CN107503231B - Application of vinyl silicone oil with hydroxyl at tail end as release force regulator in preparation of release agent, release agent and release film - Google Patents
Application of vinyl silicone oil with hydroxyl at tail end as release force regulator in preparation of release agent, release agent and release film Download PDFInfo
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- CN107503231B CN107503231B CN201710736953.8A CN201710736953A CN107503231B CN 107503231 B CN107503231 B CN 107503231B CN 201710736953 A CN201710736953 A CN 201710736953A CN 107503231 B CN107503231 B CN 107503231B
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H19/00—Coated paper; Coating material
- D21H19/10—Coatings without pigments
- D21H19/14—Coatings without pigments applied in a form other than the aqueous solution defined in group D21H19/12
- D21H19/24—Coatings without pigments applied in a form other than the aqueous solution defined in group D21H19/12 comprising macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D21H19/32—Coatings without pigments applied in a form other than the aqueous solution defined in group D21H19/12 comprising macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds obtained by reactions forming a linkage containing silicon in the main chain of the macromolecule
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H19/00—Coated paper; Coating material
- D21H19/10—Coatings without pigments
- D21H19/14—Coatings without pigments applied in a form other than the aqueous solution defined in group D21H19/12
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
- D21H21/14—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties characterised by function or properties in or on the paper
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2400/00—Presence of inorganic and organic materials
- C09J2400/20—Presence of organic materials
- C09J2400/28—Presence of paper
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Adhesive Tapes (AREA)
- Paints Or Removers (AREA)
- Laminated Bodies (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Medicinal Preparation (AREA)
Abstract
The invention belongs to the technical field of release force regulators, and discloses application of vinyl silicone oil with hydroxyl at the tail end as a release force regulator in preparation of a release agent, the release agent and a release film, in particular application in preparation of an addition type organic silicon release agent. The invention discloses an application of vinyl silicone oil with hydroxyl at the tail end as a release force regulator in the preparation of a release agent, wherein the structural formula of the vinyl silicone oil with hydroxyl at the tail end is as follows:
Description
Technical Field
The invention belongs to the technical field of release force regulators, and particularly relates to application of vinyl silicone oil with hydroxyl at the tail end as a release force regulator in preparation of a release agent, the release agent and a release film, in particular to application in preparation of an addition type organic silicon release agent.
Background
The addition type organosilicon release agent is a substance which is obtained by the addition reaction of vinyl-containing organopolysiloxane and organopolysiloxane containing Si-H bond under the catalysis of a transition metal compound of the eighth group (such as Pt, Ni) and the like, can reduce or eliminate the adhesion effect existing on the surface and separate two surfaces which are difficult to separate or cannot be separated, and has wide application and important position in organosilicon chemistry. Can be widely applied to the industries of pressure-sensitive adhesive tapes, self-adhesive labels, medical and sanitary products, food release agent cooking paper, printing, decoration and the like. The organosilicon release agent can be coated on the surface of various substrates (such as release paper, glassine paper, crepe paper, kraft paper, white board paper, coated paper, PET (polyethylene terephthalate) film, OPP (oriented polypropylene) film, PE (polyethylene) film, sanitary back materials and the like) to form a non-migratory low-surface-energy coating, so that the surface of the substrate is endowed with non-sticking performance, slight stickiness or a certain degree of stickiness, and the degree of stickiness can be measured by light peeling force, medium peeling force, heavy peeling force and overweight peeling force. The general release force is 0.10N/25mm, namely the release force below 10 g, which is called light peeling; a peel force of 0.20N/25mm, i.e., 20 g or less, is called medium peel, and a peel force of 0.35 to 0.45N/25mm, i.e., 35 to 45 g, is called heavy peel; 0.60-0.80N/25 mm, namely 60-80 g of stripping force, commonly called heavy stripping; there is also a peel force of 1.00N/25mm, i.e., above 100 grams, referred to as extra heavy peel.
The above-mentioned peel force is the force required to peel the tesa7475 tape from the release agent coated substrate at a peel speed of 300mm/min at an angle of 180 degrees, and the magnitude of the peel force is controlled depending on many factors: such as crosslinking density (ratio of Si-H/Si-Vi), adhesion work, coating amount, MQ resin content and the like, although release paper/films with different release forces can be obtained by changing or adjusting the influencing factors, the prepared release paper/film has some problems such as unstable release force, large addition amount, high cost, uneven dispersion and the like.
Patent 20141033222495.X made a release force of type 7200 of dow corning company as follows: 3-5 g of release film with light release force. The release force regulator can only be used for preparing films with light release force. Patent 201210275191.3 discloses a method for preparing an overweight release film, which uses a vinyl MQ silicone resin with double bonds to enhance the release force, and the additive accounts for a larger proportion of the total mass.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention mainly aims to provide the application of vinyl silicone oil with hydroxyl at the terminal as a release force regulator in the preparation of the release agent, in particular to the application of vinyl polydimethylsiloxane with hydroxyl at the terminal as a release force regulator in the preparation of the release agent, and particularly the application in the preparation of addition type organic silicon release agent. The vinyl silicone oil with hydroxyl at the tail end of the invention is used as a regulator and has bifunctional groups: hydroxyl and vinyl play a dual role when being applied to the release agent, the hydroxyl enhances the firmness of combination with the base material, simultaneously, the surface tension of the material is improved due to the introduction of the hydroxyl, and the vinyl participates in the hydrosilylation reaction to enhance the compatibility with the release agent.
The invention also aims to provide a release agent.
The invention further aims to provide a release film based on the release agent.
The purpose of the invention is realized by the following scheme:
the vinyl silicone oil with the hydroxyl at the tail end is used as a release force regulator to be applied to the preparation of a release agent, and the structural formula of the vinyl silicone oil with the hydroxyl at the tail end is shown as follows:
wherein n and m represent a repeating structural unit, and n is preferably 1 to 10, and m is preferably 0 to 6.
The hydroxyl-containing vinyl silicone oil at the tail end has the hydroxyl content as follows: 3-13%, and the vinyl content is: 2-10%.
The viscosity range of the vinyl silicone oil containing hydroxyl at the tail end is preferably 30-100 cps.
The vinyl silicone oil containing hydroxyl at the tail end can be vinyl polydimethylsiloxane containing hydroxyl at the tail end.
The invention also provides a release agent, which comprises the following components in parts by mass: 60-100 parts of a main agent; 3-25 parts of a crosslinking agent; 0.1-0.5 part of inhibitor; 1-30 parts of vinyl silicone oil with a hydroxyl group at the tail end; 5-10 parts of a catalyst.
The structural formula of the vinyl silicone oil containing hydroxyl at the tail end is as follows:
wherein n and m represent a repeating structural unit, and n is preferably 1 to 10, and m is preferably 0 to 6.
The main agent is preferably vinyl silicone oil.
The viscosity range of the vinyl silicone oil is preferably 100-350 cps.
The cross-linking agent is the cross-linking agent which is conventionally used in the field, and hydrogen-containing silicone oil is preferred.
The viscosity of the cross-linking agent is preferably in the range of 50 to 200 cps.
The inhibitor is an inhibitor conventionally used in the art, and is preferably at least one of methylbutynol, ethynylcyclohexanol, 2-phenyl-3-butyn-ethanol, 3-methyl-1-penten-4-yn-3-ol, and 3- (trimethylsilyl) propynol.
The catalyst is any catalyst conventionally used in the art, and is preferably platinum.
The viscosity range of the catalyst is preferably 100 to 300 cps.
The release agent is obtained by uniformly stirring and mixing the components, and preferably stirring and mixing for 20-30 min.
The invention also provides a release film based on the release agent, which is specifically obtained by coating the release agent on a substrate, drying and rolling.
The substrate is conventional in the art, and may be, but not limited to, release paper, glassine paper, textured paper, kraft paper, white board paper, coated paper, PET film, OPP film, PE film, sanitary back material, and the like.
The thickness of the coating is preferably 0.6-1.2 g/m2. The curing time of the coating is preferably 2-20 s.
The drying temperature is 120-200 ℃.
The vinyl silicone oil with hydroxyl at the tail end of the invention is used as a regulator and has bifunctional groups: hydroxyl and vinyl play a dual role when being applied to the release agent, the hydroxyl enhances the firmness of combination with the base material, simultaneously, the surface tension of the material is improved due to the introduction of the hydroxyl, and the vinyl participates in the hydrosilylation reaction to enhance the compatibility with the release agent.
The vinyl silicone oil with the hydroxyl at the tail end is used as a release force regulator to be applied to the preparation of the release agent, so that the release film is obtained, the release films with different release forces can be obtained by regulating the content of the added vinyl silicone oil with the hydroxyl at the tail end, and the higher the content of the vinyl silicone oil with the hydroxyl at the tail end is, the larger the release force of the obtained release film is.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto. The materials referred to in the following examples are commercially available.
Example (b): preparation of release film
The vinyl silicone oil containing hydroxyl at the tail end has the structural formula as follows:
wherein n is 1-10, and m is 0-6.
Base material: glassine paper.
The release agent comprises the following components: the main agent is vinyl silicone oil with the viscosity of 180 cps; the cross-linking agent is hydrogen-containing silicone oil with the viscosity of 100cps, and the terminal hydroxyl-containing vinyl silicone oil has the viscosity of 40 cps; the catalyst is a platinum catalyst with a viscosity of 190 cps; the inhibitor is ethynyl cyclohexanol and 2-phenyl-3-butyne-ethanol.
The release agent comprises the following components: mechanically stirring the main agent, the cross-linking agent, the inhibitor, the release force regulator and the catalyst, and fully and uniformly stirring for about 20-30 minutes; coating the stirred release agent on the surface of the substrate, wherein the temperature of an oven is 120-200 ℃, the curing time is 2-30 s, and the coating thickness is 0.6-1.2 g/m2(ii) a And (5) after coating, rewetting and rolling to obtain the release film.
TABLE 1 Release agent in the proportions (by weight)
Wherein, MQ resin: the vinyl content is 2-8%, and the viscosity is 6000-10000 mPa.s.
And (3) performance characterization of the release film:
the release films prepared in the above examples 1 to 6 and comparative examples 1 to 3 were sampled, adhered to a release film with a tesa7475 tape, prepared into a sample (width 25mm and length 12cm), and placed in an aging oven for 24 hours (humidity 80%, temperature 90 ℃, constant temperature 24 hours) at room temperature for 20 minutes and 24 hours respectively to test the release force of the release film.
10 data were tested for each set of samples and averaged.
TABLE 2 Performance index of release film
From the above, the vinyl silicone oil with hydroxyl at the terminal is applied to the preparation of the release agent as the release force regulator, so that the release film with the significantly improved release force can be obtained compared with the conventional MQ resin, and the release films with different release forces can be obtained by regulating the content of the added vinyl silicone oil with hydroxyl at the terminal, wherein the higher the content of the vinyl silicone oil with hydroxyl at the terminal is, the larger the release force of the obtained release film is.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (6)
1. The release agent is characterized by comprising the following components in parts by mass: 60-100 parts of a main agent; 3-25 parts of a crosslinking agent; 0.1-0.5 part of inhibitor; 1-30 parts of vinyl silicone oil with a hydroxyl group at the tail end; 5-10 parts of a catalyst;
the structural formula of the vinyl silicone oil containing hydroxyl at the tail end is as follows:
wherein n and m represent a repeating structural unit, n is 1-10, and m is 0-6;
the main agent is vinyl silicone oil; the cross-linking agent is hydrogen-containing silicone oil.
2. The release agent according to claim 1, characterized in that: the inhibitor is at least one of methylbutynol, ethynylcyclohexanol, 2-phenyl-3-butyne-ethanol, 3-methyl-1-pentene-4-alkyne-3 alcohol and 3- (trimethylsilyl) propiolic alcohol; the catalyst is platinum.
3. The release agent according to claim 1, characterized in that: the viscosity range of the main agent is 100-350 cps; the viscosity range of the cross-linking agent is 50-200 cps.
4. The release agent according to claim 1, characterized in that: the preparation is obtained by stirring and mixing the components uniformly.
5. A release film based on the release agent of any one of claims 1 to 4, which is obtained by coating the release agent of any one of claims 1 to 4 on a substrate, drying and rolling.
6. The release film according to claim 5, wherein: the base material is at least one of release paper, glassine paper, crepe paper, kraft paper, white board paper, coated paper, PET film, OPP film, PE film and sanitary backing material; the thickness of the coating is 0.6-1.2 g/m2(ii) a The curing time of the coating is 2-20 s; the drying temperature is 120-200 ℃.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710736953.8A CN107503231B (en) | 2017-08-24 | 2017-08-24 | Application of vinyl silicone oil with hydroxyl at tail end as release force regulator in preparation of release agent, release agent and release film |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710736953.8A CN107503231B (en) | 2017-08-24 | 2017-08-24 | Application of vinyl silicone oil with hydroxyl at tail end as release force regulator in preparation of release agent, release agent and release film |
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| CN107503231A CN107503231A (en) | 2017-12-22 |
| CN107503231B true CN107503231B (en) | 2020-01-17 |
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| CN108203568B (en) * | 2018-01-30 | 2020-10-27 | 广州国显科技有限公司 | Release film preparation method, release film and optical transparent adhesive |
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| CN115787352B (en) * | 2021-09-13 | 2023-12-19 | 万华化学集团股份有限公司 | Release agent and release paper |
| CN114016327A (en) * | 2021-11-17 | 2022-02-08 | 江苏新丰之星膜材料有限公司 | Formula for producing double-sided release paper |
| CN114058290B (en) * | 2021-11-18 | 2023-08-08 | 成都富彩新材料有限公司 | Solvent-free organosilicon release agent with ultralow release force and preparation method thereof |
| CN116925357B (en) * | 2023-07-11 | 2024-04-19 | 杭州崇耀科技发展有限公司 | Organosilicon polymer for release agent, preparation method and organosilicon release agent |
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| GB2005288A (en) * | 1977-09-30 | 1979-04-19 | Shinetsu Chemical Co | Curable organopolysiloxane compositions |
| CN101517002A (en) * | 2006-08-14 | 2009-08-26 | 陶氏康宁公司 | Silicone release coating compositions |
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