Vinyl MQ silicon resin, preparation method thereof and heavy stripping regulator

Abstract

The invention discloses vinyl MQ silicon resin, a preparation method thereof and a heavy stripping regulator. The method comprises the following steps: S1, mixing and stirring tetraethoxysilane, hexamethyldisiloxane, divinyl tetramethyldisiloxane, divinyl tetra (trimethylsiloxy) disiloxane and ethanol; then dropwise adding a hydrochloric acid aqueous solution while stirring; s2, heating and carrying out reflux reaction; s3, adding methylbenzene into a product obtained in the step S2, stirring, adding deionized water, layering, taking a methylbenzene layer, washing until chloride ions do not exist, adding a potassium hydroxide solution, heating, and reacting; and S4, after the reaction is finished, carrying out reduced pressure distillation, and removing the solvent to obtain the vinyl MQ silicon resin. The special monomer is directly added in the synthesis of the MQ resin to modify the MQ resin, and the closed MQ resin is modified after being synthesized, so that the obtained product has the advantages of stable release force, environmental measurement resistance, good adhesive force and the like after being prepared into the heavy stripping regulator.

Description

Technical Field

[0001] The invention relates to the field of release materials, and in particular to a vinyl MQ silicone resin, a preparation method thereof, and a heavy release regulator. Background Art

[0002] At present, the re-release regulators of release materials mainly rely on foreign companies such as Wacker Dow Corning. Domestic products rely on MQ resin directly dissolved in solvent as a means of re-release regulation. The performance is unstable and pollutes the environment. It is necessary to provide an independently developed re-release regulator. Summary of the Invention

[0003] The technical problem to be solved by the present invention is to provide a vinyl MQ silicone resin, a preparation method thereof and a heavy release regulator in view of the above-mentioned deficiencies in the prior art.

[0004] In order to solve the above technical problems, the technical solution adopted by the present invention is as follows: In a first aspect of the present invention, a method for preparing a vinyl MQ silicone resin is provided, comprising the following steps:

[0005] S1. Mix ethyl orthosilicate, hexamethyldisiloxane, divinyltetramethyldisiloxane, divinyltetra(trimethylsiloxy)disiloxane, and ethanol, and stir; then dropwise add aqueous hydrochloric acid solution while stirring;

[0006] S2, heating, reflux reaction;

[0007] S3, add toluene to the product obtained in step S2, stir, add deionized water, separate the layers, take the toluene layer and wash it with water until there is no chloride ion, then add potassium hydroxide solution, heat and react;

[0008] S4. After the reaction is completed, the solvent is removed by distillation under reduced pressure to obtain the vinyl MQ silicone resin.

[0009] Preferably, the preparation method of the vinyl MQ silicone resin comprises the following steps:

[0010] S1. Mix ethyl orthosilicate, hexamethyldisiloxane, divinyltetramethyldisiloxane, divinyltetra(trimethylsiloxy)disiloxane, and ethanol, and stir in a water bath at 20-30°C for 0.5-2h; add aqueous hydrochloric acid solution dropwise while stirring for 0.5-2h;

[0011] S2, heating to 70-80°C, reflux reaction for 1.5-6h;

[0012] S3. Add toluene to the product obtained in step S2, stir, add deionized water, separate the layers, wash the toluene layer with water until there is no chloride ion, add potassium hydroxide solution, heat to 100-140°C, and react for 1-4h;

[0013] S4. After the reaction is completed, the solvent is removed by distillation under reduced pressure to obtain the vinyl MQ silicone resin.

[0014] Preferably, the preparation method of the vinyl MQ silicone resin comprises the following steps:

[0015] S1. Mix ethyl orthosilicate, hexamethyldisiloxane, divinyltetramethyldisiloxane, divinyltetra(trimethylsiloxy)disiloxane, and ethanol, and stir in a water bath at 25°C for 1 hour; add aqueous hydrochloric acid solution dropwise while stirring for 1 hour;

[0016] S2, heating to 75°C, reflux reaction for 3h;

[0017] S3. Add toluene to the product obtained in step S2, stir, add deionized water, separate the layers, wash the toluene layer with water until there is no chloride ion, add potassium hydroxide solution, heat to 120°C, and react for 2h;

[0018] S4. After the reaction is completed, the solvent is removed by distillation under reduced pressure to obtain the vinyl MQ silicone resin.

[0019] Preferably, the M / Q value of the vinyl MQ silicone resin is 0.6-1.2.

[0020] Preferably, in step S1, the molar ratio of divinyltetrakis(trimethylsiloxy)disiloxane to divinyltetramethyldisiloxane is 5-20:1, and the ratio of the molar amount of hexamethyldisiloxane to the sum of the molar amounts of divinyltetrakis(trimethylsiloxy)disiloxane and divinyltetramethyldisiloxane is 2.5-10:1;

[0021] The mass of ethanol is 5-20% of the total mass of ethyl orthosilicate, hexamethyldisiloxane, divinyltetramethyldisiloxane and divinyltetra(trimethylsiloxy)disiloxane.

[0022] Preferably, the concentration of the hydrochloric acid aqueous solution is 10-15 mol / L, and the mass of the hydrochloric acid in the hydrochloric acid aqueous solution added accounts for 0.5-2% of the mass of the total feed; the total feed includes: tetraethyl orthosilicate, hexamethyldisiloxane, divinyltetramethyldisiloxane, divinyltetra(trimethylsiloxy)disiloxane and ethanol.

[0023] Preferably, the molar ratio of water added in step S3 to ethoxy groups in the reaction system is 0.4-1.6:1.

[0024] Preferably, the mass of toluene added in step S3 is 1.5-6 times the mass of the total feed;

[0025] The concentration of the potassium hydroxide solution is 20-60 wt %, and the mass ratio of potassium hydroxide to HCl is 1.5-6:2-8.

[0026] In a second aspect of the present invention, a vinyl MQ silicone resin is provided, which is prepared by the method described above.

[0027] A third aspect of the present invention provides a heavy peeling agent, which is obtained by uniformly mixing the following raw materials in parts by weight:

[0028] 40-160 parts vinyl MQ silicone resin, 50-200 parts polydimethylsiloxane, 10-40 parts C18 olefin, 1-4 parts inhibitor acetylenic alcohol.

[0029] The beneficial effects of the present invention are:

[0030] The present invention provides a vinyl MQ silicone resin, a preparation method thereof, and a heavy-release regulating agent based on the vinyl MQ silicone resin. The present invention modifies the MQ resin by directly adding a special monomer during the synthesis of the MQ resin. The MQ resin is modified after being synthesized. The obtained product is prepared into a heavy-release regulating agent, which has the advantages of stable release force, ring test resistance, good adhesion, and the like. DETAILED DESCRIPTION

[0031] The present invention is further described in detail below with reference to the embodiments so that those skilled in the art can implement the invention with reference to the description.

[0032] It should be understood that terms such as “having”, “including” and “comprising” used herein do not preclude the existence or addition of one or more other elements or combinations thereof.

[0033] Unless otherwise specified, the experimental methods used in the following examples are conventional methods. Materials and reagents used in the following examples are commercially available unless otherwise specified. In the following examples, where specific conditions are not specified, the experiments were conducted under conventional conditions or those recommended by the manufacturer. Reagents and instruments used, where the manufacturer is not specified, are commercially available conventional products.

[0034] The present invention provides a method for preparing a vinyl MQ silicone resin, comprising the following steps:

[0035] S1. Mix ethyl orthosilicate, hexamethyldisiloxane, divinyltetramethyldisiloxane, divinyltetra(trimethylsiloxy)disiloxane, and ethanol, and stir in a water bath at 20-30°C for 0.5-2h; add aqueous hydrochloric acid solution dropwise while stirring for 0.5-2h;

[0036] S2, heating to 70-80°C, reflux reaction for 1.5-6h;

[0037] S3. Add toluene to the product obtained in step S2, stir, add deionized water, separate the layers, wash the toluene layer with water until there is no chloride ion, add potassium hydroxide solution, heat to 100-140°C, and react for 1-4h;

[0038] S4. After the reaction is completed, the solvent is removed by distillation under reduced pressure to obtain vinyl MQ silicone resin.

[0039] In a preferred embodiment, the M / Q value of the vinyl MQ silicone resin is 0.6-1.2.

[0040] In a preferred embodiment, in step S1, the molar ratio of divinyltetrakis(trimethylsiloxy)disiloxane to divinyltetramethyldisiloxane is 5-20:1, the amount of ethyl orthosilicate added is based on the molar ratio of MQ to MQ resin, the M / Q ratio is 0.6-1.2, and the ratio of the molar amount of hexamethyldisiloxane to the sum of the molar amounts of divinyltetrakis(trimethylsiloxy)disiloxane and divinyltetramethyldisiloxane is 2.5-10:1.

[0041] The mass of ethanol is 5-20% of the total mass of ethyl orthosilicate, hexamethyldisiloxane, divinyltetramethyldisiloxane and divinyltetra(trimethylsiloxy)disiloxane.

[0042] Preferably, the concentration of the hydrochloric acid aqueous solution is 10-15 mol / L, and the mass of the hydrochloric acid in the hydrochloric acid aqueous solution added accounts for 0.5-2% of the mass of the total feed; the total feed includes: tetraethyl orthosilicate, hexamethyldisiloxane, divinyltetramethyldisiloxane, divinyltetra(trimethylsiloxy)disiloxane and ethanol.

[0043] Preferably, the molar ratio of water added in step S3 to ethoxy groups in the reaction system is 0.4-1.6:1.

[0044] Preferably, the mass of toluene added in step S3 is 1.5-6 times the mass of the total feed;

[0045] The concentration of the potassium hydroxide solution is 20-60 wt %, and the mass ratio of potassium hydroxide to HCl is 1.5-6:2-8.

[0046] The present invention also provides a heavy peeling regulator, which is obtained by uniformly mixing the following raw materials in parts by weight: 40-160 parts of vinyl MQ silicone resin, 50-200 parts of polydimethylsiloxane, 10-40 parts of C18 olefin, and 1-4 parts of inhibitor alkynol.

[0047] The above is the overall concept of the present invention. Detailed examples and comparative examples are provided below to further illustrate the present invention.

[0048] Example 1

[0049] A method for preparing an MQ resin for regulating heavy release force comprises the following steps:

[0050] S1. Mix ethyl orthosilicate, hexamethyldisiloxane, divinyltetramethyldisiloxane, divinyltetra(trimethylsiloxy)disiloxane, and ethanol, and stir in a water bath at 25°C for 1 hour; add aqueous hydrochloric acid solution dropwise while stirring for 1 hour;

[0051] S2, heating to 75°C, reflux reaction for 3h;

[0052] S3. Add toluene to the product obtained in step S2, stir, add deionized water, separate the layers, wash the toluene layer with water until there is no chloride ion, add potassium hydroxide solution, heat to 120°C, and react for 2h;

[0053] S4. After the reaction is completed, the solvent is removed by distillation under reduced pressure to obtain a colorless and transparent product, namely the vinyl MQ silicone resin.

[0054] The M / Q value is 0.9;

[0055] In step S1, the molar ratio of divinyltetrakis(trimethylsiloxy)disiloxane and divinyltetramethyldisiloxane is 10:1, the amount of ethyl orthosilicate added is added according to the molar ratio of MQ of the MQ resin, the M / Q ratio is 0.9, the ratio of the molar amount of hexamethyldisiloxane to the sum of the molar amounts of divinyltetrakis(trimethylsiloxy)disiloxane and divinyltetramethyldisiloxane is 5:1; the mass of ethanol is 10% of the sum of the mass of ethyl orthosilicate, hexamethyldisiloxane, divinyltetramethyldisiloxane and divinyltetrakis(trimethylsiloxy)disiloxane.

[0056] The concentration of the hydrochloric acid aqueous solution is 11.9 mol / L, and the mass of the hydrochloric acid in the added hydrochloric acid aqueous solution accounts for 1% of the total feed mass.

[0057] In step S3, the mass of toluene added is 3 times the mass of the total feed;

[0058] The concentration of potassium hydroxide solution is 40%, and the mass ratio of KOH to HCl is 3:4.

[0059] This embodiment also provides a heavy release regulator, which is obtained by uniformly mixing the following raw materials in parts by weight: 80 parts of the vinyl MQ silicone resin prepared in this embodiment, 100 parts of polydimethylsiloxane, 20 parts of C18 olefin, and 2 parts of inhibitor acetylenic alcohol.

[0060] Example 2

[0061] A method for preparing an MQ resin for regulating heavy release force comprises the following steps:

[0062] S1. Mix ethyl orthosilicate, hexamethyldisiloxane, divinyltetramethyldisiloxane, divinyltetra(trimethylsiloxy)disiloxane, and ethanol, and stir in a water bath at 25°C for 1 hour; add aqueous hydrochloric acid solution dropwise while stirring for 1 hour;

[0063] S2, heating to 75°C, reflux reaction for 3h;

[0064] S3. Add toluene to the product obtained in step S2, stir, add deionized water, separate the layers, wash the toluene layer with water until there is no chloride ion, add potassium hydroxide solution, heat to 120°C, and react for 2h;

[0065] S4. After the reaction is completed, the solvent is removed by distillation under reduced pressure to obtain a colorless and transparent product, namely the vinyl MQ silicone resin.

[0066] The M / Q value is 0.6;

[0067] In step S1, the molar ratio of divinyltetrakis(trimethylsiloxy)disiloxane and divinyltetramethyldisiloxane is 10:1, the amount of ethyl orthosilicate added is added according to the molar ratio of MQ of the MQ resin, the M / Q ratio is 0.6, the ratio of the molar amount of hexamethyldisiloxane to the sum of the molar amounts of divinyltetrakis(trimethylsiloxy)disiloxane and divinyltetramethyldisiloxane is 5:1; the mass of ethanol is 10% of the sum of the mass of ethyl orthosilicate, hexamethyldisiloxane, divinyltetramethyldisiloxane and divinyltetrakis(trimethylsiloxy)disiloxane.

[0068] The concentration of the hydrochloric acid aqueous solution is 11.9 mol / L, and the mass of the hydrochloric acid in the added hydrochloric acid aqueous solution accounts for 1% of the total feed mass.

[0069] In step S3, the mass of toluene added is 3 times the mass of the total feed;

[0070] The concentration of potassium hydroxide solution is 40%, and the mass ratio of KOH to HCl is 3:4.

[0071] This embodiment also provides a heavy release regulator, which is obtained by uniformly mixing the following raw materials in parts by weight: 80 parts of the vinyl MQ silicone resin prepared in this embodiment, 100 parts of polydimethylsiloxane, 20 parts of C18 olefin, and 2 parts of inhibitor acetylenic alcohol.

[0072] This embodiment also provides a heavy release regulator, which is obtained by uniformly mixing the following raw materials in parts by weight: 80 parts of the vinyl MQ silicone resin prepared in this embodiment, 100 parts of polydimethylsiloxane, 20 parts of C18 olefin, and 2 parts of inhibitor acetylenic alcohol.

[0073] Example 3

[0074] A method for preparing an MQ resin for regulating heavy release force comprises the following steps:

[0075] S1. Mix ethyl orthosilicate, hexamethyldisiloxane, divinyltetramethyldisiloxane, divinyltetra(trimethylsiloxy)disiloxane, and ethanol, and stir in a water bath at 25°C for 1 hour; add aqueous hydrochloric acid solution dropwise while stirring for 1 hour;

[0076] S2, heating to 75°C, reflux reaction for 3h;

[0077] S3. Add toluene to the product obtained in step S2, stir, add deionized water, separate the layers, wash the toluene layer with water until there is no chloride ion, add potassium hydroxide solution, heat to 120°C, and react for 2h;

[0078] S4. After the reaction is completed, the solvent is removed by distillation under reduced pressure to obtain a colorless and transparent product, namely the vinyl MQ silicone resin.

[0079] The M / Q value is 1.2;

[0080] In step S1, the molar ratio of divinyltetrakis(trimethylsiloxy)disiloxane and divinyltetramethyldisiloxane is 10:1, the amount of ethyl orthosilicate added is added according to the molar ratio of MQ of the MQ resin, the M / Q ratio is 1.2, the ratio of the molar amount of hexamethyldisiloxane to the sum of the molar amounts of divinyltetrakis(trimethylsiloxy)disiloxane and divinyltetramethyldisiloxane is 5:1; the mass of ethanol is 10% of the sum of the mass of ethyl orthosilicate, hexamethyldisiloxane, divinyltetramethyldisiloxane and divinyltetrakis(trimethylsiloxy)disiloxane.

[0081] The concentration of the hydrochloric acid aqueous solution is 11.9 mol / L, and the mass of the hydrochloric acid in the added hydrochloric acid aqueous solution accounts for 1% of the total feed mass.

[0082] In step S3, the mass of toluene added is 3 times the mass of the total feed;

[0083] The concentration of potassium hydroxide solution is 40%, and the mass ratio of KOH to HCl is 3:4.

[0084] This embodiment also provides a heavy release regulator, which is obtained by uniformly mixing the following raw materials in parts by weight: 80 parts of the vinyl MQ silicone resin prepared in this embodiment, 100 parts of polydimethylsiloxane, 20 parts of C18 olefin, and 2 parts of inhibitor acetylenic alcohol.

[0085] This embodiment also provides a heavy release regulator, which is obtained by uniformly mixing the following raw materials in parts by weight: 80 parts of the vinyl MQ silicone resin prepared in this embodiment, 100 parts of polydimethylsiloxane, 20 parts of C18 olefin, and 2 parts of inhibitor acetylenic alcohol.

[0086] Comparative Example 1

[0087] A method for preparing an MQ resin for regulating heavy release force comprises the following steps:

[0088] S1. Mix ethyl orthosilicate, hexamethyldisiloxane, divinyltetramethyldisiloxane, divinyltetra(trimethylsiloxy)disiloxane, and ethanol, and stir in a water bath at 25°C for 1 hour; add aqueous hydrochloric acid solution dropwise while stirring for 1 hour;

[0089] S2, heating to 75°C, reflux reaction for 3h;

[0090] S3. Add toluene to the product obtained in step S2, stir, add deionized water, separate the layers, wash the toluene layer with water until there is no chloride ion, add potassium hydroxide solution, heat to 120°C, and react for 2h;

[0091] S4. After the reaction is completed, the solvent is removed by distillation under reduced pressure to obtain a colorless and transparent product, namely the vinyl MQ silicone resin.

[0092] The M / Q value is 2.0;

[0093] In step S1, the molar ratio of divinyltetrakis(trimethylsiloxy)disiloxane and divinyltetramethyldisiloxane is 10:1, the amount of ethyl orthosilicate added is added according to the molar ratio of MQ to MQ resin, the M / Q ratio is 2.0, the ratio of the molar amount of hexamethyldisiloxane to the sum of the molar amounts of divinyltetrakis(trimethylsiloxy)disiloxane and divinyltetramethyldisiloxane is 5:1; the mass of ethanol is 10% of the sum of the mass of ethyl orthosilicate, hexamethyldisiloxane, divinyltetramethyldisiloxane and divinyltetrakis(trimethylsiloxy)disiloxane.

[0094] The concentration of the hydrochloric acid aqueous solution is 11.9 mol / L, and the mass of the hydrochloric acid in the added hydrochloric acid aqueous solution accounts for 1% of the total feed mass.

[0095] In step S3, the mass of toluene added is 3 times the mass of the total feed;

[0096] The concentration of potassium hydroxide solution is 40%, and the mass ratio of KOH to HCl is 3:4.

[0097] This embodiment also provides a heavy release regulator, which is obtained by uniformly mixing the following raw materials in parts by weight: 80 parts of the vinyl MQ silicone resin prepared in this embodiment, 100 parts of polydimethylsiloxane, 20 parts of C18 olefin, and 2 parts of inhibitor acetylenic alcohol.

[0098] This example also provides a heavy release regulator, which is obtained by uniformly mixing the following raw materials in parts by weight: 80 parts of the vinyl MQ silicone resin prepared in this example, 100 parts of polydimethylsiloxane, 20 parts of C18 olefin, and 2 parts of inhibitor acetylenic alcohol.

[0099] Comparative Example 2

[0100] A method for preparing an MQ resin for regulating heavy release force comprises the following steps:

[0101] S1. Mix ethyl orthosilicate, hexamethyldisiloxane, divinyltetramethyldisiloxane, divinyltetra(trimethylsiloxy)disiloxane, and ethanol, and stir in a water bath at 25°C for 1 hour; add aqueous hydrochloric acid solution dropwise while stirring for 1 hour;

[0102] S2, heating to 75°C, reflux reaction for 3h;

[0103] S3. Add toluene to the product obtained in step S2, stir, add deionized water, separate the layers, wash the toluene layer with water until there is no chloride ion, add potassium hydroxide solution, heat to 120°C, and react for 2h;

[0104] S4. After the reaction is completed, the solvent is removed by distillation under reduced pressure to obtain a colorless and transparent product, namely the vinyl MQ silicone resin.

[0105] The M / Q value is 0.5;

[0106] In step S1, the molar ratio of divinyltetrakis(trimethylsiloxy)disiloxane and divinyltetramethyldisiloxane is 10:1, the amount of ethyl orthosilicate added is based on the molar ratio of MQ to MQ resin, the M / Q ratio is 0.5, the molar ratio of hexamethyldisiloxane to "divinyltetrakis(trimethylsiloxy)disiloxane and divinyltetramethyldisiloxane" is 5:1, and the mass of ethanol is 10% of the sum of the masses of ethyl orthosilicate, hexamethyldisiloxane, divinyltetramethyldisiloxane, and divinyltetrakis(trimethylsiloxy)disiloxane.

[0107] The concentration of the hydrochloric acid aqueous solution is 11.9 mol / L, and the mass of the hydrochloric acid in the added hydrochloric acid aqueous solution accounts for 1% of the total feed mass.

[0108] In step S3, the mass of toluene added is 3 times the mass of the total feed;

[0109] The concentration of potassium hydroxide solution is 40%, and the mass ratio of KOH to HCl is 3:4.

[0110] This embodiment also provides a heavy release regulator, which is obtained by uniformly mixing the following raw materials in parts by weight: 80 parts of the vinyl MQ silicone resin prepared in this embodiment, 100 parts of polydimethylsiloxane, 20 parts of C18 olefin, and 2 parts of inhibitor acetylenic alcohol.

[0111] This example also provides a heavy release regulator, which is obtained by uniformly mixing the following raw materials in parts by weight: 80 parts of the vinyl MQ silicone resin prepared in this example, 100 parts of polydimethylsiloxane, 20 parts of C18 olefin, and 2 parts of inhibitor acetylenic alcohol.

[0112] The heavy release conditioning agents prepared in the examples and comparative examples were used to prepare release agents, and then the relevant performance tests were performed:

[0113] Dow SL200, a heavy release agent, methyl hydrogen silicone oil 7028, and Perkin catalyst 4000 were mixed uniformly in a mass ratio of 70:30:2.2:1.5 and then coated onto a PET base film at a coating weight of 1.2 g / m². The resulting release film was subjected to the following performance tests. A separate comparative example, Example 3, was prepared. In this comparative example, the heavy release agent was omitted. Instead, Dow SL200, methyl hydrogen silicone oil 7028, and Perkin catalyst 4000 were mixed uniformly in a mass ratio of 70:2.2:1.5. All other conditions were the same as above.

[0114] Release force at room temperature for 24 hours (7475), test standard is FTM-10;

[0115] Aged release force (7475), tested according to FTM-10;

[0116] Residual adhesion rate (%), testing standard is FTM-11;

[0117] 65 / 95 ring test release force, test standard is FTM-10;

[0118] 65 / 95 ring test residual bonding rate (%), test standard is FTM-11;

[0119] The test results are shown in Table 1 below:

[0120] Table 1

[0121]

[0122]

[0123] According to the test results in Table 1, it can be seen that MQ resin with an MQ value of 0.6-1.2 can increase the aged release force from 12 to 20-32, and the bonding rate is greater than 90%, and it is resistant to 65 / 95 ring test.

[0124] Although the embodiments of the present invention have been disclosed above, they are not limited to the applications listed in the description and implementation methods. They can be fully applied to various fields suitable for the present invention. For those familiar with the art, additional modifications can be easily implemented. Therefore, without departing from the general concept defined by the claims and the scope of equivalents, the present invention is not limited to specific details.

Claims

1. A method for preparing a vinyl MQ silicone resin, characterized in that: The following steps are involved: S1, mixing tetraethyl orthosilicate, hexamethyldisiloxane, divinyltetramethyldisiloxane, divinyltetra(trimethylsiloxy)disiloxane and ethanol, stirring; then adding dropwise hydrochloric acid aqueous solution while stirring; S2, heating, reflux reaction; S3, adding toluene to the product obtained in step S2, stirring, adding deionized water, layering, washing the toluene layer with water until there is no chloride ion, adding potassium hydroxide solution, heating, and reacting; S4. After the reaction is completed, the solvent is removed by distillation under reduced pressure to obtain the vinyl MQ silicone resin.

2. The method for preparing vinyl MQ silicone resin according to claim 1, characterized in that: The following steps are involved: S1. Mix ethyl orthosilicate, hexamethyldisiloxane, divinyltetramethyldisiloxane, divinyltetra(trimethylsiloxy)disiloxane and ethanol, and stir for 0.5-2h in a water bath at 20-30°C; add hydrochloric acid solution dropwise while stirring for 0.5-2h; S2, heating to 70-80°C, reflux reaction for 1.5-6h; S3, add toluene to the product obtained in step S2, stir, add deionized water, separate the layers, wash the toluene layer with water until there is no chloride ion, add potassium hydroxide solution, heat to 100-140°C, and react for 1-4h; S4. After the reaction is completed, the solvent is removed by distillation under reduced pressure to obtain the vinyl MQ silicone resin.

3. The method for preparing vinyl MQ silicone resin according to claim 2, characterized in that: The following steps are involved: S1. Mix ethyl orthosilicate, hexamethyldisiloxane, divinyltetramethyldisiloxane, divinyltetra(trimethylsiloxy)disiloxane and ethanol, and stir in a water bath at 25°C for 1 hour; add hydrochloric acid aqueous solution dropwise while stirring for 1 hour; S2, heating to 75°C, reflux reaction for 3h; S3, add toluene to the product obtained in step S2, stir, add deionized water, separate the layers, wash the toluene layer with water until there is no chloride ion, add potassium hydroxide solution, heat to 120°C, and react for 2h; S4. After the reaction is completed, the solvent is removed by distillation under reduced pressure to obtain the vinyl MQ silicone resin.

4. The method for preparing a vinyl MQ silicone resin according to any one of claims 1 to 3, characterized in that: The M / Q value in vinyl MQ silicone resin is 0.6-1.

2.

5. The method for preparing a vinyl MQ silicone resin according to any one of claims 1 to 3, characterized in that: In step S1, the molar ratio of divinyltetrakis(trimethylsiloxy)disiloxane to divinyltetramethyldisiloxane is 5-20:1, and the ratio of the molar amount of hexamethyldisiloxane to the sum of the molar amounts of divinyltetrakis(trimethylsiloxy)disiloxane and divinyltetramethyldisiloxane is 2.5-10:1; The mass of ethanol is 5-20% of the sum of the mass of ethyl orthosilicate, hexamethyldisiloxane, divinyltetramethyldisiloxane and divinyltetra(trimethylsiloxy)disiloxane.

6. The method for preparing a vinyl MQ silicone resin according to any one of claims 1 to 3, characterized in that: The concentration of the hydrochloric acid aqueous solution is 10-15 mol / L, and the mass of the hydrochloric acid in the hydrochloric acid aqueous solution added accounts for 0.5-2% of the mass of the total feed; the total feed includes: tetraethyl orthosilicate, hexamethyldisiloxane, divinyltetramethyldisiloxane, divinyltetra(trimethylsiloxy)disiloxane and ethanol.

7. The method for preparing a vinyl MQ silicone resin according to any one of claims 1 to 3, characterized in that: The molar ratio of the water added in step S3 to the ethoxy group in the reaction system is 0.4-1.6:

1.

8. The method for preparing a vinyl MQ silicone resin according to any one of claims 1 to 3, characterized in that: The mass of toluene added in step S3 is 1.5-6 times the mass of the total feed; The concentration of the potassium hydroxide solution is 20-60wt%, and the mass ratio of potassium hydroxide to HCl is 1.5-6:2-8.

9. A vinyl MQ silicone resin, characterized in that It is prepared by the method according to any one of claims 1 to 8.

10. A heavy peeling regulator, characterized in that The method is obtained by uniformly mixing the following raw materials in parts by weight: 40-160 parts of vinyl MQ silicone resin, 50-200 parts of polydimethylsiloxane, 10-40 parts of C18 olefin, 1-4 parts of inhibitor acetylenic alcohol.

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