CN106351026A - Silicon rubber membrane and preparation method thereof - Google Patents
Silicon rubber membrane and preparation method thereof Download PDFInfo
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- CN106351026A CN106351026A CN201610731882.8A CN201610731882A CN106351026A CN 106351026 A CN106351026 A CN 106351026A CN 201610731882 A CN201610731882 A CN 201610731882A CN 106351026 A CN106351026 A CN 106351026A
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- Prior art keywords
- membrane
- resin
- oatmeal
- silicone rubber
- rubber membrane
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- 239000012528 membrane Substances 0.000 title claims abstract description 30
- 229920002379 silicone rubber Polymers 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- -1 polydimethylsiloxane Polymers 0.000 claims abstract description 26
- 239000000203 mixture Substances 0.000 claims abstract description 23
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims abstract description 19
- 239000004205 dimethyl polysiloxane Substances 0.000 claims abstract description 18
- 238000005266 casting Methods 0.000 claims abstract description 17
- 239000003054 catalyst Substances 0.000 claims abstract description 15
- 239000002131 composite material Substances 0.000 claims abstract description 15
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 13
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 11
- 239000011347 resin Substances 0.000 claims abstract description 9
- 229920005989 resin Polymers 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000005345 coagulation Methods 0.000 claims abstract description 6
- 230000015271 coagulation Effects 0.000 claims abstract description 6
- 239000004745 nonwoven fabric Substances 0.000 claims abstract description 6
- 229920000728 polyester Polymers 0.000 claims abstract description 6
- 238000001556 precipitation Methods 0.000 claims abstract description 6
- 239000002904 solvent Substances 0.000 claims abstract description 6
- 238000001291 vacuum drying Methods 0.000 claims abstract description 6
- 239000004945 silicone rubber Substances 0.000 claims description 24
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- 239000003463 adsorbent Substances 0.000 claims description 7
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical group CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 5
- WFKAJVHLWXSISD-UHFFFAOYSA-N isobutyramide Chemical compound CC(C)C(N)=O WFKAJVHLWXSISD-UHFFFAOYSA-N 0.000 claims description 5
- 238000004137 mechanical activation Methods 0.000 claims description 5
- 230000004048 modification Effects 0.000 claims description 5
- 238000012986 modification Methods 0.000 claims description 5
- 239000013589 supplement Substances 0.000 claims description 5
- 229920001577 copolymer Polymers 0.000 claims description 4
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims description 4
- 125000002347 octyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 4
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical group CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 3
- JCVQKRGIASEUKR-UHFFFAOYSA-N triethoxy(phenyl)silane Chemical compound CCO[Si](OCC)(OCC)C1=CC=CC=C1 JCVQKRGIASEUKR-UHFFFAOYSA-N 0.000 claims description 3
- CWAFVXWRGIEBPL-UHFFFAOYSA-N ethoxysilane Chemical compound CCO[SiH3] CWAFVXWRGIEBPL-UHFFFAOYSA-N 0.000 claims description 2
- 238000002386 leaching Methods 0.000 claims description 2
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 claims description 2
- 235000013824 polyphenols Nutrition 0.000 abstract description 13
- 150000008442 polyphenolic compounds Chemical class 0.000 abstract description 11
- 229930003935 flavonoid Natural products 0.000 abstract description 5
- 235000017173 flavonoids Nutrition 0.000 abstract description 5
- 150000002215 flavonoids Chemical class 0.000 abstract description 5
- 239000003960 organic solvent Substances 0.000 abstract description 5
- 238000007654 immersion Methods 0.000 abstract description 4
- 238000002156 mixing Methods 0.000 abstract description 3
- 238000005373 pervaporation Methods 0.000 abstract description 2
- 239000002033 PVDF binder Substances 0.000 abstract 3
- 229920002981 polyvinylidene fluoride Polymers 0.000 abstract 3
- 238000007605 air drying Methods 0.000 abstract 2
- 239000000843 powder Substances 0.000 abstract 2
- 238000007790 scraping Methods 0.000 abstract 2
- 238000001179 sorption measurement Methods 0.000 abstract 2
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 abstract 1
- 238000004132 cross linking Methods 0.000 abstract 1
- 238000001914 filtration Methods 0.000 abstract 1
- 230000035515 penetration Effects 0.000 abstract 1
- 238000000614 phase inversion technique Methods 0.000 abstract 1
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 15
- 238000000605 extraction Methods 0.000 description 10
- 238000000926 separation method Methods 0.000 description 8
- 239000012530 fluid Substances 0.000 description 7
- 230000008595 infiltration Effects 0.000 description 7
- 238000001764 infiltration Methods 0.000 description 7
- 230000000149 penetrating effect Effects 0.000 description 7
- 241000219095 Vitis Species 0.000 description 5
- 238000001704 evaporation Methods 0.000 description 4
- 230000008020 evaporation Effects 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 241000207199 Citrus Species 0.000 description 3
- 244000269722 Thea sinensis Species 0.000 description 3
- 235000009754 Vitis X bourquina Nutrition 0.000 description 3
- 235000012333 Vitis X labruscana Nutrition 0.000 description 3
- 235000014787 Vitis vinifera Nutrition 0.000 description 3
- 235000020971 citrus fruits Nutrition 0.000 description 3
- 239000000470 constituent Substances 0.000 description 3
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 235000009392 Vitis Nutrition 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 230000004907 flux Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 210000000582 semen Anatomy 0.000 description 2
- 235000013616 tea Nutrition 0.000 description 2
- 238000009834 vaporization Methods 0.000 description 2
- 230000008016 vaporization Effects 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000000975 bioactive effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 235000009569 green tea Nutrition 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- MSRJTTSHWYDFIU-UHFFFAOYSA-N octyltriethoxysilane Chemical compound CCCCCCCC[Si](OCC)(OCC)OCC MSRJTTSHWYDFIU-UHFFFAOYSA-N 0.000 description 1
- 229960003493 octyltriethoxysilane Drugs 0.000 description 1
- 229920002414 procyanidin Polymers 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/18—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with two layers of different macromolecular materials
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0002—Organic membrane manufacture
- B01D67/0009—Organic membrane manufacture by phase separation, sol-gel transition, evaporation or solvent quenching
- B01D67/0011—Casting solutions therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0002—Organic membrane manufacture
- B01D67/0009—Organic membrane manufacture by phase separation, sol-gel transition, evaporation or solvent quenching
- B01D67/0013—Casting processes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0081—After-treatment of organic or inorganic membranes
- B01D67/0093—Chemical modification
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/12—Composite membranes; Ultra-thin membranes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/12—Composite membranes; Ultra-thin membranes
- B01D69/125—In situ manufacturing by polymerisation, polycondensation, cross-linking or chemical reaction
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/30—Polyalkenyl halides
- B01D71/32—Polyalkenyl halides containing fluorine atoms
- B01D71/34—Polyvinylidene fluoride
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0002—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate
- D06N3/0011—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate using non-woven fabrics
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0002—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate
- D06N3/0015—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate using fibres of specified chemical or physical nature, e.g. natural silk
- D06N3/0036—Polyester fibres
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2323/00—Details relating to membrane preparation
- B01D2323/30—Cross-linking
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Dispersion Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention discloses a preparation method of a silicon rubber membrane. The preparation method comprises the following steps: dissolving polydimethylsiloxane in n-hexane, uniformly stirring, then adding macroporous adsorption resin powder, ultrasonically dispersing, adding a cross-linking agent, mixing, stirring, adding a catalyst, stirring at a room temperature, and defoaming, thus obtaining a membrane casting solution; mixing dried polyvinylidene fluoride and crushed macroporous adsorption resin powder into a mixture, adding the mixture into a solvent, dimethylacetamide, ultrasonically dispersing, uniformly stirring, filtering, standing, defoaming, pouring onto a polyester nonwoven fabric, scraping a membrane by using water as a coagulation bath to obtain a modified polyvinylidene fluoride bottom membrane by adopting an immersion precipitation phase inversion method, and air drying at a room temperature; and pouring the membrane casting solution onto the polyvinylidene fluoride bottom membrane, scraping the membrane, air drying at a normal temperature, performing vacuum drying in a vacuum baking oven at 50 to 100 DEG C until complete cross-linking, thus obtaining the silicon rubber composite membrane. The silicon rubber membrane can be used for separating organic solvents and plant polyphenols and flavonoid components by virtue of penetration and pervaporation.
Description
Technical field
The present invention relates to a kind of preparation method for extracting separation polyphenol, the silicone rubber membrane of Flavonoid substances, belong to silicon
Rubber materials.
Background technology
Infiltration evaporation (pervaporation, pv) isolation technics are limited by membrane material, be currently used primarily in nearly boiling point,
Constant boiling point mixture and the separation of isomerss, a small amount of in the removing to minor amount of water in organic solvent and mixed solvent and waste water
The separation of organic pollution, not yet report have in the extraction of active components of plants.
Polyphenol and flavonoid are relatively common bioactive substances in nature, all contain as in Folium Camelliae sinensis, Semen Vitis viniferae, can use
Medium in food, medicine and cosmetics.Based on the extraction of this two classes material is prepared in the way of first slightly carrying rear purification at present,
Operation is complex, long the production cycle.
Content of the invention
The purpose of the present invention is for above key issue, provides a kind of silicone rubber membrane and preparation method thereof.
For achieving the above object, the technical solution used in the present invention is: the preparation method of this silicone rubber membrane includes following
Step:
(1) prepare resin-oatmeal: macroporous adsorbent resin mechanical activation comminution, cross 800-1000 mesh, be placed in 80 DEG C of vacuum drying ovens and dry
Resin-oatmeal, standby；
(2) prepare casting solution: polydimethylsiloxane is dissolved in normal hexane, is stirring evenly and then adding into resin-oatmeal, ultrasonic disperse,
Add cross-linking agent mix and blend 0.5～2 hour, add catalyst, supplement afterwards and add normal hexane to poly dimethyl in mixed liquor
The concentration of siloxanes is 8～20wt%, is stirred at room temperature 8～16 hours, casting solution is made in deaeration；Described resin-oatmeal and poly dimethyl
The mass ratio of siloxanes is 0.001～0.01:1；Described cross-linking agent is tetraethyl orthosilicate, phenyl triethoxysilane, octyl group three
Any one in Ethoxysilane and octyl group trimethoxy silane, described cross-linking agent with the mass ratio of polydimethylsiloxane is
0.05～0.1:1；Described catalyst is dibutyl tin laurate, and described catalyst with the mass ratio of polydimethylsiloxane is
0.001～0.005:1；
(3) prepare Kynoar counterdie: by dried Kynoar with resin-oatmeal according to mass ratio 1:0.002～0.02
It is mixed into mixture, mixture is added in solvent dimethyl acetylamide, is made into the solution of 10-25wt%, ultrasonic disperse, and
Stir under the conditions of 65～85 DEG C, filter, standing and defoaming, after be poured on knifing on polyester non-woven fabric, water be coagulation bath, using leaching
No precipitation phase inversion does not obtain the Kynoar counterdie of modification, and room temperature is dried；
(4) prepare composite silicone rubber film: casting solution is poured on knifing on Kynoar counterdie, room temperature dries, is then placed in true
It is dried under vacuum to fully crosslinked, prepared composite silicone rubber membrane at 50～100 DEG C in empty baking oven.
Wherein, described macroporous adsorbent resin is styrene type low pole copolymer or the nonpolar copolymer of styrene type.
Additionally, the present invention also provides a kind of silicone rubber membrane, prepared by above method.
Compared with prior art, present invention has the advantage that
A. the silicone rubber membrane that the present invention provides can be used for separating from low-concentration organic solvent solution as infiltration vaporization separation film
Organic solvent, possesses high separation factor and permeation flux, for the ethanol solution of 0.05wt%, in 40 DEG C, film downstream vacuum degree
Under the conditions of 0.3kpa, permeation flux is 190.7gm-2h-1, separation factor 27.6；
B. the silicone rubber membrane of this law is alternatively arranged as infiltration vaporization separation film for the extraction separation of polyphenol, Flavonoid substances, infiltration
In liquid, polyphenol or flavonoid purity are high, reach more than 95, need not be further purified, after processing penetrating fluid concentrate drying i.e.
Available.And need in traditional extraction technique to consume substantial amounts of organic solvent and carry out eluting etc., complex process, and environmental pollution is tight
Weight.
Specific embodiment
Below in conjunction with instantiation, technical scheme is described further.
Embodiment 1: the present embodiment provides a kind of silicone rubber membrane, has following methods to prepare
(1) prepare resin-oatmeal: ab-8 macroporous adsorbent resin mechanical activation comminution, cross 1000 mesh, be placed in 80 DEG C of vacuum drying ovens and dry
Resin-oatmeal, standby；
(2) prepare casting solution: polydimethylsiloxane is dissolved in normal hexane, is stirring evenly and then adding into resin-oatmeal, ultrasonic disperse,
Add cross-linking agent tetraethyl orthosilicate mix and blend 2 hours, add catalyst, supplement afterwards and add normal hexane in mixed liquor poly- two
The concentration of methylsiloxane is 8wt%, is stirred at room temperature 8 hours, casting solution is made in deaeration；Described resin-oatmeal and polydimethylsiloxanes
The mass ratio of alkane is 0.0011:1；Described cross-linking agent is 0.1:1 with the mass ratio of polydimethylsiloxane；Described catalyst is two
Dibutyl tin laurate, described catalyst is 0.001:1 with the mass ratio of polydimethylsiloxane；
(3) prepare Kynoar counterdie: dried Kynoar is mixed into according to mass ratio 1:0.002 with resin-oatmeal
Mixture, mixture is added in solvent dimethyl acetylamide, is made into the solution of 25wt%, ultrasonic disperse, and under the conditions of 65 DEG C
Stir, filter, standing and defoaming, after be poured on knifing on polyester non-woven fabric, water be coagulation bath, using immersion precipitation phase inversion process
Obtain the Kynoar counterdie of modification, room temperature is dried；
(4) prepare composite silicone rubber film: casting solution is poured on knifing on Kynoar counterdie, room temperature dries, is then placed in true
It is dried under vacuum to fully crosslinked, prepared composite silicone rubber membrane at 100 DEG C in empty baking oven.
Extraction is followed the steps below with the film that the present embodiment prepares to tea leaf polyphenols: take green tea, be crushed to
50 mesh, add the 5wt% ethanol water of 5 times of quality, obtain extracting solution in 60 DEG C of extraction 1h；Extracting solution composite silicone rubber membrane exists
60 DEG C, film downstream vacuum degree be 0.5kpa under carry out infiltration evaporation separate, collect penetrating fluid；Penetrating fluid is dense through 60 DEG C of cryogenic vacuums
It is dried after contracting, the solid constituent obtaining is tea polyphenols, polyphenol content is 95.8%.
Embodiment 2:
(1) prepare resin-oatmeal: d-101 macroporous adsorbent resin mechanical activation comminution, cross 800 mesh, be placed in 80 DEG C of vacuum drying ovens and dry
Resin-oatmeal, standby；
(2) prepare casting solution: polydimethylsiloxane is dissolved in normal hexane, is stirring evenly and then adding into resin-oatmeal, ultrasonic disperse,
Add cross-linking agent phenyl triethoxysilane mix and blend 0.5 hour, add catalyst, supplement afterwards and add normal hexane to mixing
In liquid, the concentration of polydimethylsiloxane is 20wt%, is stirred at room temperature 16 hours, casting solution is made in deaeration；Described resin-oatmeal with poly-
The mass ratio of dimethyl siloxane is 0.01:1；Described cross-linking agent is 0.05:1 with the mass ratio of polydimethylsiloxane；Described
Catalyst is dibutyl tin laurate, and described catalyst is 0.005:1 with the mass ratio of polydimethylsiloxane；
(3) prepare Kynoar counterdie: dried Kynoar is mixed into according to mass ratio 1:0.02 with resin-oatmeal
Mixture, mixture is added in solvent dimethyl acetylamide, is made into the solution of 10wt%, ultrasonic disperse, and under the conditions of 85 DEG C
Stir, filter, standing and defoaming, after be poured on knifing on polyester non-woven fabric, water be coagulation bath, using immersion precipitation phase inversion process
Obtain the Kynoar counterdie of modification, room temperature is dried；
(4) prepare composite silicone rubber film: casting solution is poured on knifing on Kynoar counterdie, room temperature dries, is then placed in true
It is dried under vacuum to fully crosslinked, prepared composite silicone rubber membrane at 50 DEG C in empty baking oven.
Extraction is followed the steps below with the film that the present embodiment prepares to grape procyanidinses: take Semen Vitis viniferae, be crushed to
100 mesh, add the 20wt% ethanol water of 50 times of quality, obtain extracting solution in 40 DEG C of extraction 5h；Extracting solution composite silicone rubber membrane
Carry out infiltration evaporation under 30 DEG C, film downstream vacuum degree are for 0.2kpa to separate, collect penetrating fluid；Penetrating fluid is through 45 DEG C of cryogenic vacuums
It is dried after concentration, the solid constituent obtaining is grape polyphenolss, and the content of grape polyphenolss is 97.2%.
Embodiment 3:
(1) prepare resin-oatmeal: dm-130 macroporous adsorbent resin mechanical activation comminution, cross 1000 mesh, be placed in 80 DEG C of vacuum drying ovens and dry
Obtain resin-oatmeal, standby；
(2) prepare casting solution: polydimethylsiloxane is dissolved in normal hexane, is stirring evenly and then adding into resin-oatmeal, ultrasonic disperse,
Add cross-linking agent octyltri-ethoxysilane mix and blend 1 hour, add catalyst, supplement afterwards and add normal hexane to mixed liquor
The concentration of middle polydimethylsiloxane is 10wt%, is stirred at room temperature 10 hours, casting solution is made in deaeration；Described resin-oatmeal and poly- two
The mass ratio of methylsiloxane is 0.005:1；Described cross-linking agent is 0.08:1 with the mass ratio of polydimethylsiloxane；Described urge
Agent is dibutyl tin laurate, and described catalyst is 0.002:1 with the mass ratio of polydimethylsiloxane；
(3) prepare Kynoar counterdie: dried Kynoar is mixed into according to mass ratio 1:0.005 with resin-oatmeal
Mixture, mixture is added in solvent dimethyl acetylamide, is made into the solution of 15wt%, ultrasonic disperse, and under the conditions of 75 DEG C
Stir, filter, standing and defoaming, after be poured on knifing on polyester non-woven fabric, water be coagulation bath, using immersion precipitation phase inversion process
Obtain the Kynoar counterdie of modification, room temperature is dried；
(4) prepare composite silicone rubber film: casting solution is poured on knifing on Kynoar counterdie, room temperature dries, is then placed in true
It is dried under vacuum to fully crosslinked, prepared composite silicone rubber membrane at 80 DEG C in empty baking oven.
Extraction is followed the steps below to Citrus polyphenol with the film that the present embodiment prepares: take Pericarpium Citri Reticulatae, be crushed to 80
Mesh, adds the 10wt% ethanol water of 20 times of quality, obtains extracting solution in 45 DEG C of extraction 3h；Extracting solution composite silicone rubber membrane exists
40 DEG C, film downstream vacuum degree be 0.3kpa under carry out infiltration evaporation separate, collect penetrating fluid；Penetrating fluid is dense through 45 DEG C of cryogenic vacuums
It is dried after contracting, the solid constituent obtaining is Citrus polyphenol, and the content of Citrus polyphenol is 98.3%.
Claims (3)
1. a kind of preparation method of silicone rubber membrane is it is characterised in that the method comprises the following steps:
(1) prepare resin-oatmeal: macroporous adsorbent resin mechanical activation comminution, cross 800-1000 mesh, be placed in 80 DEG C of vacuum drying ovens and dry
Resin-oatmeal, standby；
(2) prepare casting solution: polydimethylsiloxane is dissolved in normal hexane, is stirring evenly and then adding into resin-oatmeal, ultrasonic disperse,
Add cross-linking agent mix and blend 0.5～2 hour, add catalyst, supplement afterwards and add normal hexane to poly dimethyl in mixed liquor
The concentration of siloxanes is 8～20wt%, is stirred at room temperature 8～16 hours, casting solution is made in deaeration；Described resin-oatmeal and poly dimethyl
The mass ratio of siloxanes is 0.001～0.01 1；Described cross-linking agent is tetraethyl orthosilicate, phenyl triethoxysilane, octyl group three
Any one in Ethoxysilane and octyl group trimethoxy silane, described cross-linking agent with the mass ratio of polydimethylsiloxane is
0.05～0.1 1；Described catalyst is dibutyl tin laurate, and described catalyst with the mass ratio of polydimethylsiloxane is
0.001～0.005 1；
(3) prepare Kynoar counterdie: by dried Kynoar with resin-oatmeal according to mass ratio 1:0.002～0.02
It is mixed into mixture, mixture is added in solvent dimethyl acetylamide, is made into the solution of 10-25wt%, ultrasonic disperse, and
Stir under the conditions of 65～85 DEG C, filter, standing and defoaming, after be poured on knifing on polyester non-woven fabric, water be coagulation bath, using leaching
No precipitation phase inversion does not obtain the Kynoar counterdie of modification, and room temperature is dried；
(4) prepare composite silicone rubber film: casting solution is poured on knifing on Kynoar counterdie, room temperature dries, is then placed in true
It is dried under vacuum to fully crosslinked, prepared composite silicone rubber membrane at 50～100 DEG C in empty baking oven.
2. the preparation method of composite silicone rubber membrane according to claim 1, described macroporous adsorbent resin is styrene type
Low pole copolymer or the nonpolar copolymer of styrene type.
3. a kind of silicone rubber membrane is it is characterised in that prepared by any one of claim 1-2.
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