CN108704494A - A kind of silicon rubber inierpeneirating network structure polymer penetration vaporization film and preparation method thereof - Google Patents
A kind of silicon rubber inierpeneirating network structure polymer penetration vaporization film and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of silicon rubber inierpeneirating network structure polymer penetration vaporization film and preparation method thereof, it is the product that silicone rubber solution is polymerized with vinyl monomer by in-situ solution；Wherein, silicone rubber solution is made of end hydroxyl silicone oil and alkoxy silane and solvent, and three forms mass ratio and is（1-5）：（0.01-3）：（0-100）.Polymer penetration vaporization film remains silicon rubber hydrophobicity, acid and alkali-resistance, low temperature resistant advantage while improving its mechanical property and separating capacity.
Description
Technical field
The present invention relates to a kind of silicon rubber inierpeneirating network structure polymer penetrations to vaporize film and preparation method thereof, it belongs to high
Molecular chemistry technical field.
Background technology
With the increasingly depleted of petroleum resources, bio-fuel is increasingly valued by people and favors.Bio-ethanol with
Biological butanol is known respectively as the first generation and second generation bio-fuel, can since its raw materials for production is cheap and derives from a wealth of sources
It is renewable and of greatest concern using replacing gasoline as the fuel of internal combustion engine.Till now, fermentation method prepares the technology of ethyl alcohol and butanol
Ripe and large-scale industrialization, however, the concentration of fuel is relatively low to detach in the aqueous solution obtained due to fermentation
Cost is higher so that the application that fermentation method prepares bio-fuel is restricted.
Infiltration evaporation (PV) partition method is a kind of method detaching different component using polymer film, since low energy consumption for it,
It is efficient to be separated from the water one of organic matter most efficient method to become.Pervaporation Technology most critical is its separation
The performance of film, seperation film directly determines the application range and economic value of the technology.The performance for judging seperation film mainly selects two
A parameter, one is separation factor (α characterizes the selectivity of seperation film), and for flux, (J characterizes the processing energy of seperation film for another
Power).And the infiltrating and vaporizing membrane of existing separating butanol and ethyl alcohol mainly has silicone rubber membrane at present, polyurethane film, modified silicon rubber
Film, inoranic membrane, ionic liquid film etc., these films are since its separating capacity is inadequate or cost is excessively high or stability is bad without having
There is corresponding practical value.
Invention content
The technical problem to be solved by the present invention is to provide a kind of silicon rubber in view of the deficiency of the prior art
Inierpeneirating network structure polymer penetration vaporizes film and preparation method thereof, using a certain proportion of end hydroxyl silicone oil with crosslinking agent molten
After reaction prepares silicone rubber solution in agent, then in-situ polymerization obtains interpenetrating networks knot in silicone rubber solution by vinyl monomer
Structure polymer penetration vaporizes film, improves the mechanical property and separating capacity and processing capacity of silicone rubber membrane.
The present invention be solve the problems, such as it is set forth above used by technical solution be：
A kind of silicon rubber inierpeneirating network structure polymer penetration vaporization film, which is silicone rubber solution and ethylene
The product that base monomer is polymerized by in-situ solution；Wherein, silicone rubber solution be by end hydroxyl silicone oil and alkoxy silane and
Solvent forms, and it is (1-5) that three, which forms mass ratio,：(0.01-3)：(0-100).
By said program, it is the integer of 10-10000 that the end hydroxyl silicone oil, which has the following general formula, wherein n,.
By said program, the alkoxy silane is tetraalkoxysilane, alkyltrialkoxysilaneand, three alkane of modified alkyl
One or more of mixture in oxysilane, cycloalkyl alkoxy silane etc..
By said program, the solvent is selected from hexamethylene, n-hexane, pentamethylene, pentane, cycloheptane, normal heptane, just pungent
One or more of mixture in alkane, isooctane benzene,toluene,xylene, petroleum ether etc..
By said program, vinyl monomer is selected from methyl methacrylate, ethyl methacrylate, methacrylic acid third
Ester, isopropyl methacrylate, butyl methacrylate, metering system heptyl heptylate, methyl acrylate, ethyl acrylate, propylene
Propyl propionate, isopropyl acrylate, butyl acrylate, heptylacrylate, methacrylic acid (1-3) fluorine methyl esters, methacrylic acid (1-
5) fluorine ethyl ester, methacrylic acid (1-7) fluorine propyl ester, methacrylic acid (1-7) fluorine isopropyl ester, methacrylic acid (1-9) fluorine butyl ester,
Methacrylic acid (1-15) fluorine heptyl ester, acrylic acid (1-3) fluorine methyl esters, acrylic acid (1-5) fluorine ethyl ester, acrylic acid (1-7) fluorine propyl ester,
Acrylic acid (1-7) fluorine isopropyl ester, acrylic acid (1-9) fluorine butyl ester, acrylic acid (1-15) fluorine heptyl ester, styrene, divinylbenzene and
One or more of mixtures of p-methylstyrene etc..(note：Number in bracket represents fluorine-substituted number, such as methyl
Methyl acrylate, fluorine can replace 1-3 hydrogen.)
The preparation method of silicon rubber inierpeneirating network structure polymer penetration vaporization film of the present invention, main includes two
Step：The first step is reacted by end hydroxyl silicone oil with crosslinking agent alkoxy silane and forms silicone rubber solution in a solvent；Second step,
Vinyl monomer in-situ polymerization in silicone rubber solution forms silicon rubber inierpeneirating network structure polymer penetration and vaporizes film.
By said program, the more specific technique of the preparation method first step is：Hydroxyl-terminated injecting two methyl siloxane and crosslinking agent
Alkoxy silane carries out cross-linking reaction under the catalytic action of catalyst, obtains silastic polymer solution, reaction temperature 30-80
DEG C, in reaction time 2-6 hour, it is down to room temperature after reaction, obtains silastic polymer solution.
By said program, the mass percentage of the reaction each component involved in the first step is as follows：End hydroxyl silicone oil 10-
40%, crosslinking agent alkoxy silane 1-10%, catalyst 0.1-2%, solvent 48-89%.Wherein, catalyst is dibutyl tin
The mixture of one or more of cinnamic acid tin, dibutyl disuccinic acid tin, iron chloride, aluminium chloride, titanium tetrachloride etc.；Solvent selects
From hexamethylene, n-hexane, pentamethylene, pentane, cycloheptane, normal heptane, normal octane, isooctane benzene,toluene,xylene, oil
The mixture of one or more of ether etc.；
By said program, the more specific technique of preparation method second step is：By silastic polymer solution obtained by the first step
Polymerisation is carried out after being mixed with vinyl monomer, solvent, initiator, reaction temperature is 65-95 DEG C, and the reaction time is that 2-6 is small
When, acquired solution is placed on counterdie and spontaneously dries to get to silicon rubber inierpeneirating network structure polymer penetration vapour after reaction
Change film.
By said program, the mass percentage of the reaction each component involved in second step is as follows：Silastic polymer is molten
Liquid 10-50%, vinyl monomer 0.2-10%, initiator 0.1-1%, solvent 39-89.7%.Wherein, initiator is selected from peroxide
Benzoyl, azodiisobutyronitrile, hydrogen peroxide, potassium peroxydisulfate, n-BuLi, boron trifluoride, anhydrous Aluminum chloride, anhydrous ferric chloride
Deng one or more of mixture；Solvent is selected from hexamethylene, n-hexane, pentamethylene, pentane, cycloheptane, normal heptane, just pungent
Alkane, isooctane benzene,toluene,xylene, petroleum ether, methanol, ethyl alcohol, isopropanol, normal propyl alcohol, n-butanol, tetrahydrofuran, ether,
The mixture of one or more of dimethyl ether, n-butyl ether etc..
The thickness of silicon rubber inierpeneirating network structure polymer penetration vaporization film of the present invention can be used in 2-200 μ ms
Methanol in a certain concentration (0.2wt.%-30wt.%) range detached in water, ethyl alcohol, propyl alcohol, isopropanol, n-butanol etc.
The application of organic matter.
Compared with prior art, the beneficial effects of the invention are as follows：
First, the present invention improves mechanical property and the separation of silicone rubber membrane by forming inierpeneirating network structure polymer
Ability and processing capacity, have it is at low cost, stability is good, and mechanical strength is good, and heat resistance, stain resistance, creep resistance are good, point
It is strong from ability, the high advantage of processing capacity；
Second, silicon rubber inierpeneirating network structure polymer penetration of the invention vaporization film can be used in detaching certain in water
The organic matters such as methanol, ethyl alcohol, propyl alcohol, isopropanol, n-butanol in concentration range, separating capacity and processing capacity are strong, cost
Low, stability is good, has broad application prospects.
Description of the drawings
Fig. 1 is the formation schematic diagram of inierpeneirating network structure, by taking PDMS and polymethyl acrylate as an example.
Specific implementation mode
The present invention is further illustrated by following unrestricted embodiment, but it should be understood that the embodiment is only used
With the present invention, rather than to limit the scope of the invention.
In the following embodiments of the present invention gained silicon rubber interpenetrating networks are measured according to the method described in GB/T 1701-2001
Mechanical property and separating capacity of structural polymer infiltrating and vaporizing membrane etc..
Polymer penetration vaporizes the measurement of the water resistance of film：The film of certain thickness, area is first made, then 50 DEG C in constant temperature
Case is dried, until after constant weight, is impregnated in 25 DEG C of water for 24 hours, is blotted film surface droplet with filter paper, claim quality.
Water absorption rate=(wet film quality-dry film quality)/dry film quality × 100%, glued membrane water absorption rate is smaller, and water resistance is got over
It is good.
Infrared detection：By polymeric articles in AVATAR 360FT-IR infrared spectrums spectrometer (Nicolet companies of the U.S.)
It is characterized.
The detection of infiltration evaporation effect：It is equipped using infiltration evaporation, selects different feed liquid concentration (with mass concentration respectively
Meter) ethyl alcohol, butanol aqueous solution carry out infiltration evaporation experiment at different temperature, under this condition the selective factor B (α) of film and
Flux (J) calculates according to the following formula respectively：
Wherein, XpWith XfMass fraction of the expression alcohols (ethyl alcohol, butanol) in diffusate and feed liquid respectively, and YpWith Yf
Mass fraction of the water in feed liquid and diffusate is indicated respectively.mpFor diffusate quality, S and t indicate effective area and reality respectively
Test the time.
Embodiment 1
A kind of preparation method of silicon rubber inierpeneirating network structure polymer penetration vaporization film, is as follows：
The first step prepares silicone rubber solution：End hydroxyl silicone oil PDMS (Mn=10000) is added in 250mL four-hole boiling flasks
50g, crosslinking agent tetraethoxysilane 1.0g, catalyst dibutyl tin dilaurate 10g, solvent dry toluene 200g, then 80
Silicone rubber solution is obtained after DEG C being heated to reflux 3h；
Second step prepares interpenetrating net polymer film：50g silicone rubber solutions are taken, 20g methyl acrylates, 0.2g mistakes is added
Oxygen benzoyl, 50g dry toluenes after 90 DEG C are heated at reflux 3h, obtain silicon rubber inierpeneirating network structure polymer solution；
Third walks, and 5mL second steps acquired solution is taken to prepare infiltrating and vaporizing membrane on PAN counterdies；Separately take 20mL second steps institute
It obtains solution solidification on tetrafluoroethene plate and prepares polymeric film, to detect infrared and water absorption rate.
Embodiment 2
A kind of preparation method of silicon rubber inierpeneirating network structure polymer penetration vaporization film, is as follows：
The first step prepares silicone rubber solution：End hydroxyl silicone oil PDMS (Mn=4000) is added in 250mL four-hole boiling flasks
50g, crosslinking agent methyltriethoxysilane 1.0g, catalyst dibutyl tin dilaurate 10g, solvent dry toluene 200g, 80
Also silicone rubber solution is obtained after DEG C being heated to reflux 3h；
Second step, takes 50g silicone rubber solutions, is added 20g styrene, 0.2g benzoyl peroxides, 50g dry toluenes, 90 DEG C
After being heated at reflux 3h, silicon rubber inierpeneirating network structure polymer solution is obtained；
Third walks, and 5mL second steps acquired solution is taken to prepare infiltrating and vaporizing membrane on PAN counterdies；Separately take 20mL second steps institute
It obtains solution solidification on tetrafluoroethene plate and prepares polymeric film.
Embodiment 3
A kind of preparation method of silicon rubber inierpeneirating network structure polymer penetration vaporization film, is as follows：
The first step prepares silicone rubber solution：End hydroxyl silicone oil PDMS (Mn=50000) is added in 250mL four-hole boiling flasks
50g, crosslinking agent tetraethoxysilane 0.1g, catalyst dibutyl tin dilaurate 1g, solvent dry toluene 800g, 80 DEG C of heating
Silicone rubber solution is obtained after reflux 2h；
Second step, takes 50g silicone rubber solutions, is added 2g methyl methacrylates, 0.2g azodiisobutyronitriles, and 100g is anhydrous
Toluene after 90 DEG C are heated at reflux 6h, obtains silicon rubber inierpeneirating network structure polymer solution；
Third walks, and 5mL second steps acquired solution is taken to prepare infiltrating and vaporizing membrane on PAN counterdies；Separately take 20mL second steps institute
It obtains solution solidification on tetrafluoroethene plate and prepares polymeric film.
Embodiment 4
A kind of preparation method of silicon rubber inierpeneirating network structure polymer penetration vaporization film, is as follows：
The first step prepares silicone rubber solution：End hydroxyl silicone oil PDMS (Mn=100000) is added in 250mL four-hole boiling flasks
50g, crosslinking agent vinyltriethoxysilane 0.5g, catalyst dibutyl tin dilaurate 5g, solvent dry toluene 400g, 80
Silicone rubber solution is obtained after DEG C being heated to reflux 4h；
Second step prepares interpenetrating net polymer film：50g silicone rubber solutions are taken, 10g butyl acrylates are added, 0.2g is even
Nitrogen bis-isobutyronitrile, 50g normal heptanes after 90 DEG C are heated at reflux 6h, obtain silicon rubber inierpeneirating network structure polymer solution；
Third walks, and 5mL second steps acquired solution is taken to prepare infiltrating and vaporizing membrane on PAN counterdies；Separately take 20mL second steps institute
It obtains solution solidification on tetrafluoroethene plate and prepares polymeric film.
Embodiment 5
A kind of preparation method of silicon rubber inierpeneirating network structure polymer penetration vaporization film, is as follows：
The first step prepares silicone rubber solution：End hydroxyl silicone oil PDMS (Mn=10000) is added in 250mL four-hole boiling flasks
50g, crosslinking agent aminopropyl triethoxysilane 1g, catalyst dibutyl tin dilaurate 1g, solvent benzol 400g, 90 DEG C are heated back
Silicone rubber solution is obtained after stream 4h；
Second step prepares interpenetrating net polymer film：50g silicone rubber solutions are taken, 5g methacrylic acid perfluor ethyl esters are added,
0.2g benzoyl peroxides, 50g petroleum ethers after 75 DEG C are heated at reflux 5h, obtain silicon rubber inierpeneirating network structure polymer solution；
Third walks, and 5mL second steps acquired solution is taken to prepare infiltrating and vaporizing membrane on PAN counterdies；Separately take 20mL second steps institute
It obtains solution solidification on tetrafluoroethene plate and prepares polymeric film.
The performance for the polymer film that embodiment 1-5 is obtained is as shown in table 1；Film obtained by embodiment 1-5 is through infrared and water suction
Rate detects, and proves to obtain target product, water absorption rate is between 0.2%-0.4%.
Table 1
From table 1 it follows that obtained interpenetrating networks result film has good mechanical property, meanwhile, with good
The processing capacity that good separating capacity has had simultaneously.
The above is only a preferred embodiment of the present invention, it is noted that come for those of ordinary skill in the art
It says, without departing from the concept of the premise of the invention, several modifications and variations can also be made, these belong to the present invention's
Protection domain.
Claims (10)
1. a kind of silicon rubber inierpeneirating network structure polymer penetration vaporizes film, it is characterised in that it is silicone rubber solution and contains double
The product that the monomer of key is polymerized by in-situ solution；Wherein, silicone rubber solution is by end hydroxyl silicone oil and alkoxy silane
It is formed with solvent, three forms mass ratio and is（1-5）：（0.01-3）：（0-100）.
2. a kind of silicon rubber inierpeneirating network structure polymer penetration according to claim 1 vaporizes film, it is characterised in that it
Thickness in 2-200 μ ms.
3. silicon rubber inierpeneirating network structure polymer penetration vaporization film described in claim 1 is used to detach the organic matter in water
Using.
4. a kind of silicon rubber inierpeneirating network structure polymer penetration according to claim 1 vaporizes film, it is characterised in that institute
It is tetraalkoxysilane, alkyltrialkoxysilaneand, modified alkyl trialkoxy silane, cycloalkyl alkoxy to state alkoxy silane
The mixture of one or more of silane；The solvent is selected from hexamethylene, n-hexane, pentamethylene, pentane, cycloheptane, just
The mixture of one or more of heptane, normal octane, isooctane benzene,toluene,xylene, petroleum ether.
5. a kind of silicon rubber inierpeneirating network structure polymer penetration according to claim 1 vaporizes film, it is characterised in that contain
It is vinyl monomer to have the monomer of double bond, is selected from methyl methacrylate, ethyl methacrylate, propyl methacrylate, first
Base isopropyl acrylate, butyl methacrylate, metering system heptyl heptylate, methyl acrylate, ethyl acrylate, acrylic acid third
Ester, isopropyl acrylate, butyl acrylate, heptylacrylate, methacrylic acid（1-3）Fluorine methyl esters, methacrylic acid（1-5）Fluorine
Ethyl ester, methacrylic acid（1-7）Fluorine propyl ester, methacrylic acid（1-7）Fluorine isopropyl ester, methacrylic acid（1-9）Fluorine butyl ester, methyl
Acrylic acid（1-15）Fluorine heptyl ester, acrylic acid（1-3）Fluorine methyl esters, acrylic acid（1-5）Fluorine ethyl ester, acrylic acid（1-7）Fluorine propyl ester, propylene
Acid（1-7）Fluorine isopropyl ester, acrylic acid（1-9）Fluorine butyl ester, acrylic acid（1-15）Fluorine heptyl ester, styrene, divinylbenzene and to first
The mixture of one or more of base styrene.
6. a kind of preparation method of silicon rubber inierpeneirating network structure polymer penetration vaporization film, it is characterised in that main includes two
Step：The first step is reacted by end hydroxyl silicone oil with alkoxy silane and forms silicone rubber solution in a solvent；Second step, vinyl
Monomer in-situ polymerization in silicone rubber solution forms silicon rubber inierpeneirating network structure polymer penetration and vaporizes film.
7. a kind of preparation method of silicon rubber inierpeneirating network structure polymer penetration vaporization film according to claim 6,
It is characterized in that the concrete technology of the first step is：The catalytic action of hydroxyl-terminated injecting two methyl siloxane and alkoxy silane in catalyst
Lower carry out cross-linking reaction, obtains silastic polymer solution, 30-80 DEG C of reaction temperature, in reaction time 2-6 hour, reaction terminates
After be down to room temperature, obtain silastic polymer solution.
8. a kind of preparation method of silicon rubber inierpeneirating network structure polymer penetration vaporization film according to claim 6,
It is characterized in that the mass percentage of the reaction each component involved in the first step is as follows：End hydroxyl silicone oil 10-40 %, alkoxyl silicone
Alkane 1-10 %, catalyst 0.1-2 %, solvent 48-89 %.
9. a kind of preparation method of silicon rubber inierpeneirating network structure polymer penetration vaporization film according to claim 6,
It is characterized in that the concrete technology of second step is：By silastic polymer solution obtained by the first step and vinyl monomer, solvent, initiation
Polymerisation is carried out after agent mixing, reaction temperature is 65-95 DEG C, and the reaction time is 2-6 hours, after reaction acquired solution
It is placed in spontaneously dry on counterdie and vaporizes film to get to silicon rubber inierpeneirating network structure polymer penetration.
10. a kind of preparation method of silicon rubber inierpeneirating network structure polymer penetration vaporization film according to claim 6,
It is characterized in that the mass percentage of the reaction each component involved in second step is as follows：Silastic polymer solution 10-50 %, second
Alkenyl monomer 0.2-10 %, initiator 0.1-1 %, solvent 39-89.7 %.
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| CN109847601A (en) * | 2019-03-06 | 2019-06-07 | 常州大学 | A kind of preparation method and application of fluosilicic hydridization copolymer membrane |
| CN110591373A (en) * | 2019-08-22 | 2019-12-20 | 四川塔牌电缆绕组线有限责任公司 | Fireproof flame-retardant cable and manufacturing method thereof |
| CN110935199A (en) * | 2019-11-26 | 2020-03-31 | 广东省测试分析研究所（中国广州分析测试中心） | Organosilicon foam with interpenetrating network pH responsiveness |
| CN114425246A (en) * | 2020-09-28 | 2022-05-03 | 中国石油化工股份有限公司 | Ionic liquid supported composite membrane and preparation method and application thereof |
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| CN114425246A (en) * | 2020-09-28 | 2022-05-03 | 中国石油化工股份有限公司 | Ionic liquid supported composite membrane and preparation method and application thereof |
| CN114425246B (en) * | 2020-09-28 | 2023-04-11 | 中国石油化工股份有限公司 | Ionic liquid supported composite membrane and preparation method and application thereof |
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Application publication date: 20181026 |