阅读说明：本技术 一种溶剂型超轻离型剂 (Solvent type ultra-light release agent ) 是由 邹游 于 2020-12-23 设计创作，主要内容包括：一种溶剂型超轻离型剂,由以下制备方法而得到,具体步骤如下：(一)甲基乙烯基硅橡胶原料的制备,具体过程如下：(1)将Me4NOH结晶与DMC混合,将反应过程产生的水带出,得到油状硅醇盐即碱胶；(2)将二甲基硅氧烷混合环体DMC、四甲基四乙烯基环四硅氧烷V4、四甲基二乙烯基二硅氧烷混合、搅拌并抽真空脱去物料中的水分,加入碱胶持续反应；(3)脱去物料中未反应完全的环体,得到甲基乙烯基硅橡胶原料；(二)溶剂型超轻离型剂成品制备,将制得的甲基乙烯基硅橡胶原料与含氢硅油混合搅拌分散,并加入120#溶剂油混合物,制得溶剂型超轻离型剂。本发明在同等硅层厚度条件下离型力低,同时残余接着率基本不损失。(A solvent-type ultra-light release agent is prepared by the following preparation method, which comprises the following specific steps: the preparation method of the (I) methyl vinyl silicone rubber raw material comprises the following specific steps: (1) mixing the Me4NOH crystal with DMC, and taking out water generated in the reaction process to obtain oily silicon alkoxide, namely alkali gel; (2) mixing dimethyl siloxane mixed ring body DMC, tetramethyl tetravinylcyclotetrasiloxane V4 and tetramethyl divinyl disiloxane, stirring, vacuumizing to remove water in the materials, and adding alkali glue for continuous reaction; (3) removing unreacted cyclic bodies in the materials to obtain a methyl vinyl silicone rubber raw material; and (II) preparing a finished solvent type ultra-light release agent product, mixing and stirring the prepared methyl vinyl silicone rubber raw material and hydrogen-containing silicone oil for dispersion, and adding a mixture of No. 120 solvent oil to prepare the solvent type ultra-light release agent. The invention has low release force under the condition of the same silicon layer thickness, and the residual adhesion rate is not lost basically.)

1. The solvent type ultra-light release agent is characterized by being prepared by the following preparation method, comprising the following specific steps:

the preparation method of the (I) methyl vinyl silicone rubber raw material comprises the following specific steps:

(1) mixing Me4NOH crystal and DMC according to the mass ratio of 1: 100, placing the mixture in a round-bottom flask, heating the mixture to 70 ℃ under reduced pressure and nitrogen bubbling, taking out water generated in the reaction process by using nitrogen to obtain uniform transparent oily silicon alkoxide (namely alkali glue) with the mass content of Me4NOH being 1%, and filling the uniform transparent oily silicon alkoxide (namely alkali glue) into a bottle to be sealed for later use;

(2) adding dimethyl siloxane mixed ring DMC, tetramethyl tetravinylcyclotetrasiloxane V4 and tetramethyl divinyl disiloxane into a reaction kettle according to the mol ratio of (2000 + 2500) to (5-12) to (1-4), stirring and vacuumizing at the temperature of 50 ℃ to remove water in the materials, adding a proper amount of alkali gel after vacuumizing is stopped, and heating to 110 ℃ for continuous reaction for about 5H;

(3) after the reaction is completed, heating to 170 ℃, controlling the vacuum degree to-0.095 MPa, removing unreacted cyclic bodies in the materials, and cooling to obtain a methyl vinyl silicone rubber raw material;

and (II) preparing a finished solvent type ultralight release agent product, namely putting the prepared methyl vinyl silicone rubber raw material and hydrogen-containing silicone oil into a high-speed stirring dispersion equipment container according to the mass ratio of 1: 2, adding a 120# solvent oil mixture, and uniformly stirring to obtain the finished solvent type ultralight release agent product.

2. The solvent-based ultralight release agent according to claim 1, wherein in the specific process (2) of the specific step (one), the dimethylsiloxane mixed ring body DMC, tetramethyltetravinylcyclotetrasiloxane V4, and tetramethyldivinyldisiloxane are present in a molar ratio of 2300: 8.3: 2.

3. The solvent-based ultra-light release agent as claimed in claim 1 or 2, wherein in the step (3), the molecular weight of the siloxane in the methyl vinyl silicone rubber raw material is between 16 ten thousand and 17 ten thousand, and the vinyl molar fraction is 0.15mol/100 g.

4. The solvent-based ultra-light release agent as claimed in claim 3, wherein in the specific step (II), the solvent oil mixture is prepared by mixing methyl vinyl silicone rubber and 120# solvent oil according to the mass ratio of (20-40) to (60-80).

5. The solvent-based ultra-light release agent as claimed in claim 4, wherein the solvent oil mixture is prepared by mixing methyl vinyl silicone rubber and 120# solvent oil according to a mass ratio of 30: 70.

6. The solvent-based ultra-light release agent according to claim 1, wherein the solid content of the solvent-based ultra-light release agent is 30%.

Technical Field

The invention relates to the technical field of release agents, in particular to a solvent type ultralight release agent.

Background

The parting agent is used for preventing the formed composite material product from adhering on the mould, and a type of isolating film is applied between the product and the mould so that the product can be easily released from the mould, and simultaneously the surface quality of the product and the integrity of the mould are ensured.

The solvent type release agent commonly used in the release agent industry at present is prepared by dissolving methyl vinyl silicone rubber (commonly known as 110 crude rubber) in a toluene solvent and matching with hydrogen-containing silicone oil and a platinum catalyst, wherein the 110 crude rubber of the industry standard is generally methyl vinyl polysiloxane with the molecular weight of 50-100 ten thousand. Due to the influence of the toluene solvent, the release force tested by the solvent type release agent prepared from the toluene solvent is higher under the same silicon layer thickness, but the thin coating process (less than 0.6um) cannot be realized due to the fact that the solvent-free organic silicon release agent with small molecular weight is used and the dilution ratio cannot be enlarged.

Disclosure of Invention

Aiming at the defects of the prior art, the invention solves the technical problem of how to combine the advantages of a solvent-type release agent and a solvent-free release agent to obtain a novel release agent.

In order to solve the technical problems, the invention adopts the technical scheme that the solvent type ultra-light release agent is prepared by the following preparation method, which comprises the following specific steps:

the preparation method of the (I) methyl vinyl silicone rubber raw material comprises the following specific steps:

(1) placing the Me4NOH crystal and DMC in a round-bottom flask according to the mass ratio of 1: 100, heating to 70 ℃ under reduced pressure and nitrogen bubbling, taking out water generated in the reaction process by using nitrogen to obtain uniform transparent oily silicon alkoxide (namely alkali glue) with the mass content of Me4NOH of 1%, and filling the uniform transparent oily silicon alkoxide (namely alkali glue) into a bottle to seal for later use;

(2) adding dimethyl siloxane mixed ring DMC, tetramethyl tetravinylcyclotetrasiloxane V4 and tetramethyl divinyl disiloxane into a reaction kettle according to the mol ratio of (2000 + 2500) to (5-12) to (1-4), stirring and vacuumizing at the temperature of 50 ℃ to remove water in the materials, adding a proper amount of alkali gel after vacuumizing is stopped, and heating to 110 ℃ for continuous reaction for about 5H;

preferably, dimethyl siloxane mixed ring DMC, tetramethyl tetravinylcyclotetrasiloxane V4, tetramethyl divinyl disiloxane in a molar ratio of 2300: 8.3: 2;

(3) after the reaction is completed, heating to 170 ℃, controlling the vacuum degree to-0.095 MPa, removing unreacted cyclic bodies in the materials, and cooling to obtain a methyl vinyl silicone rubber raw material;

the molecular weight of the siloxane in the methyl vinyl silicone rubber raw material is between 16 and 17 million, and the molar fraction of vinyl is 0.15mol/100g, so that the requirement can be met;

and (II) preparing a finished solvent type ultralight release agent product, namely putting the prepared methyl vinyl silicone rubber raw material and hydrogen-containing silicone oil into a high-speed stirring dispersion equipment container according to the mass ratio of 1: 2, adding a 120# solvent oil mixture, and uniformly stirring to obtain the finished solvent type ultralight release agent product.

The solvent oil mixture is formed by mixing methyl vinyl silicone rubber and 120# solvent oil according to the mass ratio of (20-40) to (60-80); the preferred mass ratio is 30: 70.

The solid content of the solvent type ultra-light release agent is 30%.

Compared with the prior art, the invention combines the advantages of the solvent-free release agent and the conventional solvent-type release agent, has low release force under the condition of the same silicon layer thickness, and basically does not lose residual adhesion rate.

Detailed Description

The following examples are given to further illustrate the embodiments of the present invention, but are not intended to limit the invention.

Example 1:

a solvent type ultra-light release agent is prepared by the following specific steps:

the preparation method of the (I) methyl vinyl silicone rubber raw material comprises the following specific steps:

(1) placing the Me4NOH crystal and DMC in a round-bottom flask according to the mass ratio of 1: 100, heating to 70 ℃ under reduced pressure and nitrogen bubbling, taking out water generated in the reaction process by using nitrogen to obtain uniform transparent oily silicon alkoxide (namely alkali glue) with the mass content of Me4NOH of 1%, and filling the uniform transparent oily silicon alkoxide (namely alkali glue) into a bottle to seal for later use;

(2) putting dimethyl siloxane mixed ring body DMC, tetramethyl tetravinylcyclotetrasiloxane V4 and tetramethyl divinyl disiloxane into a reaction kettle according to the mol ratio of 2000: 5: 1, stirring and vacuumizing at the temperature of 50 ℃ to remove water in materials, adding a proper amount of alkali glue after vacuumizing is stopped, and heating to 110 ℃ for continuous reaction for about 5H;

(3) after the reaction is completed, heating to 170 ℃, controlling the vacuum degree to-0.095 MPa, removing unreacted cyclic bodies in the materials, and cooling to obtain a methyl vinyl silicone rubber raw material;

the molecular weight of the siloxane in the methyl vinyl silicone rubber raw material is between 16 and 17 million, and the molar fraction of vinyl is 0.15mol/100g, so that the requirement can be met;

and (II) preparing a finished solvent type ultralight release agent product, namely putting the prepared methyl vinyl silicone rubber raw material and hydrogen-containing silicone oil into a high-speed stirring dispersion equipment container according to the mass ratio of 1: 2, adding a 120# solvent oil mixture, and uniformly stirring to obtain the finished solvent type ultralight release agent product.

The solvent oil mixture is formed by mixing methyl vinyl silicone rubber and 120# solvent oil according to the mass ratio of 20: 60;

the solid content of the solvent type ultra-light release agent is 30%.

Example 2:

a solvent type ultra-light release agent is prepared by the following specific steps:

the preparation method of the (I) methyl vinyl silicone rubber raw material comprises the following specific steps:

(1) placing the Me4NOH crystal and DMC in a round-bottom flask according to the mass ratio of 1: 100, heating to 70 ℃ under reduced pressure and nitrogen bubbling, taking out water generated in the reaction process by using nitrogen to obtain uniform transparent oily silicon alkoxide (namely alkali glue) with the mass content of Me4NOH of 1%, and filling the uniform transparent oily silicon alkoxide (namely alkali glue) into a bottle to seal for later use;

(2) putting dimethyl siloxane mixed ring body DMC, tetramethyl tetravinylcyclotetrasiloxane V4 and tetramethyl divinyl disiloxane into a reaction kettle according to the mol ratio of 2300: 8.3: 2, stirring and vacuumizing at the temperature of 50 ℃ to remove water in materials, adding a proper amount of alkali glue after vacuumizing is stopped, and heating to 110 ℃ to continuously react for about 5H;

(3) after the reaction is completed, heating to 170 ℃, controlling the vacuum degree to-0.095 MPa, removing unreacted cyclic bodies in the materials, and cooling to obtain a methyl vinyl silicone rubber raw material;

the molecular weight of the siloxane in the methyl vinyl silicone rubber raw material is between 16 and 17 million, and the molar fraction of vinyl is 0.15mol/100g, so that the requirement can be met;

and (II) preparing a finished solvent type ultralight release agent product, namely putting the prepared methyl vinyl silicone rubber raw material and hydrogen-containing silicone oil into a high-speed stirring dispersion equipment container according to the mass ratio of 1: 2, adding a 120# solvent oil mixture, and uniformly stirring to obtain the finished solvent type ultralight release agent product.

The solvent oil mixture is formed by mixing methyl vinyl silicone rubber and 120# solvent oil according to the mass ratio of 30: 70;

the solid content of the solvent type ultra-light release agent is 30%.

Example 3:

a solvent type ultra-light release agent is prepared by the following specific steps:

the preparation method of the (I) methyl vinyl silicone rubber raw material comprises the following specific steps:

(1) placing the Me4NOH crystal and DMC in a round-bottom flask according to the mass ratio of 1: 100, heating to 70 ℃ under reduced pressure and nitrogen bubbling, taking out water generated in the reaction process by using nitrogen to obtain uniform transparent oily silicon alkoxide (namely alkali glue) with the mass content of Me4NOH of 1%, and filling the uniform transparent oily silicon alkoxide (namely alkali glue) into a bottle to seal for later use;

(2) putting dimethyl siloxane mixed ring body DMC, tetramethyl tetravinylcyclotetrasiloxane V4 and tetramethyl divinyl disiloxane into a reaction kettle according to the mol ratio of 2500: 12: 4, stirring and vacuumizing at the temperature of 50 ℃ to remove water in materials, adding a proper amount of alkali glue after vacuumizing is stopped, and heating to 110 ℃ for continuous reaction for about 5H;

(3) after the reaction is completed, heating to 170 ℃, controlling the vacuum degree to-0.095 MPa, removing unreacted cyclic bodies in the materials, and cooling to obtain a methyl vinyl silicone rubber raw material;

the molecular weight of the siloxane in the methyl vinyl silicone rubber raw material is between 16 and 17 million, and the molar fraction of vinyl is 0.15mol/100g, so that the requirement can be met;

and (II) preparing a finished solvent type ultralight release agent product, namely putting the prepared methyl vinyl silicone rubber raw material and hydrogen-containing silicone oil into a high-speed stirring dispersion equipment container according to the mass ratio of 1: 2, adding a 120# solvent oil mixture, and uniformly stirring to obtain the finished solvent type ultralight release agent product.

The solvent oil mixture is formed by mixing methyl vinyl silicone rubber and 120# solvent oil according to the mass ratio of 40: 80;

the solid content of the solvent type ultra-light release agent is 30%.

According to the invention, the molecular weight of the 110 raw rubber is changed, the dissolution difficulty of the methyl vinyl raw rubber is reduced, the defect that the methyl vinyl raw rubber must be dissolved by using a toluene solvent in a standard solvent type release agent in the market is avoided, and simultaneously, a higher dilution ratio is kept compared with a solvent-free release agent, the 110 raw rubber can be diluted by using 120# alkane gasoline with a high boiling point, compared with a common solvent type release agent in the market, the release force is low under the condition of the same silicon layer thickness, and meanwhile, the residual adhesion rate is not lost basically.

To better illustrate the beneficial effects of the present invention, efficacy evaluation tests were performed:

taking 1-5 g of release film product as an example, the test data is compared as follows:

the formula 1 and the formula 3 are conventional products in the market, and the formula 2 is the product of the invention, and as can be seen from the table, the solvent-free release agent in the formula 3 has low molecular weight and insufficient cohesive strength of a silicone oil layer, so that a part of a cross-linked polysiloxane network structure is easily pulled by an adhesive tape after the adhesive tape is attached to a test adhesive tape, and the residual adhesion rate is reduced; while the solvent type release agent of the formula 1 in the market has enough molecular weight and high cohesive strength, and is not easy to damage, the toluene can cause the release force to increase. The structure of the formula 2 combines the advantages of the solvent-free release agent and the conventional solvent-type release agent, ensures that the release force is low under the condition of the same silicon layer thickness, and basically does not lose the residual adhesion rate.

Compared with the prior art, the invention combines the advantages of the solvent-free release agent and the conventional solvent-type release agent, has low release force under the condition of the same silicon layer thickness, and basically does not lose residual adhesion rate.

The embodiments of the present invention have been described in detail with reference to the examples, but the present invention is not limited to the described embodiments. It will be apparent to those skilled in the art that various changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention.