阅读说明：本技术 一种硅橡胶膜及工艺便捷的制备方法 (Silicone rubber membrane and preparation method with convenient process ) 是由 崔号东 于 2021-09-17 设计创作，主要内容包括：本发明提供了一种硅橡胶膜及工艺便捷的制备方法。其中,一种硅橡胶膜,包括底层和涂敷在所述底层上的复合层,所述底层为聚偏氟乙烯多孔底膜；所述复合层为高硅沸石填充橡胶层,所述高硅沸石填充橡胶层是由聚二甲基硅氧烷溶于乙酸丁酯混合液中经过均质机分散再在真空室中在聚偏氟乙烯多孔底膜上利用雾化沉积制备而成。本发明通过真空下利用雾化沉积制备,相比于传统的刮膜法,雾化沉积可以有效的控制膜体的整体均匀性和厚度。(The invention provides a silicone rubber membrane and a preparation method with a convenient process. The silicon rubber membrane comprises a bottom layer and a composite layer coated on the bottom layer, wherein the bottom layer is a polyvinylidene fluoride porous base membrane; the composite layer is a high-silicon zeolite filled rubber layer, and the high-silicon zeolite filled rubber layer is prepared by dissolving polydimethylsiloxane in butyl acetate mixed solution, dispersing the dimethyl siloxane in a homogenizer, and performing atomization deposition on a polyvinylidene fluoride porous base membrane in a vacuum chamber. The invention is prepared by utilizing atomization deposition in vacuum, and compared with the traditional film scraping method, the atomization deposition can effectively control the integral uniformity and thickness of the film body.)

1. A silicone rubber film, characterized by comprising

The bottom layer is a polyvinylidene fluoride porous basement membrane;

the composite layer is a high-silicon zeolite filled rubber layer, and the high-silicon zeolite filled rubber layer is prepared by dissolving polydimethylsiloxane in butyl acetate mixed solution, dispersing the dimethyl siloxane in a homogenizer, and performing atomization deposition on a polyvinylidene fluoride porous base membrane in a vacuum chamber.

2. The silicone rubber membrane of claim 1, wherein the thickness of the polyvinylidene fluoride porous primary membrane is 25-70 μm.

3. The silicone rubber membrane of claim 1, wherein the thickness of the high-silica zeolite filled rubber layer is 3-200 μm.

4. The silicone rubber film according to claim 1, wherein the homogenizer dispersion is carried out at a low temperature and a pressure of 2 to 3 Mpa.

5. The preparation method of the silicone rubber membrane with convenient process is characterized by comprising the following steps:

1) preparation of the bottom layer: drying polyvinylidene fluoride, dissolving the dried polyvinylidene fluoride in an organic mixed solution of N, N-dimethylformamide and N-methylpyrrolidone to prepare a solution with the mass fraction of 15-25%, dispersing for 3-5 times at 10-15 ℃ under 3-3.5Mpa by using a homogenizer, standing, scraping a film on polyester non-woven fabric after standing, taking water as a gel bath to obtain a polyvinylidene fluoride base film supported by the polyester non-woven fabric, and naturally drying;

2) preparing a composite layer: mixing butyl acetate and petroleum ether according to the volume ratio of 5-1 to form a mixed solution, and then mixing polydimethylsiloxane and the mixed solution according to the volume ratio of 2: 6-3: 8, mixing and stirring, adding the high-silicon zeolite molecular sieve, the cross-linking agent and the catalyst, stirring again, then introducing into a homogenizer, homogenizing and dispersing for 3-5 times at 2-3Mpa by adopting low temperature and pressure, forming casting membrane liquid after dispersion is finished, introducing the casting membrane liquid into an atomizer on the upper part of a vacuum box, placing the dried polyvinylidene fluoride base membrane on a carrying platform, putting into the vacuum box, vacuumizing the vacuum box, then atomizing and depositing the casting membrane liquid on the polyvinylidene fluoride porous base membrane by utilizing the atomizer under the condition of supersaturated inert gas, keeping the vacuum pressure for 2 hours, opening the cover of the vacuum box, heating the vacuum box, promoting solvent volatilization and cross-linking, and preparing the high-silicon zeolite filled rubber membrane.

6. The method for preparing the silicone rubber membrane with convenient process according to claim 5, wherein the particle size of the high-silicon zeolite molecular sieve is 3-20 μm.

7. The method for preparing the silicone rubber film with convenient process according to claim 5, wherein the cross-linking agent is methyltrimethoxysilane, methyltriethoxysilane or methyltribunoxime silane.

8. The method for preparing the silicone rubber film with convenient process according to claim 5, wherein the catalyst is organic tin.

9. The method for preparing the silicone rubber membrane with convenient process according to claim 5, characterized in that in the casting solution, the mass of the high-silicon zeolite molecular sieve is 45-70% of the total mass, the mass of the cross-linking agent is 10-20% of the total mass, the mass of the catalyst is 1-2% of the total mass, and the balance is polydimethylsiloxane.

10. The method for preparing the silicone rubber membrane with convenient process according to claim 5, wherein in step 5), the heating temperature is as follows: 60-85 ℃.

Technical Field

The invention provides a silicone rubber membrane, particularly relates to a silicone rubber membrane and a preparation method thereof, and particularly relates to a silicone rubber membrane with a saved process and a preparation method thereof.

Background

The existing silicone rubber film is basically a two-layer composite film, the silicone rubber film is prepared on a polyvinylidene fluoride base film, the existing technical means are all obtained by blade coating, and the thickness of the film obtained by blade coating cannot be effectively controlled. In addition, in the prior art, the casting solution is basically obtained by stirring, mixing, standing and defoaming, the standing and defoaming time is long, and the preparation process time is prolonged.

Disclosure of Invention

In view of this, the invention provides a silicone rubber membrane and a preparation method with a convenient process.

The technical scheme adopted by the invention is as follows:

a silicone rubber membrane comprises

The bottom layer is a polyvinylidene fluoride porous basement membrane;

the composite layer is a high-silicon zeolite filled rubber layer, and the high-silicon zeolite filled rubber layer is prepared by dissolving polydimethylsiloxane in butyl acetate mixed solution, dispersing the dimethyl siloxane in a homogenizer, and performing atomization deposition on a polyvinylidene fluoride porous base membrane in a vacuum chamber.

Preferably, the thickness of the polyvinylidene fluoride porous base film is 25-70 μm.

Preferably, the thickness of the high-silicon zeolite filled rubber layer is 3-200 μm.

Preferably, the homogenizer is used for dispersing at low temperature and under 2-3 MPa.

The invention also provides a method for preparing the silicone rubber membrane with convenient process, which comprises the following steps:

1) preparation of the bottom layer: drying polyvinylidene fluoride, dissolving the dried polyvinylidene fluoride in an organic mixed solution of N, N-dimethylformamide and N-methylpyrrolidone to prepare a solution with the mass fraction of 15-25%, dispersing for 3-5 times at 10-15 ℃ under 3-3.5Mpa by using a homogenizer, standing, scraping a film on polyester non-woven fabric after standing, taking water as a gel bath to obtain a polyvinylidene fluoride base film supported by the polyester non-woven fabric, and naturally drying;

2) preparing a composite layer: mixing butyl acetate and petroleum ether according to the volume ratio of 5-1 to form a mixed solution, and then mixing polydimethylsiloxane and the mixed solution according to the volume ratio of 2: 6-3: 8, mixing and stirring, adding the high-silicon zeolite molecular sieve, the cross-linking agent and the catalyst, stirring again, then introducing into a homogenizer, homogenizing and dispersing for 3-5 times at 2-3Mpa by adopting low temperature and pressure, forming casting membrane liquid after dispersion is finished, introducing the casting membrane liquid into an atomizer on the upper part of a vacuum box, placing the dried polyvinylidene fluoride base membrane on a carrying platform, putting into the vacuum box, vacuumizing the vacuum box, then atomizing and depositing the casting membrane liquid on the polyvinylidene fluoride porous base membrane by utilizing the atomizer under the condition of supersaturated inert gas, keeping the vacuum pressure for 2 hours, opening the cover of the vacuum box, heating the vacuum box, promoting solvent volatilization and cross-linking, and preparing the high-silicon zeolite filled rubber membrane.

Preferably, the high-silicon zeolite molecular sieve has a particle size of 3 to 20 μm.

Preferably, the cross-linking agent is methyltrimethoxysilane or methyltriethoxysilane or methyltributone oxime silane.

Preferably, the catalyst is organotin.

Preferably, in the casting solution, the mass of the high-silicon zeolite molecular sieve is 45-70% of the total mass, the mass of the cross-linking agent is 10-20% of the total mass, the mass of the catalyst is 1-2% of the total mass, and the balance is polydimethylsiloxane.

Preferably, in step 5), the heating is carried out at a temperature of: 60-85 ℃.

The invention has the beneficial effects that:

the invention carries out dispersion by the homogenizer, compared with the traditional stirring and mixing method, the homogenization can carry out sufficient micronization and homogenization on the solution under certain pressure, and after multiple times of homogenization, the solution does not contain bubbles, and the defoaming procedure is not needed, and only the standing for a short time is needed.

The invention is prepared by utilizing atomization deposition in vacuum, and compared with the traditional film scraping method, the atomization deposition can effectively control the integral uniformity and thickness of the film body.

Drawings

In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.

FIG. 1 is a schematic view of the structure of a vacuum chamber according to the present invention.

Detailed Description

The present invention will now be described in detail with reference to the drawings and specific embodiments, wherein the exemplary embodiments and descriptions of the present invention are provided to explain the present invention without limiting the invention thereto.

First, the present invention provides a silicone rubber film comprising

The bottom layer is a polyvinylidene fluoride porous basement membrane;

the composite layer is a high-silicon zeolite filled rubber layer, and the high-silicon zeolite filled rubber layer is prepared by dissolving polydimethylsiloxane in butyl acetate mixed solution, dispersing the dimethyl siloxane in a homogenizer, and performing atomization deposition on a polyvinylidene fluoride porous base membrane in a vacuum chamber.

The thickness of the polyvinylidene fluoride porous basement membrane is 25-70 μm.

The homogenizer is used for dispersing, and compared with the traditional stirring and mixing method, the homogenizer is used for dispersing, the homogenization can be used for fully micronizing and homogenizing the solution under a certain pressure, and after multiple times of homogenization, the solution does not contain bubbles, and a defoaming procedure is not needed, and only a short-time standing is needed.

The invention is prepared by utilizing atomization deposition in vacuum, and compared with the traditional film scraping method, the atomization deposition can effectively control the integral uniformity and thickness of the film body. The thickness of the high-silicon zeolite filling rubber layer can be controlled to be 3-200 μm, and the thickness error is less than 0.3 μm.

In order to facilitate the implementation of the invention, the invention also discloses a vacuum box for carrying out atomization deposition, which comprises a box body 100, wherein the upper part of the box body is provided with an upper cover 105, and the upper cover and the box body are sealed by adopting a traditional sealing means. The two sides of the box body are uniformly provided with a plurality of heating wires, the lower side in the box body is provided with a groove body 101, the groove body 101 is used for fixing an object stage 102 for atomization and deposition, a first air vent 104 for vacuumizing is arranged on a box cover, an atomizer 108 is arranged on the box cover, an atomization nozzle 109 of the atomizer 108 is arranged on the lower surface of the box cover and is connected with the atomizer 108 through a pipeline, and a second air vent 106 and a liquid inlet 107 are arranged on the atomizer 108.

Example 1

This example describes the case where the thickness of the high-silica zeolite-filled rubber layer is 20 μm.

A method for preparing a silicone rubber membrane with convenient process comprises the following steps:

1) preparation of the bottom layer: drying polyvinylidene fluoride, dissolving the dried polyvinylidene fluoride in an organic mixed solution of N, N-dimethylformamide and N-methylpyrrolidone to prepare a solution with the mass fraction of 15-25%, dispersing for 3-5 times at 10-15 ℃ under 3-3.5Mpa by using a homogenizer, standing, scraping a film on polyester non-woven fabric after standing, taking water as a gel bath to obtain a polyvinylidene fluoride base film supported by the polyester non-woven fabric, and naturally drying; the thickness of the polyvinylidene fluoride porous basement membrane is controlled to be 50 mu m.

2) Preparing a composite layer: mixing butyl acetate and petroleum ether according to the volume ratio of 5-1 to form a mixed solution, and then mixing polydimethylsiloxane and the mixed solution according to the volume ratio of 2: 6-3: 8, mixing and stirring, adding the high-silicon zeolite molecular sieve with the particle size of 3-20 mu m, methyltrimethoxysilane and organic tin, stirring again, then introducing into a homogenizer, homogenizing and dispersing for 3-5 times at low temperature and under the pressure of 2-3Mpa, and finishing dispersion to form a casting solution, wherein in the casting solution, the mass of the high-silicon zeolite molecular sieve is 45-70% of the total mass, the mass of the crosslinking agent is 10-20% of the total mass, the mass of the catalyst is 1-2% of the total mass, and the balance is polydimethylsiloxane. Introducing the casting solution into an atomizer on the upper part of a vacuum box, placing the dried polyvinylidene fluoride base membrane on an objective table, putting the object table into the vacuum box, vacuumizing the vacuum box, then atomizing and depositing the casting solution on the polyvinylidene fluoride porous base membrane by using the atomizer under the condition of supersaturated inert gas, maintaining the vacuum pressure for 2 hours, opening a box cover of the vacuum box, heating the vacuum box at the temperature of 60-85 ℃, promoting solvent volatilization and crosslinking, and preparing the high-silicon zeolite filled rubber membrane.

In the above examples, the examples were set up as 5 comparative examples, e.g., 3, 4, 5 for homogenization, according to various setting conditions, including the control of the pressure and number of homogenization, and the ratio of the casting solution raw materials.

The casting solution A for the comparative example comprises 45% by mass of the high-silicon zeolite molecular sieve, 10% by mass of the cross-linking agent, 1% by mass of the catalyst and the balance of polydimethylsiloxane.

And the casting solution B for the comparative example comprises 50% by mass of the high-silicon zeolite molecular sieve, 15% by mass of the cross-linking agent, 1.2% by mass of the catalyst and the balance of polydimethylsiloxane.

And the casting solution C for the comparative example comprises 55% by mass of the high-silicon zeolite molecular sieve, 17% by mass of the cross-linking agent, 1.5% by mass of the catalyst and the balance of polydimethylsiloxane.

And the casting solution D for the comparative example comprises 65% by mass of the high-silicon zeolite molecular sieve, 18% by mass of the cross-linking agent, 1.8% by mass of the catalyst and the balance of polydimethylsiloxane.

And the casting solution E for the comparative example comprises 75% by mass of the high-silicon zeolite molecular sieve, 15% by mass of the cross-linking agent, 1.5% by mass of the catalyst and the balance of polydimethylsiloxane.

The overall thickness of the prepared silicone rubber film was measured to be controlled at 0.28 μm.

Example 2

This example describes the thickness of the high-silica zeolite-filled rubber layer of 50 μm as an example.

A method for preparing a silicone rubber membrane with convenient process comprises the following steps:

1) preparation of the bottom layer: drying polyvinylidene fluoride, dissolving the dried polyvinylidene fluoride in an organic mixed solution of N, N-dimethylformamide and N-methylpyrrolidone to prepare a solution with the mass fraction of 15-25%, dispersing for 3-5 times at 10-15 ℃ under 3-3.5Mpa by using a homogenizer, standing, scraping a film on polyester non-woven fabric after standing, taking water as a gel bath to obtain a polyvinylidene fluoride base film supported by the polyester non-woven fabric, and naturally drying; the thickness of the polyvinylidene fluoride porous basement membrane is controlled to be 50 mu m.

2) Preparing a composite layer: mixing butyl acetate and petroleum ether according to the volume ratio of 5-1 to form a mixed solution, and then mixing polydimethylsiloxane and the mixed solution according to the volume ratio of 2: 6-3: 8, mixing and stirring, adding the high-silicon zeolite molecular sieve with the particle size of 3-20 mu m, methyltrimethoxysilane and organic tin, stirring again, then introducing into a homogenizer, homogenizing and dispersing for 3-5 times at low temperature and under the pressure of 2-3Mpa, and finishing dispersion to form a casting solution, wherein in the casting solution, the mass of the high-silicon zeolite molecular sieve is 45-70% of the total mass, the mass of the crosslinking agent is 10-20% of the total mass, the mass of the catalyst is 1-2% of the total mass, and the balance is polydimethylsiloxane. Introducing the casting solution into an atomizer on the upper part of a vacuum box, placing the dried polyvinylidene fluoride base membrane on an objective table, putting the object table into the vacuum box, vacuumizing the vacuum box, then atomizing and depositing the casting solution on the polyvinylidene fluoride porous base membrane by using the atomizer under the condition of supersaturated inert gas, maintaining the vacuum pressure for 2 hours, opening a box cover of the vacuum box, heating the vacuum box at the temperature of 60-85 ℃, promoting solvent volatilization and crosslinking, and preparing the high-silicon zeolite filled rubber membrane.

In the above examples, the examples were set up as 5 comparative examples, e.g., 3, 4, 5 for homogenization, according to various setting conditions, including the control of the pressure and number of homogenization, and the ratio of the casting solution raw materials.

The casting solution A for the comparative example comprises 45% by mass of the high-silicon zeolite molecular sieve, 10% by mass of the cross-linking agent, 1% by mass of the catalyst and the balance of polydimethylsiloxane.

And the casting solution B for the comparative example comprises 50% by mass of the high-silicon zeolite molecular sieve, 15% by mass of the cross-linking agent, 1.2% by mass of the catalyst and the balance of polydimethylsiloxane.

And the casting solution C for the comparative example comprises 55% by mass of the high-silicon zeolite molecular sieve, 17% by mass of the cross-linking agent, 1.5% by mass of the catalyst and the balance of polydimethylsiloxane.

And the casting solution D for the comparative example comprises 65% by mass of the high-silicon zeolite molecular sieve, 18% by mass of the cross-linking agent, 1.8% by mass of the catalyst and the balance of polydimethylsiloxane.

And the casting solution E for the comparative example comprises 75% by mass of the high-silicon zeolite molecular sieve, 15% by mass of the cross-linking agent, 1.5% by mass of the catalyst and the balance of polydimethylsiloxane.

Through measurement, the whole thickness of the prepared silicon rubber film is controlled to be 0.23 mu m.

Example 3

This example describes the thickness of the high silica zeolite filled rubber layer as 100 μm.

A method for preparing a silicone rubber membrane with convenient process comprises the following steps:

1) preparation of the bottom layer: drying polyvinylidene fluoride, dissolving the dried polyvinylidene fluoride in an organic mixed solution of N, N-dimethylformamide and N-methylpyrrolidone to prepare a solution with the mass fraction of 15-25%, dispersing for 3-5 times at 10-15 ℃ under 3-3.5Mpa by using a homogenizer, standing, scraping a film on polyester non-woven fabric after standing, taking water as a gel bath to obtain a polyvinylidene fluoride base film supported by the polyester non-woven fabric, and naturally drying; the thickness of the polyvinylidene fluoride porous basement membrane is controlled to be 50 mu m.

2) Preparing a composite layer: mixing butyl acetate and petroleum ether according to the volume ratio of 5-1 to form a mixed solution, and then mixing polydimethylsiloxane and the mixed solution according to the volume ratio of 2: 6-3: 8, mixing and stirring, adding the high-silicon zeolite molecular sieve with the particle size of 3-20 mu m, methyltrimethoxysilane and organic tin, stirring again, then introducing into a homogenizer, homogenizing and dispersing for 3-5 times at low temperature and under the pressure of 2-3Mpa, and finishing dispersion to form a casting solution, wherein in the casting solution, the mass of the high-silicon zeolite molecular sieve is 45-70% of the total mass, the mass of the crosslinking agent is 10-20% of the total mass, the mass of the catalyst is 1-2% of the total mass, and the balance is polydimethylsiloxane. Introducing the casting solution into an atomizer on the upper part of a vacuum box, placing the dried polyvinylidene fluoride base membrane on an objective table, putting the object table into the vacuum box, vacuumizing the vacuum box, then atomizing and depositing the casting solution on the polyvinylidene fluoride porous base membrane by using the atomizer under the condition of supersaturated inert gas, maintaining the vacuum pressure for 2 hours, opening a box cover of the vacuum box, heating the vacuum box at the temperature of 60-85 ℃, promoting solvent volatilization and crosslinking, and preparing the high-silicon zeolite filled rubber membrane.

In the above examples, the examples were set up as 5 comparative examples, e.g., 3, 4, 5 for homogenization, according to various setting conditions, including the control of the pressure and number of homogenization, and the ratio of the casting solution raw materials.

The casting solution A for the comparative example comprises 45% by mass of the high-silicon zeolite molecular sieve, 10% by mass of the cross-linking agent, 1% by mass of the catalyst and the balance of polydimethylsiloxane.

And the casting solution B for the comparative example comprises 50% by mass of the high-silicon zeolite molecular sieve, 15% by mass of the cross-linking agent, 1.2% by mass of the catalyst and the balance of polydimethylsiloxane.

And the casting solution C for the comparative example comprises 55% by mass of the high-silicon zeolite molecular sieve, 17% by mass of the cross-linking agent, 1.5% by mass of the catalyst and the balance of polydimethylsiloxane.

And the casting solution D for the comparative example comprises 65% by mass of the high-silicon zeolite molecular sieve, 18% by mass of the cross-linking agent, 1.8% by mass of the catalyst and the balance of polydimethylsiloxane.

And the casting solution E for the comparative example comprises 75% by mass of the high-silicon zeolite molecular sieve, 15% by mass of the cross-linking agent, 1.5% by mass of the catalyst and the balance of polydimethylsiloxane.

Through measurement, the whole thickness of the prepared silicon rubber film is controlled to be 0.15 mu m.

Example 4

This example describes the thickness of the high-silica zeolite-filled rubber layer as 150 μm.

A method for preparing a silicone rubber membrane with convenient process comprises the following steps:

1) preparation of the bottom layer: drying polyvinylidene fluoride, dissolving the dried polyvinylidene fluoride in an organic mixed solution of N, N-dimethylformamide and N-methylpyrrolidone to prepare a solution with the mass fraction of 15-25%, dispersing for 3-5 times at 10-15 ℃ under 3-3.5Mpa by using a homogenizer, standing, scraping a film on polyester non-woven fabric after standing, taking water as a gel bath to obtain a polyvinylidene fluoride base film supported by the polyester non-woven fabric, and naturally drying; the thickness of the polyvinylidene fluoride porous basement membrane is controlled to be 50 mu m.

2) Preparing a composite layer: mixing butyl acetate and petroleum ether according to the volume ratio of 5-1 to form a mixed solution, and then mixing polydimethylsiloxane and the mixed solution according to the volume ratio of 2: 6-3: 8, mixing and stirring, adding the high-silicon zeolite molecular sieve with the particle size of 3-20 mu m, methyltrimethoxysilane and organic tin, stirring again, then introducing into a homogenizer, homogenizing and dispersing for 3-5 times at low temperature and under the pressure of 2-3Mpa, and finishing dispersion to form a casting solution, wherein in the casting solution, the mass of the high-silicon zeolite molecular sieve is 45-70% of the total mass, the mass of the crosslinking agent is 10-20% of the total mass, the mass of the catalyst is 1-2% of the total mass, and the balance is polydimethylsiloxane. Introducing the casting solution into an atomizer on the upper part of a vacuum box, placing the dried polyvinylidene fluoride base membrane on an objective table, putting the object table into the vacuum box, vacuumizing the vacuum box, then atomizing and depositing the casting solution on the polyvinylidene fluoride porous base membrane by using the atomizer under the condition of supersaturated inert gas, maintaining the vacuum pressure for 2 hours, opening a box cover of the vacuum box, heating the vacuum box at the temperature of 60-85 ℃, promoting solvent volatilization and crosslinking, and preparing the high-silicon zeolite filled rubber membrane.

In the above examples, the examples were set up as 5 comparative examples, e.g., 3, 4, 5 for homogenization, according to various setting conditions, including the control of the pressure and number of homogenization, and the ratio of the casting solution raw materials.

The casting solution A for the comparative example comprises 45% by mass of the high-silicon zeolite molecular sieve, 10% by mass of the cross-linking agent, 1% by mass of the catalyst and the balance of polydimethylsiloxane.

And the casting solution B for the comparative example comprises 50% by mass of the high-silicon zeolite molecular sieve, 15% by mass of the cross-linking agent, 1.2% by mass of the catalyst and the balance of polydimethylsiloxane.

And the casting solution C for the comparative example comprises 55% by mass of the high-silicon zeolite molecular sieve, 17% by mass of the cross-linking agent, 1.5% by mass of the catalyst and the balance of polydimethylsiloxane.

And the casting solution D for the comparative example comprises 65% by mass of the high-silicon zeolite molecular sieve, 18% by mass of the cross-linking agent, 1.8% by mass of the catalyst and the balance of polydimethylsiloxane.

And the casting solution E for the comparative example comprises 75% by mass of the high-silicon zeolite molecular sieve, 15% by mass of the cross-linking agent, 1.5% by mass of the catalyst and the balance of polydimethylsiloxane.

Through measurement, the whole thickness of the prepared silicon rubber film is controlled to be 0.18 mu m.

Example 5

This example describes the thickness of the high-silica zeolite-filled rubber layer as being 200 μm.

A preparation method of a silicone rubber membrane comprises the following steps:

1) preparation of the bottom layer: drying polyvinylidene fluoride, dissolving the dried polyvinylidene fluoride in an organic mixed solution of N, N-dimethylformamide and N-methylpyrrolidone to prepare a solution with the mass fraction of 15-25%, dispersing for 3-5 times at 10-15 ℃ under 3-3.5Mpa by using a homogenizer, standing, scraping a film on polyester non-woven fabric after standing, taking water as a gel bath to obtain a polyvinylidene fluoride base film supported by the polyester non-woven fabric, and naturally drying; the thickness of the polyvinylidene fluoride porous basement membrane is controlled to be 50 mu m.

2) Preparing a composite layer: mixing butyl acetate and petroleum ether according to the volume ratio of 5-1 to form a mixed solution, and then mixing polydimethylsiloxane and the mixed solution according to the volume ratio of 2: 6-3: 8, mixing and stirring, adding the high-silicon zeolite molecular sieve with the particle size of 3-20 mu m, methyltrimethoxysilane and organic tin, stirring again, then introducing into a homogenizer, homogenizing and dispersing for 3-5 times at low temperature and under the pressure of 2-3Mpa, and finishing dispersion to form a casting solution, wherein in the casting solution, the mass of the high-silicon zeolite molecular sieve is 45-70% of the total mass, the mass of the crosslinking agent is 10-20% of the total mass, the mass of the catalyst is 1-2% of the total mass, and the balance is polydimethylsiloxane. Introducing the casting solution into an atomizer on the upper part of a vacuum box, placing the dried polyvinylidene fluoride base membrane on an objective table, putting the object table into the vacuum box, vacuumizing the vacuum box, then atomizing and depositing the casting solution on the polyvinylidene fluoride porous base membrane by using the atomizer under the condition of supersaturated inert gas, maintaining the vacuum pressure for 2 hours, opening a box cover of the vacuum box, heating the vacuum box at the temperature of 60-85 ℃, promoting solvent volatilization and crosslinking, and preparing the high-silicon zeolite filled rubber membrane.

In the above examples, the examples were set up as 5 comparative examples, e.g., 3, 4, 5 for homogenization, according to various setting conditions, including the control of the pressure and number of homogenization, and the ratio of the casting solution raw materials.

The casting solution A for the comparative example comprises 45% by mass of the high-silicon zeolite molecular sieve, 10% by mass of the cross-linking agent, 1% by mass of the catalyst and the balance of polydimethylsiloxane.

And the casting solution B for the comparative example comprises 50% by mass of the high-silicon zeolite molecular sieve, 15% by mass of the cross-linking agent, 1.2% by mass of the catalyst and the balance of polydimethylsiloxane.

And the casting solution C for the comparative example comprises 55% by mass of the high-silicon zeolite molecular sieve, 17% by mass of the cross-linking agent, 1.5% by mass of the catalyst and the balance of polydimethylsiloxane.

And the casting solution D for the comparative example comprises 65% by mass of the high-silicon zeolite molecular sieve, 18% by mass of the cross-linking agent, 1.8% by mass of the catalyst and the balance of polydimethylsiloxane.

And the casting solution E for the comparative example comprises 75% by mass of the high-silicon zeolite molecular sieve, 15% by mass of the cross-linking agent, 1.5% by mass of the catalyst and the balance of polydimethylsiloxane.

The overall thickness of the prepared silicone rubber film was measured to be controlled at 0.27 μm.

As can be seen from the analysis of examples 1 to 5, the accuracy of the control was the best when the film thickness was 100 μm, and the error was increased both when the film thickness was more than and less than 100. mu.m. This is because the smaller the film thickness is, the less it is easy to control accurately, and the larger the film thickness is, the larger factors are disturbed by the external environment, such as the decrease in the working time efficiency of the machine, so that the film thickness cannot be controlled accurately.

The technical solutions disclosed in the embodiments of the present invention are described in detail above, and the principles and embodiments of the present invention are explained in the present document by using specific embodiments, and the descriptions of the embodiments are only used to help understanding the principles of the embodiments of the present invention; meanwhile, for a person skilled in the art, according to the embodiments of the present invention, there may be variations in the specific implementation manners and application ranges, and in summary, the content of the present description should not be construed as a limitation to the present invention.