CN113637281B - Organic silicon oxygen-enriched membrane and preparation method thereof - Google Patents

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

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Publication number
CN113637281B
CN113637281B CN202110978030.XA CN202110978030A CN113637281B CN 113637281 B CN113637281 B CN 113637281B CN 202110978030 A CN202110978030 A CN 202110978030A CN 113637281 B CN113637281 B CN 113637281B
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enriched
oxygen
organic silicon
silicon oxygen
base material
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CN113637281A (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

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  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
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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 benzoyl peroxide solution, maintaining the temperature of a reaction system at 80-90 ℃, reacting for 2-3 hours, intermittently vacuumizing until reactants are semitransparent, and cooling to obtain a base material; and uniformly stirring the base material, the organotin and the methyltributylketon oxime-based silane, exhausting steam in vacuum, and molding to obtain the organic silicon oxygen-enriched film. The oxygen-enriched membrane can effectively solve the problem of poor mechanical property of the traditional organic silicon oxygen-enriched membrane.

Description

Organic silicon oxygen-enriched membrane and preparation method thereof
Technical Field
The present invention relates to
Background
The organosilicon copolymer has many excellent properties such as high and low temperature resistance, physiological inertia, air permeability and the like, but has the defects of poor solvent resistance, mechanical property, high cost and the like, so that the organosilicon copolymer can make up the defects of organosilicon polymers by copolymerizing the organosilicon polymers with other organic polymers for developing the wide application of the organosilicon copolymer.
The modification by the graft copolymer is the main method for modification developed in seventies of the last century, has the advantages of simple and convenient operation method and environmental protection, and is widely applied to new material synthesis in recent years.
The principle of the method is that unsaturated bonds and olefin bonds on the 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 complementary advantages is achieved, the application range of the organic silicon main chain is improved, the comprehensive utilization is realized, and the cost is greatly reduced.
Organic synthetic raw materials, which are mainly from petrochemical industry at present, are increasingly barren with economic development, and it is important to find alternative raw materials.
The oxygen-enriched membrane is a new technology for preparing oxygen-enriched air, which is developed in recent years, and the oxygen-enriched membrane material which is most widely used at present is silicon rubber, has high oxygen permeation speed and has the defect of poor mechanical property.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides an organic silicon oxygen-enriched membrane and a preparation method thereof, and the oxygen-enriched membrane can effectively solve the problem of poor mechanical property of the traditional organic silicon oxygen-enriched membrane.
In order to achieve the above purpose, the technical scheme adopted by the invention for solving the technical problems is as follows:
the preparation method of the 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 benzoyl peroxide solution, maintaining the temperature of a reaction system at 80-90 ℃, reacting for 2-3 hours, intermittently vacuumizing until reactants are semitransparent, and cooling to obtain a base material;
(2) And uniformly stirring the base material, the organotin and the methyltributylketon oxime-based silane, exhausting steam in vacuum, and molding to obtain the organic silicon oxygen-enriched film.
In the scheme, the gutta percha is grafted onto the 107 glue through the methyl methacrylate, so that a three-dimensional cross-linked network is formed by the system, the mechanical properties of the material are 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 is generated after the reaction, and the water is pumped out in a vacuumizing mode, so that the subsequent operation is facilitated; and (3) exhausting gas generated in the raw materials in a vacuum steam exhausting mode after the reaction in the step (2) so as to avoid the influence on the use of the oxygen-enriched membrane due to the existence of air holes in the membrane material after the molding.
Further, in step (1).
Further, the viscosity of the 107 glue is 3500-5000 mPa.s.
Further, the mass concentration of benzoyl peroxide is 25-35%.
Further, the solvent in the benzoyl peroxide solution is ethyl acetate.
Further, in the step (2), the mass ratio of the base material to the organotin to the methyltributyloximoyl silane is 100:0.3-0.5:3-4.
The beneficial effects of the invention are as follows:
according to the invention, the gutta percha is grafted onto the 107 glue through the methyl methacrylate, so that a three-dimensional cross-linked network is formed by the system, the stability of the system is improved, 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, the preparation method comprises the following steps:
(1) Uniformly mixing 107 glue with the viscosity of 3500 mPas, methyl methacrylate and gutta-percha, heating to 55 ℃, dropwise adding a benzoyl peroxide solution with the mass concentration of 25%, 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 gutta-percha is 100:15:3:8;
(2) Uniformly stirring the base material, the organotin and the methyltributyloximoyl 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, the preparation method comprises the following steps:
(1) Uniformly mixing 107 glue with the viscosity of 5000 mPas, methyl methacrylate and gutta-percha, heating to 65 ℃, dropwise adding a benzoyl peroxide solution with the mass concentration of 35%, 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 gutta-percha is 100:25:5:12;
(2) Uniformly stirring the base material, the organotin and the methyltributyloxidoxime 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, the preparation method comprises the following steps:
(1) Uniformly mixing 107 glue with the viscosity of 4000 mPas, 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, 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 gutta-percha is 100:20:4:10;
(2) Uniformly stirring the base material, the organotin and the methyltributyloximoyl 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 oxygen-enriched membranes prepared in examples 1 to 3 were each tested for mechanical properties and oxygen permeability, and the specific test results are shown in Table 1.
Table 1: oxygen enriched membrane performance
As can be seen from the data in the above table, the oxygen enriched membranes of examples 1-3 have higher mechanical properties and higher oxygen permeability than the conventional 107 gel.

Claims (7)

1. The preparation method of the organic silicon oxygen-enriched film is characterized by comprising the following steps of:
(1) Uniformly mixing 107 glue, methyl methacrylate and gutta-percha, heating to 55-65 ℃, dropwise adding benzoyl peroxide solution, maintaining the temperature of a reaction system at 80-90 ℃ for 2-3 hours, intermittently vacuumizing until reactants are semitransparent, and cooling to obtain a base material;
(2) And uniformly stirring the base material, the organotin and the methyltributylketon oxime-based silane, exhausting steam in vacuum, and molding to obtain the organic silicon oxygen-enriched film.
2. The method for preparing the organic silicon oxygen-enriched film according to claim 1, wherein the mass ratio of the 107 glue, the methyl methacrylate, the benzoyl peroxide and the gutta-percha in the step (1) is 100:15-25:3-5:8-12.
3. The method for preparing an oxygen-enriched organosilicon membrane according to claim 1, wherein the viscosity of the 107 glue is 3500-5000mps.
4. The method for producing an oxygen-enriched organosilicon membrane according to claim 1, wherein the mass concentration of benzoyl peroxide is 25 to 35%.
5. The method for producing an oxygen-enriched organosilicon membrane according to claim 1, wherein the solvent in the benzoyl peroxide solution is ethyl acetate.
6. The method for preparing an organic silicon oxygen-enriched film according to claim 1, wherein the mass ratio of the base material, the organotin and the methyltributyloxidoxysilane in the step (2) is 100:0.3-0.5:3-4.
7. An organosilicon oxygen-enriched membrane 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
改性硅橡胶富氧膜的制备;张可达, 刘南安, 田禾;应用化学(第01期);92-94 *

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