 0.5-1 part by weight, the calcium carbonate can be 0.1-3.7 parts by weight, preferably 0.1-0.5 part by weight, and the magnesium carbonate can be 0.1-3.7 parts by weight, preferably 0.1-0.5 part by weight, based on 100 parts by weight of the first vinyl silicone oil.
In the present invention, Pt is the main catalytic component in the catalyst component. The catalyst component is preferably used in an amount of 0.002 to 0.05 parts by weight, more preferably 0.004 to 0.04 parts by weight, based on the weight of Pt therein, relative to 100 parts by weight of the first vinyl silicone oil. The term "by weight of Pt therein" means that the weight of Pt therein alone is calculated regardless of the weight of other components contained in the catalyst component, and the amount of the catalyst component used is characterized by the weight of Pt as the catalyst component.
In the present invention, the Pt is present in the form of a platinum catalyst, and the content of Pt in the platinum catalyst may be 0.05 to 20% by weight, preferably 0.2 to 5% by weight, and more preferably 0.2 to 2% by weight. The platinum catalyst may be selected from one or more of chloroplatinic acid, platinum nanoparticles, and organic-platinum complexes; wherein the organic-platinum complex is preferably an isopropanol-platinum complex and/or an organosilicon-platinum complex, wherein the organosilicon in the organosilicon-platinum complex can be, for example, tetramethyltetravinylcyclotetrasiloxane and/or 2,4, 6-trivinyl-2, 4, 6-trimethylcyclotrisiloxane; wherein the platinum nanoparticles have an average particle diameter of 1 to 50 nm, preferably 1 to 15 nm, more preferably 1 to 5 nm.
In the present invention, the catalyst component may further contain a second vinyl silicone oil. The content of the second vinyl silicone oil may be 80 to 160 parts by weight, preferably 100 to 140 parts by weight, with respect to 100 parts by weight of the first vinyl silicone oil.
In the present invention, the second vinyl silicone oil may be the same as or different from the first vinyl silicone oil, and the viscosity of the second vinyl silicone oil may be 1000-50000 mPa.s, preferably 2000-10000 mPa.s, wherein the content of vinyl groups is 0.1-2.5 wt%, more preferably 1-2 wt%.
In the present invention, the second vinyl silicone oil may be selected from one or more of monovinyl-terminated polymethylvinylsiloxane, polyvinyl-terminated polymethylvinylsiloxane, monovinyl-terminated polydimethylsiloxane, and polyvinyl-terminated polydimethylsiloxane, and is preferably monovinyl-terminated polydimethylsiloxane and/or polyvinyl-terminated polydimethylsiloxane. When the second vinyl silicone oil is a mixture of monovinyl-terminated polydimethylsiloxane and polyvinyl-terminated polydimethylsiloxane, the mass ratio of monovinyl-terminated polydimethylsiloxane to polyvinyl-terminated polydimethylsiloxane is preferably 1: 0.5-2, more preferably 1: 0.8-1.2. Wherein the polyvinyl terminated polydimethylsiloxane is preferably divinyl terminated polydimethylsiloxane and/or trivinyl terminated polydimethylsiloxane, most preferably trivinyl terminated polydimethylsiloxane. The divinyl second silicone oil of the present invention may be used together with a polydimethylsiloxane, which is preferably used in an amount of not more than 5 wt% (based on the total weight of the divinyl second silicone oil and the polydimethylsiloxane).
In the present invention, the catalyst component also contains a vinyl MQ silicone resin. The content of the vinyl MQ silicone resin may be 2 to 25 parts by weight, preferably 8 to 12 parts by weight, with respect to 100 parts by weight of the first vinyl silicone oil. The vinyl MQ silicone resin is a silicone resin comprising siloxane segments having mono-functionality and siloxane condensation segments having tetra-functionality, the content of the siloxane segments having mono-functionality in the vinyl MQ silicone resin being 1 to 12 wt%, preferably 2 to 8 wt%, and the content of the siloxane condensation segments having tetra-functionality being 2 to 30 wt%, preferably 5 to 20 wt%. Preferably, the viscosity of the vinyl MQ silicone resin is 2000-100000 mPa-s, more preferably 7000-57000 mPa-s.
The base component and the catalyst component of the present invention may each independently additionally contain common other additives such as an antioxidant, a perfume, a pigment for cosmetic foundation, etc., and the pigment for cosmetic foundation may be used in an amount of 1 to 10 parts by weight, preferably 2 to 5 parts by weight, the antioxidant may be used in an amount of 0.1 to 3.7 parts by weight, preferably 0.1 to 0.5 parts by weight, and the perfume may be used in an amount of 0.01 to 1 part by weight, preferably 0.01 to 0.05 parts by weight, based on 100 parts by weight of the first vinyl silicone oil.
The total amount ratio of the base component and the catalyst component of the present invention may be calculated based on the amount of Pt, and generally, the total amount ratio of the base component and the catalyst component may be 1: 0.5-2, preferably 1: 0.8-1.2.
The second aspect of the present invention provides an in-situ polymerized film, wherein the in-situ polymerized film is prepared by applying the matrix component and the catalyst component of the present invention to the surface of an object in sequence or after mixing, and waiting for at least 30 seconds, preferably for 150 seconds and 300 seconds.
Since the matrix component and the catalyst component react upon contact, if a post-mixing coating is selected, the coating should be carried out within 120 seconds (preferably within 30 seconds) after mixing.
In the present invention, the thickness of the in-situ polymerized film is not particularly limited, and is determined according to the application requirements. When applied to the skin, the composition used to form the in situ polymerized film is used in an amount that is about the same as the amount of a normal facial cream that is applied, and the resulting in situ polymerized film typically has a thickness of 20 to 120 microns, preferably 40 to 80 microns.
The in-situ polymerized film is a dense cross-linked reticular film, so that dust, PM2.5 particles, particulate matters which can participate in photochemical reaction in the air and bacterial viruses in the air can be isolated.
In a third aspect, the present invention provides the composition for forming an in situ polymerized film and/or the use of an in situ polymerized film of the present invention on a skin surface. When the composition for forming the in-situ polymerized film and/or the in-situ polymerized film is applied to skin, the invisible skin film with the similar property to the skin can be formed on the surface of the skin, and can be tightly attached to the surface of the skin, so that the skin with the original wrinkles relaxed is stretched and spread, the relaxation and wrinkles are effectively smoothed, and the skin looks firmer and smoother. When the invisible skin film contains functional materials with specific functions, different additional functions can be realized, such as sun protection, concealer, bacteriostasis, and even the use in the treatment of skin diseases, scalds and the like can be realized by adding or not adding medicaments. The invisible skin film has water resistance, can be removed from the skin by a peeling method, usually the edge of the film slightly turns up after being used for 16 hours, and can be easily torn off along the edge in a whole piece.
The present invention will be described in detail below by way of examples. The raw materials used in the following examples and comparative examples were purchased from the institute for field chemical industry additives.
Example 1
(1) Separately prepared were a base component and a catalyst component, which were separately stored, wherein,
a. the following ingredients were mixed and stirred in a stirring kettle for 3.1 hours to obtain a base component (denoted as a 1):
100 parts by weight of monovinyl-terminated polydimethylsiloxane (viscosity 5500mpa.s, vinyl content 1.7 mol%);
hydrogen-containing silicone oil (viscosity 10mpa.s, hydrogen content 0.21 wt%), 13.75 parts by weight.
b. The following ingredients were mixed and stirred in a stirred tank for 2.1 hours to obtain a catalyst component (noted as B1):
103 parts by weight of monovinyl-terminated polydimethylsiloxane (viscosity 10000mPa. S, vinyl content 1.7%);
high-viscosity vinyl MQ resin (content of siloxane chain segments having monofunctional degree of 8 mol%, content of siloxane polycondensation chain segments having tetrafunctional degree of 20 mol%, viscosity of 57000mpa.s), 8.75 parts by weight;
tetramethyltetravinylcyclotetrasiloxane-platinum complex (Pt content 0.2% by weight (corresponding to 0.004 parts by weight)), 2.0 parts by weight.
(2) Taking the matrix component and the catalyst component according to the weight ratio of 1: 1 by weight and immediately applied to the facial skin surface, and waited for 240 seconds to form a stealth skin film, designated C1, having a thickness of about 80 μm.
It was observed that the invisible thin film on the skin surface could not be visually distinguished, the original sagging and wrinkles of the skin were effectively smoothed, and the wrinkle degree (roughness) of the skin surface was reduced by about 790 times as observed by optical coherence tomography (instrument SD-OCT Systems, manufacturer Telesto, designation TEL1300V2-BU, hereinafter the same). The skin has no foreign body sensation. After 16 hours the film was peeled off in one piece without pain.
Example 2
(1) Separately prepared were a base component and a catalyst component, which were separately stored, wherein,
a. the following ingredients were mixed and stirred in a stirring kettle for 3.5 hours to obtain a base component (denoted as a 2):
100 parts by weight of trivinyl-terminated polydimethylsiloxane (viscosity 2000mpa.s, vinyl content 3.7 mol%);
12 parts by weight of hydrogen-containing silicone oil (viscosity of 50mPa.S, hydrogen content of 0.21% by weight);
0.005 part by weight of ethynl cyclohexanol;
silica (average particle diameter 20 nm), 21.3 parts by weight.
b. The following ingredients were mixed and stirred in a stirred tank for 2.5 hours to obtain a catalyst component (noted as B2):
trivinyl-terminated polydimethylsiloxane (viscosity 2000mpa.s, vinyl content 1.7%), 122.6 parts by weight;
vinyl MQ resin (content of siloxane chain segments having monofunctional degree of 2 mol%, content of siloxane polycondensation chain segments having tetrafunctional degree of 5 mol%, viscosity of 7000mpa.s), 10.5 parts by weight;
tetramethyltetravinylcyclotetrasiloxane-platinum complex (Pt content 1.7% (corresponding to 0.04 parts by weight)), 2.3 parts by weight.
(2) Taking the matrix component and the catalyst component according to the weight ratio of 1: 1 by weight and immediately applied to the facial skin surface, and waited for 170 seconds to form a stealth skin film, designated C2, having a thickness of about 40 μm.
The observation shows that the invisible film on the skin surface can not be distinguished by naked eyes, the original looseness and wrinkles of the skin are effectively smoothed, and the wrinkle degree of the skin surface is reduced by about 820 times through the observation of optical coherence tomography. The skin has no foreign body sensation. After 16 hours the film was peeled off in one piece without pain.
Example 3
(1) Separately prepared were a base component and a catalyst component, which were separately stored, wherein,
a. the following ingredients were mixed and stirred in a stirring kettle for 4 hours to obtain a base component (denoted as a 3):
monovinyl-terminated polydimethylsiloxane and divinyl-terminated polydimethylsiloxane were prepared in a 1: 1 (viscosity 7000mpa.s, vinyl content 4 mol%), 100 parts by weight;
22 parts by weight of hydrogen-containing silicone oil (viscosity of 5mPa.S, hydrogen content of 0.30% by weight);
12.5 parts by weight of titanium dioxide (particle size ranging from 0.02 to 2 microns);
9 parts by weight of silica (average particle diameter of 10 nm);
zinc dioxide (average particle diameter 20 nm), 12.5 parts by weight.
b. The following ingredients were mixed and stirred in a stirred tank for 3 hours to obtain a catalyst component (noted as B3):
divinyl-terminated polydimethylsiloxane and monovinyl-terminated polydimethylsiloxane were prepared in a 1: 1 weight part of a mixed mixture (viscosity: 10000mpa.s, vinyl content: 1.7%), 113.2 weight parts;
vinyl MQ resin (content of siloxane chain segments having monofunctional degree of 8 mol%, content of siloxane polycondensation chain segments having tetrafunctional degree of 20 mol%, viscosity of 57000mpa.s), 8.0 parts by weight;
isopropyl alcohol-platinum complex (Pt content 0.8% (corresponding to 0.03 parts by weight)), 3.8 parts by weight.
(2) Taking the matrix component and the catalyst component in a ratio of 1.2: 1 by weight and immediately applied to the facial skin surface, and waited for 170 seconds to form a stealth skin film, designated C3, having a thickness of about 60 μm.
The observation shows that the invisible film on the surface of the skin can not be distinguished by naked eyes, the original looseness and wrinkles of the skin are effectively smoothed, and the wrinkle degree of the surface of the skin is reduced by about 808 times through the observation of optical coherence tomography. The skin has no foreign body sensation. After 16 hours the film was peeled off in one piece without pain.
Example 4
(1) Separately prepared were a base component and a catalyst component, which were separately stored, wherein,
a. the following ingredients were mixed and stirred in a stirring kettle for 4.5 hours to obtain a base component (denoted as a 4):
100 parts by weight of monovinyl-terminated polydimethylsiloxane (viscosity 7000mpa.s, vinyl content 1.7 mol%);
hydrogen-containing silicone oil (viscosity 50mpa.s, hydrogen content 0.10 wt%), 13.75 parts by weight;
silica (average particle diameter 5 nm), 8.75 parts by weight;
0.008 parts by weight of methylbutynol;
0.0875 part by weight of nitrofurazone;
benzalkonium chloride, 0.0875 weight portions;
dexamethasone acetate, 0.0875 weight portion.
b. The following ingredients were mixed and stirred in a stirred tank for 2 hours to obtain a catalyst component (noted as B4):
130 parts by weight of trivinyl-terminated polydimethylsiloxane (viscosity 10000mPa. S, vinyl content 1.7%);
vinyl MQ resin (content of siloxane chain segments having monofunctional degree of 8 mol%, content of siloxane polycondensation chain segments having tetrafunctional degree of 20 mol%, viscosity of 57000mpa.s), 9.7 parts by weight;
2.2 parts by weight of a2, 4, 6-trivinyl-2, 4, 6-trimethylcyclotrisiloxane platinum complex (Pt content 1.7% by weight, corresponding to 0.037 parts by weight).
(2) Taking the matrix component and the catalyst component according to the weight ratio of 1: 1 by weight and immediately applied to the facial skin surface, and waited for 170 seconds to form a stealth skin film, designated C4, having a thickness of about 60 μm.
The observation shows that the invisible film on the skin surface can not be distinguished by naked eyes, the original looseness and wrinkles of the skin are effectively smoothed, and the wrinkle degree of the skin surface is reduced by about 810 times through the observation of optical coherence tomography. The skin has no foreign body sensation. After 16 hours the film was peeled off in one piece without pain.
Example 5
(1) Separately prepared were a base component and a catalyst component, which were separately stored, wherein,
a. the following ingredients were mixed and stirred in a stirring kettle for 3.1 hours to obtain a base component (denoted as a 5):
monovinyl-terminated polymethylvinylsiloxane (viscosity of 7000mpa.s, vinyl content 1.7 mol%), 100 parts by weight;
hydrogen-containing silicone oil (viscosity 50mpa.s, hydrogen content 0.21 wt%), 13.75 parts by weight;
silica (average particle diameter 20 nm), 8.75 parts by weight;
0.004 weight portion of ethyne cyclohexanol;
0.625 parts of talcum powder;
0.125 weight portion of calcium carbonate;
magnesium carbonate, 0.125 weight part;
3.75 parts by weight of a pigment for cosmetic foundation;
0.125 weight portion of antioxidant;
0.125 weight portion of spice.
b. The following ingredients were mixed and stirred in a stirred tank for 2.1 hours to obtain a catalyst component (noted as B5):
monovinyl-terminated polymethylvinylsiloxane and monovinyl-terminated polydimethylsiloxane were polymerized in a ratio of 5: 95% by weight of a mixed mixture (viscosity: 10000mPa. S, vinyl content: 1.7%), 117.25 parts by weight;
11 parts by weight of a vinyl MQ resin (content of siloxane chain segments having monofunctional degree of 8 mol%, content of siloxane polycondensation chain segments having tetrafunctional degree of 20 mol%, viscosity of 57000 mpa.s);
chloroplatinic acid powder (Pt content 1.7 wt% (corresponding to 0.02 wt)) 1.25 wt.
(2) Taking the matrix component and the catalyst component according to the weight ratio of 1: 1 by weight and immediately applied to the facial skin surface, and waited for 170 seconds to form a stealth skin film, designated C5, having a thickness of about 60 μm.
The observation shows that the invisible film on the surface of the skin can not be distinguished by naked eyes, the original looseness and wrinkles of the skin are effectively smoothed, and the wrinkle degree of the surface of the skin is reduced by about 800 times through the observation of optical coherence tomography. The invisible skin film effectively covers the pigment deposition such as scars and scars on the surface of the skin, and keeps the skin free of makeup removal and color change for 24 hours. The skin has no foreign body sensation. After 24 hours the film was peeled off in one piece without pain.
Example 6
The procedure was followed as in example 2 except that the catalyst component contained only a platinum catalyst (the same as that of example 2) and the catalyst component and the base component were other than 1: 1, 135.4 parts by weight of a2 was used in admixture with 2.3 parts by weight of a platinum catalyst.
It was observed that a stealth skin film was formed after waiting 20 minutes, and the film remained in a highly viscous state after 8 hours.
Example 7
The procedure was followed as in example 2 except that the vinyl MQ silicone resin was not included in the catalyst component.
It was observed that a stealth skin film was formed after waiting 40 minutes, and the film remained in a high viscosity state after 4 hours.
Comparative example 1
The procedure is as in example 2 except that the base component A2 does not contain hydrogen-containing silicone oil.
It was observed that the film could not be formed after waiting for 60 minutes.
Comparative example 2
After emulsification, the commercial manufacturer of Dow Corning, a commercial product with the brand number DC-1107 was tested for storage at 0 ℃ and found that significant oil-water separation occurred after 1 month of storage.
Test example
(1) Weather resistance test
The matrix component and the catalyst component obtained in examples 1 to 7 and comparative example 2 were stored in the same plural portions at-30 deg.C, -10 deg.C, 0 deg.C, 25 deg.C and 50 deg.C for 6 months, respectively, and no delamination was observed, and the matrix component activity and the catalyst component activity were measured and shown in Table 1.
The method for testing the activity of the matrix component comprises the following steps: mixing the fresh matrix components and the fresh catalyst components obtained in the examples 1-7 and the comparative example 2, respectively carrying out a film forming experiment, testing the elastic modulus of the obtained film, and recording; then respectively mixing the matrix component stored for 6 months with the fresh catalyst components of respective examples or comparative examples, respectively carrying out a film forming experiment, testing the elastic modulus of the obtained film, and comparing the elastic modulus with the elastic modulus of the fresh agent recorded before to obtain the matrix component activity (%);
the method for testing the activity of the catalyst component comprises the following steps: referring to the testing method of the activity of the matrix component, except that the catalyst component stored for 6 months was mixed with the fresh matrix component of each example or comparative example, respectively, and then a film forming experiment was performed and the elastic modulus of the obtained film was tested, and the elastic modulus was compared with the elastic modulus of the fresh agent recorded before, i.e., the activity (%) of the catalyst component;
wherein the process of the film forming experiment comprises the following steps: mixing a matrix component and a catalyst component in a ratio of 1: 1, mixing the weight ratio of the components, injecting a proper amount of the mixture into a test grinding tool (60 mm wide and 120 mm long), crosslinking for 12 hours at room temperature, removing the grinding tool to obtain a polymer sample with the thickness of about 4 mm, respectively measuring a stress-strain curve of the obtained in-situ polymerized film at room temperature under the condition of precisely controlled 30 loads and load removal circulation (100% stress deformation) by using a full-intelligent computer-controlled electronic universal material testing machine (manufacturer Shimadzu, brand AG-Xplus Series), analyzing the stress-strain curve to obtain the elastic modulus (MPa), and repeatedly testing the data under each condition for 300 times in the test to obtain an average value.
TABLE 1
As can be seen from table 1, the activities of the matrix component and the catalyst component of the examples were maintained at 99.00% or more after 6 months of storage at different temperatures, while the activity of the emulsion of comparative example 2 was reduced to 10% or less under low temperature conditions, and it was observed that the delamination phenomenon occurred. In addition, since the matrix component and the catalyst component of comparative example 1 could not react to obtain an in-situ polymerized film, the activity test was not performed on the matrix component and the catalyst component of comparative example 1.
(2) Barrier function testing
The invisible skin film C2 obtained in example 2 was peeled off and placed on a sample stage for scanning electron microscope observation, and the surface of the obtained invisible skin film was found to be dense and to have few pores. Therefore, general dust, PM2.5 particles, particulate matters which can participate in photochemical reaction in the air, bacteria and viruses in the air and the like are blocked outside the invisible skin, and cannot penetrate through the invisible skin to influence the natural skin, so that an effective barrier with the function of protecting the skin can be formed.
Further, in order to demonstrate the barrier function of the invisible skin, the base component and the catalyst component of example 1 were uniformly blended and applied on the surface of hand skin for 240 seconds to form an invisible skin film having a thickness of about 80 μm, and then the hand was placed in an environment having a high concentration of dust, suspended nanoparticles (about 250 nm), and after 8 hours, the invisible skin was peeled off from the hand. The invisible film is arranged on the outer side of the environment and close to the inner side surface of the natural skin in the particle polluted environment through the observation of a scanning electron microscope, so that partial particles are adsorbed to the outer layer of the film, but no particles penetrate through the film to enter the inner side surface close to the natural skin, and the particulate matter blocking rate reaches over 99.99 percent. Therefore, the invisible skin has excellent barrier function and can be used as an effective protective barrier for daily skin protection, skin replacement of patients with allergy and skin dysfunction and special work (such as nanoparticles, bacteria and virus contacts).
(3) Mechanical Properties and anti-wrinkle function
As a film material suitable for the skin surface, the mechanical property of the film material is similar to the natural skin of a human body so as to realize comfortable feeling in use. By regulating and controlling the weight percentage of the hydrogen-containing silicone oil in the comfortable oil, the accurate series of invisible skin films with different viscosities, softness, tensile strengths and moduli can be provided. A series of base components (the foregoing contents correspond to nos. X1 to X6) having different hydrogen-containing silicone oil contents (contents of 1 part by weight, 7 parts by weight, 13 parts by weight, 20 parts by weight, 27 parts by weight and 36 parts by weight, respectively) were prepared in accordance with the method of example 2, in the same manner as the catalyst component B2 of example 2 in a ratio of 1: 1, mixing the weight ratio of the components, injecting a proper amount of the mixture into a test grinding tool (60 mm wide and 120 mm long), crosslinking for 12 hours at room temperature, removing the grinding tool to obtain a polymer sample with the thickness of about 4 mm, respectively measuring a stress-strain curve of the obtained in-situ polymerized film at room temperature under the condition of precisely controlled 30 loads and load shedding circulation (100% stress deformation) by using a full-intelligent computer-controlled electronic universal material testing machine (manufacturer Shimadzu, brand AG-XplusSeries), and analyzing the stress-strain curve to obtain the elastic modulus (MPa) and the elongation at break (%), which are shown in Table 1. The data for each condition in the test were passed through the test repeated 300 times and the average was taken.
TABLE 2
| The content of the silicon-hydrogen-containing oil in the matrix component (parts by weight) | 1 | 7 | 13 | 20 | 27 | 36 |
| Modulus of elasticity (MPa) | 7.17 | 5.90 | 3.45 | 2.07 | 0.44 | 0.01 |
| Elongation at Break (%) | 398 | 341 | 282 | 40 | 35 | 20 |
As can be seen from Table 2, the elastic modulus and the elongation at break of the in-situ polymerized film can be adjusted within a relatively large range by controlling the content of the silicone oil in the matrix component, and the mechanical properties of the skin of a human body are usually 0.01-8.0MPa of elastic modulus and 20-360% of elongation at break, so that the mechanical parameters of the in-situ polymerized film can be effectively adjusted and controlled to have mechanical properties similar to those of the skin of the human body.
(4) Ultraviolet resistance test and sun-screening function
This test example was conducted with respect to the composition for forming an in-situ polymerized film and the in-situ polymerized film of example 3.
The specific test method comprises the following steps: the matrix component A3 and the catalyst component B3 were uniformly blended and coated on the surface of 0.1 mm thick glass, and in-situ crosslinked to form an in-situ polymerized film with a thickness of about 60 μm, an ultraviolet lamp was placed on one side of the film, and a photodetector was placed on the other side of the film, so as to test the shielding rate of the in-situ polymerized film to ultraviolet rays with different wavelengths (UVB: wavelength 290-. Further, the in-situ polymerized film was examined for changes in the ultraviolet ray shielding rate (average of UVB and UVA) under long-term irradiation, and it was found that the ultraviolet ray shielding rate was 99.25%, 98.5%, 99.3%, 96.8%, 97.8%, 97.9%, 98.5%, 99.3% and 99.35% in the order of 0, 1, 2 … … 6, 7 and 8 hours, and it was found that the in-situ polymerized film was substantially stable for 8 hours and was able to maintain 95% or more in the order of the ultraviolet ray shielding rate, and the ultraviolet ray shielding rate was 83%, 78%, 64% and 60% in the order of 9, 10, 11 and 12 hours, and gradually decreased. Therefore, the in-situ polymerized film has excellent ultraviolet absorption function and can be used as an excellent sun-proof skin care material.
In addition, the matrix component A3 and the catalyst component B3 are uniformly blended and injected into a testing grinding tool (25 mm wide and 160 mm long), crosslinked for 12 hours at room temperature, and removed from the grinding tool, after the prepared sample is radiated by an ultraviolet lamp (with the wavelength of 200-400 nm) for 3600 hours, the elastic modulus and the elongation at break of the sample are tested (the elastic modulus and the strain at break of the sample are analyzed according to a stress-strain curve measured under the full load condition), and the change range of the elastic modulus of the sample before and after radiation is found to be within 1 percent, and the change range of the elongation at break is found to be within 0.5 percent. Therefore, the invisible skin still maintains lasting excellent mechanical properties under the condition of long-term ultraviolet radiation, and the characteristic provides necessary conditions for preparing the invisible skin with the sun-screening function.
(5) Test of antibacterial Property
This test example was conducted with respect to the composition for forming an in-situ polymerized film and the in-situ polymerized film of example 4.
The specific test method comprises the following steps: the substrate component A3 and the catalyst component B3 are uniformly blended and coated on the surface of 0.1 mm thick glass, and are crosslinked in situ to form an in-situ polymerized film with the thickness of about 60 microns, or are uniformly coated on hands, and are crosslinked to form invisible skin with the thickness of about 60 microns, and the bacteriostatic effect of the in-situ polymerized film or the invisible skin is tested by testing the microbial inhibition rate (the number of residual colonies or the bacterial survival rate is tested after 6 hours of coating the microbes). Experiments show that the in-situ polymerized film has excellent antibacterial and antiviral capacity for different strains or viruses, the inhibition rate of the in-situ polymerized film exceeds 99.9%, specifically, the inhibition rate of the in-situ polymerized film on escherichia coli is 99.98%, the inhibition rate on staphylococcus aureus is 99.95%, the inhibition rate on gonococcus is 99.97%, the inhibition rate on candida albicans is 99.90%, the inhibition rate on SAPS coronavirus is 99.98%, and the inhibition rate of invisible skin on natural bacteria is 99.99%.
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention. It should be noted that the various technical features described in the above embodiments can be combined in any suitable manner without contradiction, and the invention is not described in any way for the possible combinations in order to avoid unnecessary repetition. In addition, any combination of the various embodiments of the present invention is also possible, and the same should be considered as the disclosure of the present invention as long as it does not depart from the spirit of the present invention.
Claims (31)
1. A composition for forming an in-situ polymerized film, comprising a base component and a catalyst component, wherein the base component comprises a first vinyl silicone oil and a hydrogen-containing silicone oil, wherein the hydrogen-containing silicone oil is present in an amount of 1 to 40 parts by weight based on 100 parts by weight of the first vinyl silicone oil; the catalyst component contains Pt; the catalyst component is used in an amount of 0.001 to 0.1 parts by weight based on the weight of Pt therein with respect to 100 parts by weight of the first vinyl silicone oil, and the base component further contains a functional material;
the catalyst component further contains a vinyl MQ silicone resin in an amount of 2 to 25 parts by weight, the vinyl MQ silicone resin being a silicone resin composed of monofunctional siloxane chain segments and tetrafunctional siloxane condensed chain segments, the content of the monofunctional siloxane chain segments in the vinyl MQ silicone resin being 2 to 8 mol%, and the content of the tetrafunctional siloxane condensed chain segments being 5 to 20 mol%, relative to 100 parts by weight of the first vinyl silicone oil.
2. The composition for forming an in-situ polymerized thin film according to claim 1, wherein the base component and the catalyst component are each independently preserved.
3. The composition for forming an in-situ polymerized film according to claim 1, wherein the hydrogen-containing silicone oil is contained in an amount of 5 to 30 parts by weight based on 100 parts by weight of the first vinyl silicone oil.
4. The composition for forming an in-situ polymerized film according to claim 1, wherein the hydrogen-containing silicone oil is contained in an amount of 12 to 22 parts by weight based on 100 parts by weight of the first vinyl silicone oil.
5. The composition for forming an in-situ polymerized film according to claim 1, wherein the viscosity of the first vinyl silicone oil is 2000-30000 mPa-s, and the content of vinyl groups is 0.1-7.5 mol%.
6. The composition for forming an in-situ polymerized film according to claim 5, wherein the first vinyl silicone oil has a viscosity of 2000-15000 mPa-s, in which the vinyl content is 0.1-5 mol%.
7. The composition for forming an in situ polymerized film according to any one of claims 1, 5 or 6 wherein the first vinyl silicone oil is selected from one or more of monovinyl terminated polymethylvinylsiloxane, polyvinyl terminated polymethylvinylsiloxane, monovinyl terminated polydimethylsiloxane and polyvinyl terminated polydimethylsiloxane.
8. The composition for forming an in situ polymerized film according to claim 7, wherein the first vinyl silicone oil is selected from mono-vinyl terminated polydimethylsiloxanes and/or poly-vinyl terminated polydimethylsiloxanes.
9. The composition for forming an in-situ polymerized film according to any one of claims 1 to 4, wherein the hydrogen-containing silicone oil has a viscosity of 5 to 7000 mPa-s and a hydrogen content of 0.01 to 1.5% by weight.
10. The composition for forming an in-situ polymerized film according to claim 9, wherein the hydrogen-containing silicone oil has a viscosity of 500-1500 mPa-s and a hydrogen content of 0.1-0.8 wt.%.
11. The composition for forming an in-situ polymerized film according to any one of claims 1 to 4, wherein the base component further comprises a thixotropic material in an amount of 1 to 30 parts by weight based on 100 parts by weight of the first vinyl silicone oil.
12. The composition for forming an in-situ polymerized film according to claim 11, wherein the thixotropic material is contained in an amount of 5 to 25 parts by weight based on 100 parts by weight of the first vinyl silicone oil.
13. The composition for forming an in situ polymerized film according to claim 11, wherein the thixotropic material is selected from one or more of silica, zinc oxide and titanium dioxide.
14. The composition for forming an in situ polymerized film according to claim 12, wherein the thixotropic material is selected from one or more of silica, zinc oxide and titanium dioxide.
15. The composition for forming an in situ polymerized film according to claim 13 or 14 wherein the thixotropic material has an average particle size of 5 to 50 nanometers.
16. The composition for forming an in situ polymerized film according to claim 15, wherein the thixotropic material has an average particle size of 5 to 25 nanometers.
17. The composition for forming an in-situ polymerized film according to any one of claims 1 to 4, wherein the matrix component further comprises a stabilizer.
18. The composition for forming an in-situ polymerized film according to claim 17, wherein the stabilizer is selected from one or more of ethynl cyclohexanol, methyl butynol, and silicone-modified alkynol, and is contained in an amount of 0.001 to 5 parts by weight based on 100 parts by weight of the first vinyl silicone oil.
19. The composition for forming an in-situ polymerized film according to claim 18, wherein the stabilizer is contained in an amount of 0.001 to 0.1 parts by weight based on 100 parts by weight of the first vinyl silicone oil.
20. The composition for forming an in-situ polymerized film according to claim 1, wherein the functional material is selected from one or more of an anti-ultraviolet functional material, a medicinal functional material and a concealer functional material, the anti-ultraviolet functional material is contained in an amount of 1 to 30 parts by weight, the medicinal functional material is contained in an amount of 0.01 to 1 part by weight, and the concealer functional material is contained in an amount of 0.1 to 2 parts by weight, based on 100 parts by weight of the first vinyl silicone oil.
21. The composition for forming an in-situ polymerized thin film according to claim 1, wherein the catalyst component is used in an amount of 0.002 to 0.05 parts by weight based on the weight of Pt therein, with respect to 100 parts by weight of the first vinyl silicone oil.
22. The composition for forming an in-situ polymerized thin film according to claim 21, wherein the Pt is present in the form of a platinum catalyst in which the content of Pt is 0.05 to 20 wt%.
23. The composition for forming an in-situ polymerized thin film according to claim 22, wherein the Pt is present in the form of a platinum catalyst in which the content of Pt is 0.2 to 5 wt%.
24. The composition for forming an in-situ polymerized thin film according to claim 22 or 23, wherein the platinum catalyst is selected from one or more of chloroplatinic acid, platinum nanoparticles and organic-platinum complexes.
25. The composition for forming an in-situ polymerized film according to any one of claims 1 and 21 to 23, wherein the catalyst component further comprises a second vinyl silicone oil in an amount of 80 to 160 parts by weight with respect to 100 parts by weight of the first vinyl silicone oil.
26. The composition for forming an in-situ polymerized film according to claim 25, wherein the second vinyl silicone oil is the same as or different from the first vinyl silicone oil, and has a viscosity of 1000-50000 mPa-s, wherein the vinyl content is 0.1-2.5 wt%.
27. The composition for forming an in-situ polymerized film according to claim 26, wherein the second vinyl silicone oil has a viscosity of 2000-10000 mPa-s, and a vinyl content of 1-2 wt%.
28. The composition for forming an in situ polymerized film according to claim 1, wherein the vinyl MQ silicone resin has a viscosity of 2000-100000 mPa-s.
29. The composition for forming an in situ polymerized film according to claim 28, wherein the vinyl MQ silicone resin has a viscosity of 7000-57000 mPa-s.
30. An in situ polymerized film prepared by applying the matrix component and the catalyst component of the composition of any of claims 1-29 to the surface of an object sequentially or after mixing, and waiting at least 30 seconds.
31. Use of a composition for forming an in situ polymerized film according to any of claims 1 to 29 and/or a film according to claim 30 in the manufacture of a product for application to the surface of the skin.
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| CN105586782A (en) * | 2016-03-07 | 2016-05-18 | 惠州赛力珑新材料有限公司 | Printed organic silicone synthetic leather and preparation method thereof |
| CN105729929A (en) * | 2016-03-03 | 2016-07-06 | 惠州赛力珑新材料有限公司 | Silica gel TPU composite material and preparation method |
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| CN105729929A (en) * | 2016-03-03 | 2016-07-06 | 惠州赛力珑新材料有限公司 | Silica gel TPU composite material and preparation method |
| CN105586782A (en) * | 2016-03-07 | 2016-05-18 | 惠州赛力珑新材料有限公司 | Printed organic silicone synthetic leather and preparation method thereof |
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