Light stripping regulator for silicone oil release agent as well as preparation method and application of light stripping regulator

Abstract

The invention discloses a light stripping regulator for a silicone oil release agent as well as a preparation method and application of the light stripping regulator. According to the scheme, the light stripping regulator is formed by partial addition of hydrogen-terminated polydimethylmethylphenylsiloxane and octylene. The preparation method comprises the following steps: adding hydrogen-terminated polydimethylmethylphenylsiloxane into a flask, stirring and heating to 80 DEG C in the environment of introducing N2; adding a catalyst into the reaction kettle, slowly dropwise adding alpha-octylene, releasing heat in the dropwise adding process, controlling the dropwise adding temperature not to exceed 100 DEG C, and continuously reacting for 1 hour after the dropwise adding is finished; sampling, analyzing and observing the residual amount of Si-H, and ending the reaction to obtain a light stripping regulator product; and the requirement on the release force of the release film in the production and manufacturing process of some OCA adhesive tape industries can be met.

Description

Technical Field

[0001] The invention relates to the field of organic silicon release agents, and in particular to a light release regulator for silicon release, a synthesis method thereof, and a method for applying the light release regulator to silicon release agents. Background Art

[0002] The main function of silicone oil release agent is to be used with pressure-sensitive adhesive to protect the pressure-sensitive adhesive from contamination and make it easy to peel off when in use. The components of the release agent cannot be transferred to the surface of the pressure-sensitive adhesive to affect the viscosity of the pressure-sensitive adhesive, otherwise the pressure-sensitive adhesive will fail and the adhesion effect with the adherend will be poor. Addition-type silicone oil release agent is a vinyl silicone oil and hydrogen-containing silicone oil that are cured by a silylation reaction under a Pt catalyst.

[0003] In the electronic tape die-cutting industry, the demand for release force is getting lighter and lighter while maintaining a low silicon transfer rate to prevent silicon from transferring to the adhesive surface, resulting in the adhesive surface not being sticky during later use. Especially for some OCA tape industries, the production and manufacturing process requires very light release force for the release film (peel force 1-3g / inch, 7475 tape) and a very low silicon transfer rate (residual adhesion rate>90%).

[0004] At present, the commonly used light peeling regulator mainly includes polydimethylmethylphenylsiloxane with trimethylsiloxane at one end and dimethylhydrogensiloxane or dimethylvinylsiloxane at the other end, but the peeling force cannot fully meet the above requirements. Therefore, this patent develops a polydimethylmethylphenylsiloxane with dimethyloctylsiloxane at one end and dimethylhydrogensiloxane at the other end as a light peeling regulator. Summary of the invention

[0005] The purpose of the present invention is to solve the defects in the prior art and provide a light peeling regulator for silicone oil release agent and a preparation method and application thereof.

[0006] The light release regulator for silicone oil release agent of the present invention has the structural formula:

[0007] Among them, m=50~100, n=1~3, the molecular weight range is 2000~15000; the viscosity is 100~500cs.

[0008] Preferably, the light release regulator is a product formed by partial addition of hydrogen-terminated polydimethylmethylphenylsiloxane and octene.

[0009] The present invention also provides a method for preparing a light release regulator for a silicone oil release agent, comprising the following steps: S1: Add hydrogen-terminated polydimethylmethylphenylsiloxane into the flask and pass N 2 Stir and heat to 80°C; S2: Add the catalyst, then slowly drip a-octene, the reaction is exothermic during the dripping process, and the dripping temperature is controlled not to exceed 100°C. After the dripping is completed, continue the reaction for 1 hour; take samples for analysis to see the residual Si-H content, and terminate the reaction to obtain a light stripping regulator product; The catalyst is a metal catalyst containing Pt, Rh and Pd.

[0010] Preferably, the catalyst has a mass fraction equivalent to 5x10 -6 Chloroplatinic acid-isopropanol solution.

[0011] Preferably, the molar ratio of the hydrogen-terminated polydimethylmethylphenylsiloxane to α-octene is 1 / 0.5 to 1 / 1.5.

[0012] The present invention also provides an application method of a light release regulator for a silicone oil release agent, wherein the light release regulator for a silicone release agent is applied to the formula of the silicone release agent, and the addition amount thereof is 1% to 2% by mass.

[0013] Preferably, the light release regulator for silicone oil release agent is applied to the formula of silicone oil release agent, which comprises the following components by mass percentage: Vinyl terminated silicone rubber 88~95% Crosslinking agent 0.8~1.2% Catalyst 0.8~1.2% Anchoring agent 0.1~0.7% The light release modifier used in the silicone release agent is 1% to 2%.

[0014] Preferably, the platinum concentration of the catalyst is 5000 ppm.

[0015] Preferably, the molar fraction of vinyl in the vinyl-terminated silicone rubber is 1.0%, and the solid content is 30%.

[0016] The present invention has the following beneficial effects: Since the synthetic raw material uses hydrogen-terminated polydimethylmethylphenylsiloxane, which contains phenyl groups, and since the structure of phenyl groups is cyclic and has a large steric hindrance, the light release regulator synthesized from it is added to the silicone release agent for use, which can not only reduce the release force after aging, but also significantly improve the performance of the residual adhesion rate.

[0017] Specifically, it can reduce the release force of silicone release agent, and the release force after aging is close to the release force of the test, and the residual adhesion rate can reach more than 90%. The application of pressure-sensitive adhesive in the electronics field requires strict control of the silicon content on the surface of the adhesive. Octyl has dense CH bonds and excellent hydrophobic effect, which can effectively reduce the release force of the glue. At the same time, since the chain segment of octyl does not contain silicon, it can effectively reduce the migration of silicon to the surface of the adhesive after contact with the adhesive surface. DETAILED DESCRIPTION

[0018] In order to further understand the present invention, the technical scheme in the embodiment of the present invention will be clearly and completely described below in conjunction with the embodiment of the present invention. Obviously, the described embodiment is only a part of the embodiment of the present invention, rather than all the embodiments. Unless otherwise specified, the reagents involved in the embodiment of the present invention are all commercially available products and can be purchased through commercial channels. The chemicals and consumables used in the experiment meet the industrial production standards.

[0019] The present invention discloses a light release regulator for silicone oil release agent, and its structural formula is: , Among them, m=50~100, n=1~3, the molecular weight range is 2000~15000; the viscosity is 100~500cs.

[0020] The light release regulator is a product formed by the addition of hydrogen-terminated polydimethyl methylphenyl siloxane and octene. It is prepared by the following method for preparing a light release regulator for silicone oil release agent, the method comprising the following steps: S1: Add hydrogen-terminated polydimethylmethylphenylsiloxane into the flask and pass N 2 Stir and heat to 80°C; S2: Add the catalyst thereto, then slowly drip a-octene, the dripping process is exothermic, the dripping temperature is controlled not to exceed 100°C, and the reaction is continued for 1 hour after the dripping is completed; sample analysis is performed to determine the amount of Si-H residue, and the reaction is terminated to obtain a light stripping regulator product; the catalyst is a metal catalyst containing Pt, Rh, and Pd, and the specific catalyst is a mass fraction of 5x10 equivalent to Pt -6 Chloroplatinic acid-isopropanol solution.

[0021] The molar ratio of the hydrogen-terminated polydimethylmethylphenylsiloxane to a-octene is 1 / 0.5 to 1 / 1.5.

[0022] The application method of the light release regulator in this embodiment is to apply the light release regulator for silicone release agent to the formula of silicone release agent, and the addition amount thereof is 1% to 2% by mass percentage.

[0023] Specifically, taking the release agent of vinyl-terminated silicone rubber as an example, the light release regulator for silicone oil release agent is applied to the formula of silicone oil release agent, which includes the following components by mass percentage: Vinyl terminated silicone rubber 88~95% Crosslinking agent 0.8~1.2% Catalyst 0.8~1.2% Anchoring agent 0.1~0.7% The light release modifier used in the silicone release agent is 1% to 2%.

[0024] The platinum concentration of the catalyst is 5000 ppm. The molar fraction of vinyl in the vinyl-terminated silicone rubber is 1.0%, and the solid content is 30%.

[0025] Referring to the above preparation method, the ratio of each raw material was adjusted to prepare a release agent sample using the light release agent of the present application.

[0026]

[0027] 1. Peel force test The test was carried out in accordance with GB / T 25256-2010 Test method for 180° peel force and residual adhesion rate of release agents for optical functional films.

[0028] 2. Residual Adhesion Test The test was carried out in accordance with GB / T 25256-2010 Test method for 180° peel force and residual adhesion rate of release agents for optical functional films.

[0029] The test data for this example is shown in the following table.

[0030]

[0031] The comparative example adopts some experimental data disclosed in Chinese patent CN112761022 B "An ultra-light release force silicone release agent and its preparation method and application". The main technical scheme of the invention is that the ultra-light release force silicone release agent includes the following components by weight: a. Silicone polymer containing more than 2 vinyl groups in the molecule: 100 parts; b. Hydrogen-containing silicone polymer containing more than 2 Si-H bonds in the molecule: 0.1-10 parts; c. Silicone polymer containing epoxy group: 0-5 parts; d. Platinum group metal catalyst: the mass of platinum group metal is 10-1000ppm relative to the total mass of the release agent; e. Ultra-light release force additive: 0.01-10 parts; wherein the ultra-light release force additive is a hydrocarbon-modified MDQ type silicone resin. The peeling force and residual adhesion rate data obtained according to the above test method are as follows.

[0032]

Claims

1. A light release regulator for silicone oil release agent, characterized in that: Its structural formula is: ， Among them, m=50~100, n=1~3, the molecular weight range is 2000~15000; the viscosity is 100~500cs.

2. The light release regulator for silicone release agent according to claim 1, characterized in that: The light peeling regulator is a product formed by the addition of hydrogen-terminated polydimethyl methylphenyl siloxane and octene.

3. A method for preparing a light release regulator for silicone oil release agent, characterized in that: The steps include: S1: Add hydrogen-terminated polydimethylmethylphenylsiloxane into the flask, stir and heat to 80°C under N2 environment; S2: Add the catalyst, then slowly drip a-octene, the reaction is exothermic during the dripping process, and the dripping temperature is controlled not to exceed 100°C. After the dripping is completed, continue the reaction for 1 hour; take samples for analysis to see the residual Si-H content, and terminate the reaction to obtain a light stripping regulator product; The catalyst is a metal catalyst containing Pt, Rh and Pd.

4. The method for preparing a light release regulator for silicone oil release agent according to claim 3, characterized in that: The catalyst has a mass fraction equivalent to 5x10 -6 Chloroplatinic acid-isopropanol solution.

5. The method for preparing a light release regulator for silicone oil release agent according to claim 3, characterized in that: The molar ratio of the hydrogen-terminated polydimethylmethylphenylsiloxane to a-octene is 1 / 0.5 to 1 / 1.

5.

6. A method for applying a light release regulator for a silicone oil release agent, characterized in that: The light release regulator for the silicon release agent is applied to the formula of the silicon release agent, and its addition amount is 1% to 2% by mass percentage.

7. The method for applying the light release regulator for silicone oil release agent according to claim 6, characterized in that: The light release regulator for silicone oil release agent is applied to the formula of silicone oil release agent, which includes the following components by mass percentage: Vinyl terminated silicone rubber 88~95% Crosslinking agent 0.8~1.2% Catalyst 0.8~1.2% Anchoring agent 0.1~0.7% The light release modifier used in the silicone release agent is 1% to 2%.

8. The method for applying the light release regulator for silicone oil release agent according to claim 6, characterized in that: The platinum concentration of the catalyst is 5000 ppm.

9. The method for applying the light release regulator for silicone oil release agent according to claim 6, characterized in that: The molar fraction of vinyl in the vinyl-terminated silicone rubber is 1.0%, and the solid content is 30%.

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