CN105879720A - Preparation method of heat and chemical cross-linked hyperbranched polysiloxane pervaporation membrane - Google Patents
Preparation method of heat and chemical cross-linked hyperbranched polysiloxane pervaporation membrane Download PDFInfo
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- CN105879720A CN105879720A CN201410784363.9A CN201410784363A CN105879720A CN 105879720 A CN105879720 A CN 105879720A CN 201410784363 A CN201410784363 A CN 201410784363A CN 105879720 A CN105879720 A CN 105879720A
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Abstract
The invention belongs to the field of preparation of a pervaporation separation membrane and particularly relates to a preparation method of a heat and chemical cross-linked hyperbranched polysiloxane pervaporation membrane. The preparation method of the membrane comprises the following process steps: (1) preparing a membrane casting material liquid: taking hyperbranched polysiloxane, n-hexane, glue 107 and dibutyltin dilaurate at 60-80 DEG C for 12h to form the membrane casting material liquid; and (2) carrying out cross-linking to obtain the hyperbranched polysiloxane pervaporation membrane: adding a cross-linking agent into the membrane casting material solution and reacting at 60 DEG C for 2h, carrying out ultrasonic treatment on the mixed membrane casting material solution for 10 minutes and putting the mixed membrane casting material solution on a polytetrafluoroethylene bottom die, standing in the air and vulcanizing for 2h, then converting the solution into an air blowing drying box, and drying at 80 DEG C for 12h to prepare the hyperbranched polysiloxane pervaporation membrane. According to the hyperbranched polysiloxane pervaporation membrane prepared by the preparation method, ethoxyl on the hyperbranched polysiloxane is cross-linked with terminal hydroxyl of the glue 107, and meanwhile, a carbon-carbon double bond on the hyperbranched polysiloxane is cross-linked with the cross-linking agent to form a hyperbranched crossly-linked network structure, so that the mechanical strength of the membrane is improved to a certain extent; and meanwhile, the hyperbranched polysiloxane membrane is relatively hydrophobic, and butanol can be more easily separated by pervaporation.
Description
Technical field
The invention belongs to infiltration vaporization separation film preparation field, particularly relate to the infiltration of one the most crosslinked hyperbranched polysiloxanes
The preparation method of vaporization film.
Background technology
The day by day exhausted and serious pollution of Fossil fuel has expedited the emergence of the research and development of bio-fuel, and wherein biological butanol is considered as
The second filial generation bioenergy that performance is more excellent.But during fermentation method prepares biological butanol, there is the most serious butanol to bacterium
The inhibitory action planted, makes sweat not to be carried out continuously, it is therefore desirable to be separated from fermentation liquid by butanol in time.Infiltration evaporation
Process is considered as the liquid mixture separation process of most promising low energy consumption, high separating efficiency.Some hydrophobic membrane materials
By successively for separating the developmental research of butanol in water.
The fine and close selection that osmosis vaporizing compound membrane is typically one layer thin is placed on one layer of stable support layer of porous mechanical, it is allowed to ooze
Thoroughly under certain pressure reduction, there is high flux and selectivity in vaporescence.In the evolution of high flux membrane, more grind
Study carefully and tend to change membrane structure to form the asymmetric or dense film of composite construction.But, the decline of film thickness is often accompanied
Along with film optionally reduces, this is to create substantial amounts of defect owing to the reduction of film thickness result in film surface, it is impossible to form table
Face zero defect dense film.Therefore, the reason limiting film thickness is many, generally comprises the support aperture of tunic, pore size distribution
And the degree of roughness on surface.
Dissaving polymer is a kind of new polymers with unique topological structure, has that structure height is branched, surface functional group
Density is high, chemical stability good, surface-functionalized simple, be prone to the features such as film forming.The more important thing is, hyperbranched poly
Compound has bigger free volume, and molecular structure is of a relatively loose.Three-dimensional molecular structure special for dissaving polymer is introduced
Inside the stratum disjunctum of polysiloxanes infiltrating and vaporizing membrane, the flux of film is significantly increased, but its separation factor is the highest.
Summary of the invention
It is an object of the invention to provide a kind of hyperbranched polyorganosiloxane infiltrating and vaporizing membrane for being separated from the water butanol, to overcome
The defect of prior art.
The preparation method of the most crosslinked hyperbranched polysiloxanes infiltrating and vaporizing membrane that the present invention provides, it is characterised in that include as
Lower step:
A is by hyperbranched polyorganosiloxane 1.5-2 part, normal hexane 86-89 part, 107 glue 7.5-10 parts, dibutyl tin dilaurate 0.5-1.0
After part reacts 12h at 60～80 DEG C, form casting film feed liquid；
B adds the cross-linking agent of 0.2-1.2 part in described casting film feed liquid and reacts 2h at 60 DEG C, by the mixed ultrasonic place of casting film feed liquid
Manage and within 10 minutes, be placed on Kynoar bed die, stand and air vulcanizes 2h, then proceed to air dry oven and be dried in 80 DEG C
12h, obtains hyperbranched polyorganosiloxane infiltrating and vaporizing membrane.
Preferably, the degree of branching of described hyperbranched polyorganosiloxane is 0.70,0.75,0.80.
Preferably, the viscosity of described 107 glue be 1000cs, 10,000 cs, 1,000,000 cs.
Preferably, described cross-linking agent is 1,6-hexanediyl ester, Ethylene glycol dimethacrylate or divinylbenzene.
The present invention also proposes one the most crosslinked hyperbranched polysiloxanes infiltrating and vaporizing membrane, it is characterised in that formula includes as follows
Component: hyperbranched polyorganosiloxane 1.5-2 part, normal hexane 86-89 part, 107 glue 7.5-10 parts, dibutyl tin dilaurate 0.5-1.0
Part, cross-linking agent 0.2-1.2 part.
Preferably, the degree of branching of described hyperbranched polyorganosiloxane is 0.70,0.75,0.80.
Preferably, the viscosity of described 107 glue be 1000cs, 10,000 cs, 1,000,000 cs.
Preferably, described cross-linking agent is 1,6-hexanediyl ester, Ethylene glycol dimethacrylate or divinylbenzene.
The hyperbranched polyorganosiloxane infiltrating and vaporizing membrane that the present invention provides, by the carbon-carbon double bond on crosslinked hyperbranched polysiloxanes to reach
To cross-linking modified purpose.Ethyoxyl on hyperbranched polyorganosiloxane and the terminal hydroxy group chemical crosslinking of 107 glue, hyperbranched poly subsequently
Carbon-carbon double bond on siloxanes and cross-linking agent carry out heat cross-linking, form superhigh cross-linking network structure, improve film to a certain extent
Mechanical strength, make hyperbranched polyorganosiloxane film more hydrophobic containing the introducing of double bond cross-linking agent simultaneously, be more beneficial for permeating vapour
Change separating butanol.
In sum, the preparation method of the most crosslinked hyperbranched polysiloxanes infiltrating and vaporizing membrane of the present invention, have following excellent
Point:
1, the present invention uses thermal curing method, and polymerization efficiency is high, and technique is simple, easy to operate, produces reproducible.
2, the present invention uses the hyperbranched polyorganosiloxane infiltrating and vaporizing membrane of multiple cross-linked formation superhigh cross-linking network structure, itself stability
Well, physical arrangement is stable, and the hydrophobicity of film is greatly promoted.
3, hyperbranched polyorganosiloxane infiltrating and vaporizing membrane prepared by the inventive method is used, due to the freedom that modified hyperbranched holding is bigger
Volume, molecular structure is of a relatively loose, good to the permeance property of butanol, and its separation factor is high.
Detailed description of the invention:
The following is the embodiment of the most crosslinked hyperbranched polysiloxanes infiltration evaporation membrane preparation method, but described embodiment not structure
Become limitation of the present invention.
Embodiment 1:
1) casting film feed liquid is prepared:
By 0.70 degree of branching hyperbranched polyorganosiloxane 1.5 parts, normal hexane 86 parts, 7.5 parts of 1000cs viscosity 107 glue, dibutyl
After 0.5 part of tin dilaurate stannum reacts 12h at 60～80 DEG C, form casting film feed liquid；
2) hyperbranched polyorganosiloxane infiltrating and vaporizing membrane is cross-linked to obtain:
Adding the 1 of 0.2 part in described casting film feed liquid, 6-hexanediyl ester reacts 2h at 60 DEG C, by mixed casting
Coating materials liquid supersound process is placed on Kynoar bed die for 10 minutes, stands and vulcanizes 2h in air, then proceeds to forced air drying
Case, in 80 DEG C of dry 12h, obtains hyperbranched polyorganosiloxane infiltrating and vaporizing membrane.
Above-mentioned hyperbranched polyorganosiloxane film is used for n-butyl alcohol in infiltration evaporation separation water, and its infiltration evaporation result is: permeation flux
For 753.12g/m2H, its separation factor is 43.7.
Embodiment 2:
1) casting film feed liquid is prepared:
By 0.70 degree of branching hyperbranched polyorganosiloxane 2 parts, normal hexane 89 parts, 10 parts of 1000cs viscosity 107 glue, dibutyl two
After tin laurate 1.0 parts reacts 12h at 60～80 DEG C, form casting film feed liquid；
2) hyperbranched polyorganosiloxane infiltrating and vaporizing membrane is cross-linked to obtain:
Adding the 1 of 0.2 part in described casting film feed liquid, 6-hexanediyl ester reacts 2h at 60 DEG C, by mixed casting
Coating materials liquid supersound process is placed on Kynoar bed die for 10 minutes, stands and vulcanizes 2h in air, then proceeds to forced air drying
Case, in 80 DEG C of dry 12h, obtains hyperbranched polyorganosiloxane infiltrating and vaporizing membrane.
Above-mentioned hyperbranched polyorganosiloxane film is used for n-butyl alcohol in infiltration evaporation separation water, and its infiltration evaporation result is: permeation flux
For 749.02g/m2H, its separation factor is 44.5.
Embodiment 3:
1) casting film feed liquid is prepared:
By 0.75 degree of branching hyperbranched polyorganosiloxane 1.5 parts, normal hexane 88 parts, 10,000 7.5 parts of cs viscosity 107 glue, dibutyl
After 0.5 part of tin dilaurate stannum reacts 12h at 60～80 DEG C, form casting film feed liquid；
2) hyperbranched polyorganosiloxane infiltrating and vaporizing membrane is cross-linked to obtain:
Adding the 1 of 0.4 part in described casting film feed liquid, 6-hexanediyl ester reacts 2h at 60 DEG C, by mixed casting
Coating materials liquid supersound process is placed on Kynoar bed die for 10 minutes, stands and vulcanizes 2h in air, then proceeds to forced air drying
Case, in 80 DEG C of dry 12h, obtains hyperbranched polyorganosiloxane infiltrating and vaporizing membrane.
Above-mentioned hyperbranched polyorganosiloxane film is used for n-butyl alcohol in infiltration evaporation separation water, and its infiltration evaporation result is: permeation flux
For 744.10g/m2H, its separation factor is 40.7.
Embodiment 4:
1) casting film feed liquid is prepared:
By 0.80 degree of branching hyperbranched polyorganosiloxane 2 parts, normal hexane 89 parts, 10,000 10 parts of cs viscosity 107 glue, dibutyl two
After tin laurate 1.0 parts reacts 12h at 60～80 DEG C, form casting film feed liquid；
2) hyperbranched polyorganosiloxane infiltrating and vaporizing membrane is cross-linked to obtain:
The Ethylene glycol dimethacrylate adding 0.5 part in described casting film feed liquid reacts 2h, by mixed casting film at 60 DEG C
Feed liquid supersound process is placed on Kynoar bed die for 10 minutes, stands and vulcanizes 2h in air, then proceeds to air dry oven
In 80 DEG C of dry 12h, obtain hyperbranched polyorganosiloxane infiltrating and vaporizing membrane.
Above-mentioned hyperbranched polyorganosiloxane film is used for n-butyl alcohol in infiltration evaporation separation water, and its infiltration evaporation result is: permeation flux
For 740.53g/m2H, its separation factor is 40.1.
Embodiment 5:
1) casting film feed liquid is prepared:
By 0.80 degree of branching hyperbranched polyorganosiloxane 1.8 parts, normal hexane 88 parts, 1,000,000 9 parts of cs viscosity 107 glue, dibutyl
After 0.5 part of tin dilaurate stannum reacts 12h at 60～80 DEG C, form casting film feed liquid；
2) hyperbranched polyorganosiloxane infiltrating and vaporizing membrane is cross-linked to obtain:
Adding the 1 of 1.1 parts in described casting film feed liquid, 6-hexanediyl ester reacts 2h at 60 DEG C, by mixed casting
Coating materials liquid supersound process is placed on Kynoar bed die for 10 minutes, stands and vulcanizes 2h in air, then proceeds to forced air drying
Case, in 80 DEG C of dry 12h, obtains hyperbranched polyorganosiloxane infiltrating and vaporizing membrane.
Above-mentioned hyperbranched polyorganosiloxane film is used for n-butyl alcohol in infiltration evaporation separation water, and its infiltration evaporation result is: permeation flux
For 632.55g/m2H, its separation factor is 46.8.
Embodiment 6:
1) casting film feed liquid is prepared:
By 0.80 degree of branching hyperbranched polyorganosiloxane 2 parts, normal hexane 89 parts, 10,000 8.8 parts of cs viscosity 107 glue, dibutyl two
After tin laurate 0.75 part reacts 12h at 60～80 DEG C, form casting film feed liquid；
2) hyperbranched polyorganosiloxane infiltrating and vaporizing membrane is cross-linked to obtain:
The Ethylene glycol dimethacrylate adding 1.2 parts in described casting film feed liquid reacts 2h, by mixed casting at 60 DEG C
Coating materials liquid supersound process is placed on Kynoar bed die for 10 minutes, stands and vulcanizes 2h in air, then proceeds to forced air drying
Case, in 80 DEG C of dry 12h, obtains hyperbranched polyorganosiloxane infiltrating and vaporizing membrane.
Above-mentioned hyperbranched polyorganosiloxane film is used for n-butyl alcohol in infiltration evaporation separation water, and its infiltration evaporation result is: permeation flux
For 667.34g/m2H, its separation factor is 51.4.
Embodiment 7:
1) casting film feed liquid is prepared:
By 0.80 degree of branching hyperbranched polyorganosiloxane 1.5 parts, normal hexane 86 parts, 10 parts of 1000cs viscosity 107 glue, dibutyl
After 0.75 part of tin dilaurate stannum reacts 12h at 60～80 DEG C, form casting film feed liquid；
2) hyperbranched polyorganosiloxane infiltrating and vaporizing membrane is cross-linked to obtain:
The divinylbenzene adding 0.2 part in described casting film feed liquid reacts 2h, by ultrasonic for mixed casting film feed liquid at 60 DEG C
Process and within 10 minutes, be placed on Kynoar bed die, stand and air vulcanizes 2h, then proceed to air dry oven and do in 80 DEG C
Dry 12h, obtains hyperbranched polyorganosiloxane infiltrating and vaporizing membrane.
Above-mentioned hyperbranched polyorganosiloxane film is used for n-butyl alcohol in infiltration evaporation separation water, and its infiltration evaporation result is: permeation flux
For 715.07g/m2H, its separation factor is 45.3.
Embodiment 8:
1) casting film feed liquid is prepared:
By 0.75 degree of branching hyperbranched polyorganosiloxane 1.6 parts, normal hexane 87 parts, 10,000 8.0 parts of cs viscosity 107 glue, dibutyl
After 0.75 part of tin dilaurate stannum reacts 12h at 60～80 DEG C, form casting film feed liquid；
2) hyperbranched polyorganosiloxane infiltrating and vaporizing membrane is cross-linked to obtain:
The divinylbenzene adding 0.6 part in described casting film feed liquid reacts 2h, by ultrasonic for mixed casting film feed liquid at 60 DEG C
Process and within 10 minutes, be placed on Kynoar bed die, stand and air vulcanizes 2h, then proceed to air dry oven and do in 80 DEG C
Dry 12h, obtains hyperbranched polyorganosiloxane infiltrating and vaporizing membrane.
Above-mentioned hyperbranched polyorganosiloxane film is used for n-butyl alcohol in infiltration evaporation separation water, and its infiltration evaporation result is: permeation flux
For 731.08g/m2H, its separation factor is 40.5.
Embodiment 9:
1) casting film feed liquid is prepared:
By 0.70 degree of branching hyperbranched polyorganosiloxane 2 parts, normal hexane 86 parts, 1,000,000 10 parts of cs viscosity 107 glue, dibutyl
After 1.0 parts of tin dilaurate stannum reacts 12h at 60～80 DEG C, form casting film feed liquid；
2) hyperbranched polyorganosiloxane infiltrating and vaporizing membrane is cross-linked to obtain:
The divinylbenzene adding 1.2 parts in described casting film feed liquid reacts 2h, by ultrasonic for mixed casting film feed liquid at 60 DEG C
Process and within 10 minutes, be placed on Kynoar bed die, stand and air vulcanizes 2h, then proceed to air dry oven and do in 80 DEG C
Dry 12h, obtains hyperbranched polyorganosiloxane infiltrating and vaporizing membrane.
Above-mentioned hyperbranched polyorganosiloxane film is used for n-butyl alcohol in infiltration evaporation separation water, and its infiltration evaporation result is: permeation flux
For 654.74g/m2H, its separation factor is 48.6.
The description of above-described embodiment should be considered explanation, it is easy to is understood by, can be without departing from illustrating the most in detail in the claims
The present invention in the case of use many changes and the combination of feature described above, this kind of change has been not to be regarded as a departure from this
Bright spirit and scope, and all such change be included in the range of claims below.
Claims (8)
1. the preparation method of the most crosslinked hyperbranched polysiloxanes infiltrating and vaporizing membrane, it is characterised in that comprise the steps:
A is by hyperbranched polyorganosiloxane 1.5-2 part, normal hexane 86-89 part, 107 glue 7.5-10 parts, dibutyl tin dilaurate 0.5-1.0
After part reacts 12h at 60～80 DEG C, form casting film feed liquid；
B adds the cross-linking agent of 0.2-1.2 part in described casting film feed liquid and reacts 2h at 60 DEG C, by the mixed ultrasonic place of casting film feed liquid
Manage and within 10 minutes, be placed on Kynoar bed die, stand and air vulcanizes 2h, then proceed to air dry oven and be dried in 80 DEG C
12h, obtains hyperbranched polyorganosiloxane infiltrating and vaporizing membrane.
The preparation method of the most crosslinked hyperbranched polysiloxanes infiltrating and vaporizing membrane, it is characterised in that
The degree of branching of described hyperbranched polyorganosiloxane is 0.70,0.75,0.80.
3. according to the preparation method of polysiloxanes infiltrating and vaporizing membrane the most crosslinked hyperbranched described in claim 1-2, it is characterised in that
The viscosity of described 107 glue is 1000cs, 10,000 cs, 1,000,000 cs.
4. according to the preparation method of polysiloxanes infiltrating and vaporizing membrane the most crosslinked hyperbranched described in claim 1-3, it is characterised in that
Described cross-linking agent is 1,6-hexanediyl ester, Ethylene glycol dimethacrylate or divinylbenzene.
5. the most crosslinked hyperbranched polysiloxanes infiltrating and vaporizing membrane, it is characterised in that formula includes following component: hyperbranched poly
Siloxanes 1.5-2 part, normal hexane 86-89 part, 107 glue 7.5-10 parts, dibutyl tin dilaurate 0.5-1.0 part, cross-linking agent
0.2-1.2 part.
The most crosslinked hyperbranched polysiloxanes infiltrating and vaporizing membrane, it is characterised in that described hyperbranched
The degree of branching of polysiloxanes is 0.70,0.75,0.80.
7. according to polysiloxanes infiltrating and vaporizing membrane the most crosslinked hyperbranched described in claim 5-6, it is characterised in that described 107
The viscosity of glue is 1000cs, 10,000 cs, 1,000,000 cs.
8. according to polysiloxanes infiltrating and vaporizing membrane the most crosslinked hyperbranched described in claim 5-7, it is characterised in that described crosslinking
Agent is 1,6-hexanediyl ester, Ethylene glycol dimethacrylate or divinylbenzene.
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| CN107029557A (en) * | 2016-11-30 | 2017-08-11 | 广东电网有限责任公司电力科学研究院 | A kind of preparation method of silicon rubber infiltrating and vaporizing membrane |
| CN108704494A (en) * | 2018-05-21 | 2018-10-26 | 湖北航泰科技有限公司 | A kind of silicon rubber inierpeneirating network structure polymer penetration vaporization film and preparation method thereof |
| WO2019222303A1 (en) * | 2018-05-15 | 2019-11-21 | Promerus, Llc | High separation performance polydialkylsiloxane pervaporation membranes |
| CN114536626A (en) * | 2022-02-23 | 2022-05-27 | 泰州清润环保科技有限公司 | Cross-linked cured polymer film forming die and using method thereof |
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| CN116328544A (en) * | 2023-03-29 | 2023-06-27 | 山东中盛药化设备有限公司 | Mixed matrix membrane containing cyclodextrin material and preparation method and application thereof |
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| CN107029557A (en) * | 2016-11-30 | 2017-08-11 | 广东电网有限责任公司电力科学研究院 | A kind of preparation method of silicon rubber infiltrating and vaporizing membrane |
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| CN108704494A (en) * | 2018-05-21 | 2018-10-26 | 湖北航泰科技有限公司 | A kind of silicon rubber inierpeneirating network structure polymer penetration vaporization film and preparation method thereof |
| CN114536626A (en) * | 2022-02-23 | 2022-05-27 | 泰州清润环保科技有限公司 | Cross-linked cured polymer film forming die and using method thereof |
| CN114536626B (en) * | 2022-02-23 | 2023-06-23 | 泰州禾益新材料科技有限公司 | Cross-linked cured polymer film forming die and application method thereof |
| CN114832643A (en) * | 2022-05-14 | 2022-08-02 | 阿克菲姆膜材(嘉兴)有限公司 | Preparation method of high-strength long-acting antioxidant polyvinylidene fluoride hollow fiber membrane |
| CN114832643B (en) * | 2022-05-14 | 2022-12-13 | 阿克菲姆膜材(嘉兴)有限公司 | Preparation method of high-strength long-acting antioxidant polyvinylidene fluoride hollow fiber membrane |
| CN116328544A (en) * | 2023-03-29 | 2023-06-27 | 山东中盛药化设备有限公司 | Mixed matrix membrane containing cyclodextrin material and preparation method and application thereof |
| CN116328544B (en) * | 2023-03-29 | 2023-11-21 | 山东中盛药化设备有限公司 | Mixed matrix membrane containing cyclodextrin material and preparation method and application thereof |
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