CN113637281B - Organic silicon oxygen-enriched membrane and preparation method thereof - Google Patents
Organic silicon oxygen-enriched membrane and preparation method thereof Download PDFInfo
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- 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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- organic silicon
- silicon oxygen
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- 239000012528 membrane Substances 0.000 title claims abstract description 20
- OBNDGIHQAIXEAO-UHFFFAOYSA-N [O].[Si] Chemical compound [O].[Si] OBNDGIHQAIXEAO-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000000463 material Substances 0.000 claims abstract description 18
- 239000001301 oxygen Substances 0.000 claims abstract description 18
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 18
- 239000004342 Benzoyl peroxide Substances 0.000 claims abstract description 14
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims abstract description 14
- 235000019400 benzoyl peroxide Nutrition 0.000 claims abstract description 14
- 239000003292 glue Substances 0.000 claims abstract description 14
- 239000000899 Gutta-Percha Substances 0.000 claims abstract description 12
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims abstract description 12
- 240000000342 Palaquium gutta Species 0.000 claims abstract description 12
- 229920000588 gutta-percha Polymers 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000000465 moulding Methods 0.000 claims abstract description 7
- 229910000077 silane Inorganic materials 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 239000000376 reactant Substances 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 150000002923 oximes Chemical class 0.000 claims abstract description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims 3
- 230000007547 defect Effects 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 229920001577 copolymer Polymers 0.000 description 3
- 238000007599 discharging Methods 0.000 description 3
- 230000035699 permeability Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229920001558 organosilicon polymer Polymers 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229920000578 graft copolymer Polymers 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F253/00—Macromolecular compounds obtained by polymerising monomers on to natural rubbers or derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/12—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2351/00—Characterised 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
- C08J2351/08—Characterised 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2451/00—Characterised 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
- C08J2451/04—Characterised 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/54—Silicon-containing compounds
- C08K5/544—Silicon-containing compounds containing nitrogen
- C08K5/5465—Silicon-containing compounds containing nitrogen containing at least one C=N bond
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Manufacture Of Macromolecular Shaped Articles (AREA)
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
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.
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CN202110978030.XA CN113637281B (en) | 2021-08-23 | 2021-08-23 | Organic silicon oxygen-enriched membrane and preparation method thereof |
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CN113637281B true CN113637281B (en) | 2023-12-26 |
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Non-Patent Citations (1)
Title |
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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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