CN113637281A - Organic silicon oxygen-enriched film and preparation method thereof - Google Patents

Organic silicon oxygen-enriched film and preparation method thereof Download PDF

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Publication number
CN113637281A
CN113637281A CN202110978030.XA CN202110978030A CN113637281A CN 113637281 A CN113637281 A CN 113637281A CN 202110978030 A CN202110978030 A CN 202110978030A CN 113637281 A CN113637281 A CN 113637281A
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oxygen
organic silicon
enriched film
benzoyl peroxide
glue
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CN113637281B (en
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牟六生
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Sichuan Xinda Adhesive Technology Co ltd
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Sichuan Xinda Adhesive Technology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18Manufacture of films or sheets
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F253/00Macromolecular compounds obtained by polymerising monomers on to natural rubbers or derivatives thereof
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F283/00Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
    • C08F283/12Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polysiloxanes
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2351/00Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers
    • C08J2351/08Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers grafted on to macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2451/00Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers
    • C08J2451/04Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers grafted on to rubbers
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/54Silicon-containing compounds
    • C08K5/544Silicon-containing compounds containing nitrogen
    • C08K5/5465Silicon-containing compounds containing nitrogen containing at least one C=N bond

Abstract

The invention discloses an organic silicon oxygen-enriched film and a preparation method thereof, wherein the preparation method comprises the steps of uniformly mixing 107 glue, methyl methacrylate and gutta percha, heating to 55-65 ℃, dropwise adding a benzoyl peroxide solution, maintaining the temperature of a reaction system at 80-90 ℃, reacting for 2-3h, then intermittently vacuumizing until reactants are semitransparent, and cooling to obtain a base material; and uniformly stirring the base material, the organic tin and the methyl tributyl ketoxime silane, discharging steam in vacuum, and molding to obtain the organic silicon oxygen-enriched film. The oxygen-enriched film can effectively solve the problem of poor mechanical property of the existing organic silicon oxygen-enriched film.

Description

Organic silicon oxygen-enriched film and preparation method thereof
Technical Field
The invention relates to
Background
The organic silicon copolymer has many excellent performances such as high and low temperature resistance, physiological inertia, air permeability and the like, but has the defects of poor solvent resistance and mechanical property, high cost and the like, and in order to develop the wide application of the organic silicon copolymer, the organic silicon polymer is copolymerized with other organic polymers to make up the defects of the organic silicon polymer.
The modification by the graft copolymer is a main method developed in the seventies of the last century, has simple and convenient operation method and environmental protection, and is widely applied to the synthesis of new materials in recent years.
The principle of the method is that unsaturated bonds and olefin bonds on an organic silicon main chain are grafted to the organic silicon main chain under the action of a catalyst, so that the common performance of two different molecular polymers is formed, the purpose of advantage complementation is achieved, the application range of the polymers is widened, the comprehensive utilization is realized, and the cost is greatly reduced.
At present, the raw materials of organic synthesis are mainly from petrochemical industry, and with the development of economy, natural chemical raw materials are increasingly barren, and it is particularly important to find alternative raw materials.
The oxygen-enriched membrane is a new technology for preparing oxygen-enriched air developed in recent years, and the most widely used oxygen-enriched membrane material is silicon rubber which has the defects of high oxygen permeation speed and poor mechanical property.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides an organic silicon oxygen-enriched film and a preparation method thereof, and the oxygen-enriched film can effectively solve the problem of poor mechanical property of the existing organic silicon oxygen-enriched film.
In order to achieve the purpose, the technical scheme adopted by the invention for solving the technical problems is as follows:
a preparation method of an organic silicon oxygen-enriched film comprises the following steps:
(1) uniformly mixing 107 glue, methyl methacrylate and gutta-percha, heating to 55-65 ℃, dropwise adding a benzoyl peroxide solution, maintaining the temperature of a reaction system at 80-90 ℃, reacting for 2-3 hours, then intermittently vacuumizing until reactants are semitransparent, and cooling to obtain a base material;
(2) and uniformly stirring the base material, the organic tin and the methyl tributyl ketoxime silane, discharging steam in vacuum, and molding to obtain the organic silicon oxygen-enriched film.
In the scheme, the eucommia ulmoides gum is grafted to the 107 gum through the methyl methacrylate, so that a three-dimensional cross-linked network is formed in a system, the mechanical property of the material is improved, and the mechanical properties such as the wear resistance of the prepared oxygen-enriched membrane are further improved; the reaction system is exothermic, a small amount of water can be generated after the reaction, and the water is pumped out in a vacuumizing mode, so that the subsequent operation is facilitated; and (3) after the reaction in the step (2), discharging gas generated in the raw material in a vacuum steam discharging mode, and avoiding the influence on the use of the oxygen-enriched film due to the existence of air holes on the film material after the mold is made.
Further, in step (1).
Further, the viscosity of the 107 glue was 3500 and 5000 mPas.
Furthermore, the mass concentration of the benzoyl peroxide is 25-35%.
Further, the solvent in the benzoyl peroxide solution is ethyl acetate.
Further, the mass ratio of the base material, the organic tin and the methyl tributyl ketoxime silane in the step (2) is 100:0.3-0.5: 3-4.
The beneficial effects produced by the invention are as follows:
according to the invention, the eucommia ulmoides gum is grafted to the 107 gum through the methyl methacrylate, so that a three-dimensional cross-linked network is formed in the system, the stability of the system is increased, the mechanical property of the system is further improved, and the wear resistance of the oxygen-enriched membrane is improved. The preparation method is simple and convenient to operate.
Detailed Description
Example 1
An organic silicon oxygen-enriched film is prepared by the following steps:
(1) uniformly mixing 107 glue with the viscosity of 3500 mPas, methyl methacrylate and eucommia ulmoides gum, heating to 55 ℃, dropwise adding a 25% benzoyl peroxide solution, maintaining the temperature of a reaction system at 80 ℃, reacting for 2 hours, intermittently vacuumizing until reactants are semitransparent, and cooling to obtain a base material; wherein the mass ratio of the 107 glue to the methyl methacrylate to the benzoyl peroxide to the eucommia ulmoides gum is 100:15:3: 8;
(2) uniformly stirring the base material, the organic tin and the methyl tributyl ketoxime silane according to the mass ratio of 100:0.3:3, discharging steam in vacuum, and molding to obtain the organic silicon oxygen-enriched film.
Example 2
An organic silicon oxygen-enriched film is prepared by the following steps:
(1) uniformly mixing 107 glue with the viscosity of 5000 mPas, methyl methacrylate and eucommia ulmoides gum, heating to 65 ℃, dropwise adding 35% by mass benzoyl peroxide solution, maintaining the temperature of a reaction system at 90 ℃, reacting for 3 hours, intermittently vacuumizing until reactants are semitransparent, and cooling to obtain a base material; wherein the mass ratio of the 107 glue to the methyl methacrylate to the benzoyl peroxide to the eucommia ulmoides gum is 100:25:5: 12;
(2) uniformly stirring the base material, the organic tin and the methyl tributyl ketoxime silane according to the mass ratio of 100:0.5:4, discharging steam in vacuum, and molding to obtain the organic silicon oxygen-enriched film.
Example 3
An organic silicon oxygen-enriched film is prepared by the following steps:
(1) uniformly mixing 107 glue with the viscosity of 4000mPa & s, methyl methacrylate and gutta-percha, heating to 60 ℃, dropwise adding a benzoyl peroxide solution with the mass concentration of 30%, maintaining the temperature of a reaction system at 85 ℃, reacting for 2 hours, then intermittently vacuumizing until reactants are semitransparent, and cooling to obtain a base material; wherein the mass ratio of the 107 glue to the methyl methacrylate to the benzoyl peroxide to the eucommia ulmoides gum is 100:20:4: 10;
(2) uniformly stirring the base material, the organic tin and the methyl tributyl ketoxime silane according to the mass ratio of 100:0.4:4, discharging steam in vacuum, and molding to obtain the organic silicon oxygen-enriched film.
Test examples
The mechanical properties and oxygen permeability of the oxygen-enriched films prepared in examples 1 to 3 were respectively tested, and the specific test results are shown in table 1.
Table 1: oxygen-enriched membrane performance
Figure BDA0003224732130000041
From the data in the above table, it is clear that the mechanical properties and oxygen permeability of the oxygen-rich films of examples 1-3 are higher than those of the conventional 107 glue.

Claims (7)

1. The preparation method of the organic silicon oxygen-enriched film is characterized by comprising the following steps:
(1) uniformly mixing 107 glue, methyl methacrylate and gutta-percha, heating to 55-65 ℃, dropwise adding a benzoyl peroxide solution, maintaining the temperature of a reaction system at 80-90 ℃, reacting for 2-3 hours, then intermittently vacuumizing until reactants are semitransparent, and cooling to obtain a base material;
(2) and uniformly stirring the base material, the organic tin and the methyl tributyl ketoxime silane, discharging steam in vacuum, and molding to obtain the organic silicon oxygen-enriched film.
2. The method for preparing the organosilicon oxygen-rich membrane as claimed in claim 1, wherein the mass ratio of the 107 glue, the methyl methacrylate, the benzoyl peroxide and the eucommia ulmoides gum in the step (1) is 100:15-25:3-5: 8-12.
3. The method of claim 1, wherein the viscosity of the 107 glue is 3500-5000 mps.
4. The method of producing an organosilicon oxygen-rich membrane according to claim 1, wherein the benzoyl peroxide is present in a concentration of 25 to 35% by mass.
5. The method of claim 1, wherein the solvent in the benzoyl peroxide solution is ethyl acetate.
6. The method for producing an organosilicon oxygen-rich film according to claim 1, wherein the mass ratio of the binder, the organotin and the methyltributanonoximosilane in the step (2) is 100:0.3 to 0.5:3 to 4.
7. An organosilicon oxygen-rich film produced by the production method according to any one of claims 1 to 6.
CN202110978030.XA 2021-08-23 2021-08-23 Organic silicon oxygen-enriched membrane and preparation method thereof Active CN113637281B (en)

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Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
张可达, 刘南安, 田禾: "改性硅橡胶富氧膜的制备", 应用化学, no. 01, pages 92 - 94 *

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