CN104069751A - Preparation method for PDMS (polydimethylsiloxane)/PTFE polytetrafluoroethylene pervaporation hollow-fiber membrane - Google Patents

Preparation method for PDMS (polydimethylsiloxane)/PTFE polytetrafluoroethylene pervaporation hollow-fiber membrane Download PDF

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CN104069751A
CN104069751A CN201410344280.8A CN201410344280A CN104069751A CN 104069751 A CN104069751 A CN 104069751A CN 201410344280 A CN201410344280 A CN 201410344280A CN 104069751 A CN104069751 A CN 104069751A
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fiber membrane
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pdms
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ptfe
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陈雄
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Abstract

The invention discloses a preparation method for a PDMS (polydimethylsiloxane)/PTFE polytetrafluoroethylene pervaporation hollow-fiber membrane. The method comprises the following steps: dissolving 1 weight part of PDMS into n-hexane, adding 0.04 to 0.15 part of a cross-linking agent TEOS, carrying out mixing and stirring for 0.5 to 4 hours, adding 0.01 to 0.1 part of a catalyst dibutyltin dilaurate, supplementing n-hexane till the mass concentration percentage of PDMS in the mixed liquor is 5 to 35 percent, carrying out stirring at the room temperature for 4 to 24 hours, and carrying out centrifugation and defoaming to obtain a membrane preparation liquid; cleaning a PTFE hollow-fiber membrane with distilled water till the hollow-fiber membrane is neutral, airing the neutral hollow-fiber membrane, dipping the aired hollow-fiber membrane in the membrane preparation liquid for 1 to 3 seconds, taking out the hollow-fiber membrane for airing at the room temperature, carrying out membrane dipping and airing repeatedly for 1 to 4 times, placing the aired hollow-fiber membrane into a vacuum oven for 35 to 115 DEG C' vacuum drying till crosslinking is complete, so as to obtain the PDMS/PTFE compound hollow-fiber membrane. The method is simple in technology; the hollow-fiber membrane has better separation effect for an acetone/butanol/ethyl alcohol solution in a fermentation liquid.

Description

A kind of preparation method of PDMS/PTFE infiltration evaporation hollow-fibre membrane
Technical field
The present invention relates to a kind of preferentially see through organic PDMS/PTFE(dimethyl silicone polymer/polytetrafluoroethylene (PTFE) for infiltration evaporation) preparation method of composite hollow fiber membrane, belong to infiltrating and vaporizing membrane separation field.
Background technology
As far back as 1861, Pasteur just found that bacterium can produce butanols.Biological fermentation process is prepared in the product of butanols (ABE fermentation) main containing acetone, butanols and ethanol, and three's ratio is 3:6:1.Be subject to the inhibitory action of product butanols, in zymotic fluid, total solvent concentration can only reach about 20gL -1, production capacity is lower.Because the boiling point of butanols is higher than water, industrially 98% water need to be separated from zymotic fluid when utilizing rectification method separating butanol, whole process economy is poor, high expensive, in order to address the above problem, scientist attempts some separation methods, infiltration evaporation (PV), absorption, liquid-liquid extraction, air lift and counter-infiltration etc.The original position that is directly coupled to realize butanols with sweat separates, and alleviates the inhibitory action of butanols, improves ferment strength and raw material availability.
Infiltration evaporation (pervaporation, PV) can realize with low energy consumption the separation task that the conventional methods such as distillation, extraction, absorption have been difficult to, be particularly suitable for separating the separation of nearly boiling point, constant boiling point mixture and isomer, to minor amount of water in organic solvent and mixed solvent remove and waste water in the separation of a small amount of organic pollution there is significantly technical and advantage economically.
The infiltrating and vaporizing membrane that is applied at present acetone/butanol/separation of ethanol mainly contains high molecular polymerization film, inoranic membrane and liquid film.Inoranic membrane is because material price costliness, liquid film are because the inferior positions such as poor stability have limited them in industrial application.Comparatively speaking, high molecular polymerization film research is more, as polyurethane film etc. (Shi Xuan etc. the infiltration evaporation performance study [J] of polyurethane film acetone/butanol solution. Chinese material science and technology and equipment, 2008,5 (4): 35-37), but all study as main taking flat film, the membrane module of doughnut is less, and the loading density of hollow-fibre membrane is large, floor space is little, owing to being self-cradling type, do not need backing material, cost is low.
Summary of the invention
The object of this invention is to provide a kind of preparation method of PDMS/PTFE infiltration evaporation hollow-fibre membrane.
For achieving the above object, the technical solution used in the present invention is: the preparation method of this PDMS/PTFE infiltration evaporation hollow-fibre membrane comprises the following steps:
A. by weight, getting 1 part of dimethyl silicone polymer is dissolved in n-hexane, after add 0.04~0.15 part of crosslinking agent ethyl orthosilicate, mix and blend 0.5~4 hour, add again 0.01~0.1 part of catalyst dibutyl tin laurate, rear supplement that to add n-hexane be 5~35% to the mass percent concentration of dimethyl silicone polymer in mixed liquor, stirring at room temperature 4~24 hours, preparation liquid is made in centrifugal, deaeration;
B. by polytetrafluoroethylhollow hollow fiber membrane with distilled water flushing to neutral and dry, in the described preparation liquid of rear immersion 1~3 second, rear taking-up is at room temperature dried, repeat above-mentionedly to soak film, dry operation 1~4 time, then put into vacuum drying oven vacuum drying at 35~115 DEG C and, to completely crosslinked, make PDMS/PTFE composite hollow fiber membrane.
Compared with prior art, to prepare the technique of PDMS/PTFE infiltration evaporation hollow-fibre membrane simple, easy to operate in the present invention.The PDMS separating layer of prepared PDMS/PTFE infiltration evaporation doughnut film outer surface densification is selectively good to acetone/butanol/ethanol, and separation factor is high, and flux is considerable, can be used for the separation of acetone/butanol/alcohol fermentation liquid; The hydrophobic PTFE supporting layer of this film inner surface, compares other materials, not only has better support strength, but also has stronger contamination resistance.
Detailed description of the invention
Below in conjunction with instantiation, technical scheme of the present invention is described further.
Embodiment 1:
Claim 10g dimethyl silicone polymer (PDMS) to be dissolved in 100g n-hexane, add 0.4g crosslinking agent ethyl orthosilicate, under room temperature, mix and blend adds 0.1g catalyst dibutyl tin laurate after 0.5 hour, adding n-hexane to the concentration of dimethyl silicone polymer in mixed liquor is 5wt%, stirring at room temperature 4 hours after sealing, gained solution is made preparation liquid through centrifugal, deaeration.Polytetrafluoroethylene (PTFE) hollow-fibre membrane is extremely neutral with distilled water flushing, and room temperature is dried, stand-by as basement membrane.The basement membrane of this processing is immersed in preparation liquid 1~3 second, and after taking out, room temperature is dried.Repeat film 4 times, then put into vacuum drying oven vacuum drying at 110 DEG C and make PDMS/PTFE composite hollow fiber membrane to completely crosslinked in 12 hours.The skin of gained composite hollow fiber membrane is fine and close PDMS separating layer, and internal layer is hydrophobic PTFE supporting layer.The PDMS/PTFE composite hollow fiber membrane of the present embodiment gained is carried out to infiltration evaporation separating experiment to ABE fermentation simulation liquid, and performance is as shown in table 1:
Table 1
Note: test condition: 40 DEG C of temperature, downstream vacuum 0.3KPa.
Embodiment 2:
Claim 20g dimethyl silicone polymer to be dissolved in 40g n-hexane, add 1.5g crosslinking agent ethyl orthosilicate, under room temperature, mix and blend adds 1.0g catalyst dibutyl tin laurate after 4 hours, adding n-hexane to the concentration of dimethyl silicone polymer in mixed liquor is 30wt%, stirring at room temperature 24 hours after sealing, gained solution is made preparation liquid through centrifugal, deaeration.PTFE hollow-fibre membrane is extremely neutral with distilled water flushing, and room temperature is dried, stand-by as basement membrane.The basement membrane of this processing is immersed in preparation liquid 1~3 second, and after taking out, room temperature is dried.Repeat film 1 time, then put into vacuum drying oven vacuum drying at 50 DEG C and make PDMS/PTFE composite hollow fiber membrane to completely crosslinked in 12 hours.The skin of gained composite hollow fiber membrane is fine and close PDMS separating layer, and internal layer is hydrophobic PTFE supporting layer.The PDMS/PTFE composite hollow fiber membrane of the present embodiment gained is carried out to infiltration evaporation separating experiment to ABE fermentation simulation liquid, and performance is as shown in table 2:
Table 2
Note: test condition: 40 DEG C of temperature, downstream vacuum 0.3KPa.
Embodiment 3:
Claim 20g dimethyl silicone polymer to be dissolved in 100g n-hexane, add 1.5g crosslinking agent ethyl orthosilicate, under room temperature, mix and blend adds 0.3g catalyst dibutyl tin laurate after 2 hours, adding n-hexane to the concentration of dimethyl silicone polymer in mixed liquor is 15wt%, stirring at room temperature 14 hours after sealing, gained solution is made preparation liquid through centrifugal, deaeration.PTFE hollow-fibre membrane is extremely neutral with distilled water flushing, and room temperature is dried, stand-by as basement membrane.The basement membrane of this processing is immersed in preparation liquid 1~3 second, and after taking out, room temperature is dried.Repeat film 2 times, then put into vacuum drying oven vacuum drying at 90 DEG C and make PDMS/PTFE composite hollow fiber membrane to completely crosslinked in 14 hours.The skin of gained composite hollow fiber membrane is fine and close PDMS separating layer, and internal layer is hydrophobic PTFE supporting layer.The PDMS/PTFE composite hollow fiber membrane of the present embodiment gained is carried out to infiltration evaporation separating experiment to ABE fermentation simulation liquid, and performance is as shown in table 3:
Table 3
Note: test condition: 40 DEG C of temperature, downstream vacuum 0.3KPa.

Claims (1)

1. a preparation method for PDMS/PTFE infiltration evaporation hollow-fibre membrane, is characterized in that the method comprises the following steps:
A. by weight, getting 1 part of dimethyl silicone polymer is dissolved in n-hexane, after add 0.04~0.15 part of crosslinking agent ethyl orthosilicate, mix and blend 0.5~4 hour, add again 0.01~0.1 part of catalyst dibutyl tin laurate, rear supplement that to add n-hexane be 5~35% to the mass percent concentration of dimethyl silicone polymer in mixed liquor, stirring at room temperature 4~24 hours, preparation liquid is made in centrifugal, deaeration;
B. by polytetrafluoroethylhollow hollow fiber membrane with distilled water flushing to neutral and dry, in the described preparation liquid of rear immersion 1~3 second, rear taking-up is at room temperature dried, repeat above-mentionedly to soak film, dry operation 1~4 time, after put into vacuum drying oven vacuum drying at 35~115 DEG C and to completely crosslinked, make PDMS/PTFE composite hollow fiber membrane.
CN201410344280.8A 2014-07-19 2014-07-19 Preparation method for PDMS (polydimethylsiloxane)/PTFE polytetrafluoroethylene pervaporation hollow-fiber membrane Pending CN104069751A (en)

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CN105779507A (en) * 2014-12-23 2016-07-20 北京化工大学常州先进材料研究院 Technology for removing ethanol in fermentation broth through polyvinyl triethoxysilane vapor permeation membrane
CN105771669A (en) * 2014-12-24 2016-07-20 北京化工大学常州先进材料研究院 Application of modified polyvinyl triethoxysilane membrane material in separating ethanol/water system
CN105771705A (en) * 2014-12-23 2016-07-20 北京化工大学常州先进材料研究院 Application of modified polyvinyl triethoxysilane membrane material in separating of butanol/water system
CN106268372A (en) * 2016-10-20 2017-01-04 合肥创想能源环境科技有限公司 A kind of preparation method of polyurethane infiltrating and vaporizing membrane
CN107096400A (en) * 2017-06-13 2017-08-29 北京工商大学 A kind of modified polyurethane organosilicon double-layer osmotic vaporizes the preparation method of film
CN107602874A (en) * 2017-11-01 2018-01-19 中国药科大学 A kind of method based on microflow control technique synthesis metal-organic framework materials
CN112999884A (en) * 2021-04-02 2021-06-22 上海电气集团股份有限公司 Pervaporation membrane, preparation method thereof and treatment method of coating wastewater
CN118619561A (en) * 2024-06-13 2024-09-10 中南民族大学 A preparation method and application of super hydrophobic transparent glass

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105779507A (en) * 2014-12-23 2016-07-20 北京化工大学常州先进材料研究院 Technology for removing ethanol in fermentation broth through polyvinyl triethoxysilane vapor permeation membrane
CN105771705A (en) * 2014-12-23 2016-07-20 北京化工大学常州先进材料研究院 Application of modified polyvinyl triethoxysilane membrane material in separating of butanol/water system
CN105771669A (en) * 2014-12-24 2016-07-20 北京化工大学常州先进材料研究院 Application of modified polyvinyl triethoxysilane membrane material in separating ethanol/water system
CN106268372A (en) * 2016-10-20 2017-01-04 合肥创想能源环境科技有限公司 A kind of preparation method of polyurethane infiltrating and vaporizing membrane
CN107096400A (en) * 2017-06-13 2017-08-29 北京工商大学 A kind of modified polyurethane organosilicon double-layer osmotic vaporizes the preparation method of film
CN107096400B (en) * 2017-06-13 2019-10-01 北京工商大学 A kind of preparation method of modified polyurethane-organosilicon double-layer osmotic vaporization film
CN107602874A (en) * 2017-11-01 2018-01-19 中国药科大学 A kind of method based on microflow control technique synthesis metal-organic framework materials
CN112999884A (en) * 2021-04-02 2021-06-22 上海电气集团股份有限公司 Pervaporation membrane, preparation method thereof and treatment method of coating wastewater
CN118619561A (en) * 2024-06-13 2024-09-10 中南民族大学 A preparation method and application of super hydrophobic transparent glass

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