TW201542634A - 靜電紡絲液、聚乙烯醇奈米纖維及離子交換膜 - Google Patents
靜電紡絲液、聚乙烯醇奈米纖維及離子交換膜 Download PDFInfo
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- TW201542634A TW201542634A TW103138066A TW103138066A TW201542634A TW 201542634 A TW201542634 A TW 201542634A TW 103138066 A TW103138066 A TW 103138066A TW 103138066 A TW103138066 A TW 103138066A TW 201542634 A TW201542634 A TW 201542634A
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- Prior art keywords
- polyvinyl alcohol
- ion exchange
- group
- weight
- electrospinning
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- 239000004372 Polyvinyl alcohol Substances 0.000 title claims abstract description 89
- 229920002451 polyvinyl alcohol Polymers 0.000 title claims abstract description 89
- 238000001523 electrospinning Methods 0.000 title claims abstract description 33
- 239000003014 ion exchange membrane Substances 0.000 title claims abstract description 23
- 239000002121 nanofiber Substances 0.000 title claims description 51
- 238000005342 ion exchange Methods 0.000 claims abstract description 51
- 239000003607 modifier Substances 0.000 claims abstract description 30
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 125000000524 functional group Chemical group 0.000 claims abstract description 7
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 6
- 239000001257 hydrogen Substances 0.000 claims abstract description 6
- 150000001450 anions Chemical group 0.000 claims abstract description 4
- 239000003153 chemical reaction reagent Substances 0.000 claims description 39
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 claims description 10
- LLHSEQCZSNZLRI-UHFFFAOYSA-M sodium;3,5-bis(methoxycarbonyl)benzenesulfonate Chemical compound [Na+].COC(=O)C1=CC(C(=O)OC)=CC(S([O-])(=O)=O)=C1 LLHSEQCZSNZLRI-UHFFFAOYSA-M 0.000 claims description 7
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 6
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims description 5
- 235000010413 sodium alginate Nutrition 0.000 claims description 5
- 229940005550 sodium alginate Drugs 0.000 claims description 5
- 239000000661 sodium alginate Substances 0.000 claims description 5
- 235000010288 sodium nitrite Nutrition 0.000 claims description 5
- HTXMGVTWXZBZNC-UHFFFAOYSA-N 3,5-bis(methoxycarbonyl)benzenesulfonic acid Chemical compound COC(=O)C1=CC(C(=O)OC)=CC(S(O)(=O)=O)=C1 HTXMGVTWXZBZNC-UHFFFAOYSA-N 0.000 claims description 4
- HELHAJAZNSDZJO-UHFFFAOYSA-L sodium tartrate Chemical compound [Na+].[Na+].[O-]C(=O)C(O)C(O)C([O-])=O HELHAJAZNSDZJO-UHFFFAOYSA-L 0.000 claims description 4
- 125000000129 anionic group Chemical group 0.000 claims description 3
- 125000000449 nitro group Chemical group [O-][N+](*)=O 0.000 claims description 3
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 2
- KCIDZIIHRGYJAE-YGFYJFDDSA-L dipotassium;[(2r,3r,4s,5r,6r)-3,4,5-trihydroxy-6-(hydroxymethyl)oxan-2-yl] phosphate Chemical compound [K+].[K+].OC[C@H]1O[C@H](OP([O-])([O-])=O)[C@H](O)[C@@H](O)[C@H]1O KCIDZIIHRGYJAE-YGFYJFDDSA-L 0.000 claims description 2
- 229940009662 edetate Drugs 0.000 claims description 2
- 125000001261 isocyanato group Chemical group *N=C=O 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims 1
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims 1
- SOBHUZYZLFQYFK-UHFFFAOYSA-K trisodium;hydroxy-[[phosphonatomethyl(phosphonomethyl)amino]methyl]phosphinate Chemical compound [Na+].[Na+].[Na+].OP(O)(=O)CN(CP(O)([O-])=O)CP([O-])([O-])=O SOBHUZYZLFQYFK-UHFFFAOYSA-K 0.000 claims 1
- 229920002554 vinyl polymer Polymers 0.000 claims 1
- 239000000835 fiber Substances 0.000 abstract description 27
- 150000002500 ions Chemical class 0.000 abstract description 4
- 239000012528 membrane Substances 0.000 description 41
- 239000000243 solution Substances 0.000 description 23
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 21
- 238000009987 spinning Methods 0.000 description 18
- 230000007062 hydrolysis Effects 0.000 description 15
- 238000006460 hydrolysis reaction Methods 0.000 description 15
- 239000000523 sample Substances 0.000 description 12
- 229910021529 ammonia Inorganic materials 0.000 description 9
- 239000007789 gas Substances 0.000 description 8
- 230000000694 effects Effects 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 239000000203 mixture Substances 0.000 description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 238000001914 filtration Methods 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 238000005259 measurement Methods 0.000 description 5
- 238000001878 scanning electron micrograph Methods 0.000 description 5
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 4
- 239000003344 environmental pollutant Substances 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 230000035699 permeability Effects 0.000 description 4
- 231100000719 pollutant Toxicity 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 229910052708 sodium Inorganic materials 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000005341 cation exchange Methods 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 125000004177 diethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 150000002891 organic anions Chemical class 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 3
- 238000009864 tensile test Methods 0.000 description 3
- 125000002091 cationic group Chemical group 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000009423 ventilation Methods 0.000 description 2
- XASWYPVFCVEQSU-UHFFFAOYSA-N 2-[2-[bis(carboxymethyl)amino]ethyl-(carboxymethyl)amino]acetic acid;potassium Chemical compound [K].OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O XASWYPVFCVEQSU-UHFFFAOYSA-N 0.000 description 1
- 206010059866 Drug resistance Diseases 0.000 description 1
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 1
- 229920001410 Microfiber Polymers 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000005273 aeration Methods 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 239000013068 control sample Substances 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- LFQRKUIOSYPVFY-UHFFFAOYSA-L dipotassium diacetate Chemical compound [K+].[K+].CC([O-])=O.CC([O-])=O LFQRKUIOSYPVFY-UHFFFAOYSA-L 0.000 description 1
- QLBHNVFOQLIYTH-UHFFFAOYSA-L dipotassium;2-[2-[bis(carboxymethyl)amino]ethyl-(carboxylatomethyl)amino]acetate Chemical compound [K+].[K+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O QLBHNVFOQLIYTH-UHFFFAOYSA-L 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000005685 electric field effect Effects 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- HNONEKILPDHFOL-UHFFFAOYSA-M tolonium chloride Chemical compound [Cl-].C1=C(C)C(N)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 HNONEKILPDHFOL-UHFFFAOYSA-M 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J39/00—Cation exchange; Use of material as cation exchangers; Treatment of material for improving the cation exchange properties
- B01J39/08—Use of material as cation exchangers; Treatment of material for improving the cation exchange properties
- B01J39/16—Organic material
- B01J39/18—Macromolecular compounds
- B01J39/20—Macromolecular compounds obtained by reactions only involving unsaturated carbon-to-carbon bonds
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01D71/06—Organic material
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- B01D71/76—Macromolecular material not specifically provided for in a single one of groups B01D71/08 - B01D71/74
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F116/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal or ketal radical
- C08F116/02—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal or ketal radical by an alcohol radical
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- D01F1/00—General methods for the manufacture of artificial filaments or the like
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- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/02—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D01F6/14—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds from polymers of unsaturated alcohols, e.g. polyvinyl alcohol, or of their acetals or ketals
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- C08J2329/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
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- D01D5/0015—Electro-spinning characterised by the initial state of the material
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Abstract
一種離子交換膜,上述之離子交換膜的纖維係由靜電紡絲而得。靜電紡絲所用的紡絲液組成包括100重量份的聚乙烯醇、10-100重量份的修飾劑、10-100重量份的離子交換試劑與100-2,500重量份的水。上述之修飾劑具有至少一個反應基,以與聚乙烯醇的氫氧基進行反應。上述之離子交換試劑具有一極性官能基,以與聚乙烯醇的氫氧基形成氫鍵,還具有一陰離子基以提供陽離子交換的能力。
Description
本發明是有關於一種紡絲液、奈米纖維及離子交換過濾材料,且特別是有關於一種靜電紡絲液、聚乙烯醇奈米纖維及離子交換膜。
半導體生產製程日益精密,其汙染的防治重點已由微粒轉移至氣態分子污染物。一般而言,無論是半導體業或是面板製造的光電業,以氨氣(NH3)與銨鹽(NH4 +)等極性氣體或離子氣體之汙染問題較為嚴重。目前除了活性碳濾材與離子交換樹脂外,尚無其他可有效去除上述極性或離子氣體污染物的方法。其中活性碳濾材雖然可濾除部份氣體污染物,但對於吸附極性氣體如氨氣(NH3)與其他微量離子氣體的效果卻很差,而且吸附之物有可能再釋放出來。近年來所開發的離子交換纖維濾材可改善活性碳濾材的問題,但其纖維細度不夠,造成纖維濾材與氣體接觸之表面積較小,導致離子交換效率有限。
因此,本發明之一方面是在提供一種靜電紡絲液,其包括100重量份的聚乙烯醇、10-100重量份的修飾劑、10-100重量份的離子交換試劑與100-2,500重量份的水。上述之修飾劑具有至少一個反應基,該反應基與該聚乙烯醇的氫氧基在100-200℃下進行反應。上述之離子交換試劑具有一極性官能基與一陰離子基,該極性官能基能與該聚乙烯醇的氫氧基形成氫鍵。
依據本發明一實施例,其中該聚乙烯醇的重量平均分子量為15,000-120,000。
依據本發明另一實施例,其中該修飾劑的反應基包括異氰酸基(-NCO)、羧基(-COO-)或硝基(-NO2-),例如可為、、或,其中R1為、或。
依據本發明又一實施例,其中該離子交換試劑的極性官能基包括-OH、-NH2、-COOH、-CHO、-F或前述之任意組合。
依據本發明再一實施例,其中該離子交換試劑
的陰離子基包括-SO3 -、-COO-或-NO2 -。
依據本發明再一實施例,其中該離子交換試劑包括間苯二甲酸-5-磺酸鈉(5-sodium sulfoisophthalate;5-SSIPA)、間苯二甲酸二甲酯-5-磺酸鈉(Sodium dimethyl 5-sulphonatoisophthalate;SIPM)或間苯二甲酸二乙酯-5-磺酸鈉(Dimethyl 5-sulfoisophthalate sodium salt hydrate;SIPE)、2-羥基-1,2,3-丙三羧酸三鈉、乙二胺四乙酸二鉀、2.3-二羥基丁二酸鈉、海藻酸鈉、亞硝酸鈉等其中之一者。
一種聚乙烯醇奈米纖維,其係使用如上所述的靜電紡絲液經由靜電紡絲而得,其中該聚乙烯醇奈米纖維的直徑為50-300nm。
一種離子交換膜,其包括如上所述之聚乙烯醇奈米纖維。
上述發明內容旨在提供本揭示內容的簡化摘要,以使閱讀者對本揭示內容具備基本的理解。此發明內容並非本揭示內容的完整概述,且其用意並非在指出本發明實施例的重要/關鍵元件或界定本發明的範圍。在參閱下文實施方式後,本發明所屬技術領域中具有通常知識者當可輕易瞭解本發明之基本精神及其他發明目的,以及本發明所採用之技術手段與實施方面。
為讓本發明之下述和其他目的、特徵、優點與實施例能更明顯易懂,所附附圖之說明如下:
第1圖顯示的為實驗例3B之在水解前的SEM影像。
第2圖為實驗例3B在水解後的SEM影像。
依據上述,提供一種離子交換膜及其製備方法,以應用於空氣過濾、水過濾與電池隔離膜等等用途上。離子交換膜係以聚乙烯醇經由靜電紡絲得到之超細纖維所形成,上述之聚乙烯醇的部分氫氧基係利用一些試劑修飾過,讓聚乙烯醇不易水解。另外,還在聚乙烯醇的靜電紡絲液中添加離子交換試劑,讓所得纖維膜具有離子交換的能力。
在下面的敘述中,將會介紹上述之離子交換膜的例示結構與其例示之製造方法。為了容易瞭解所述實施例之故,下面將會提供不少技術細節。當然,並不是所有的實施例皆需要這些技術細節。同時,一些廣為人知之結構或元件,僅會以示意的方式在附圖中繪出,以適當地簡化附圖內容。
聚乙烯醇(polyvinyl alcohol;PVA)的靜電紡絲的組成包括聚乙烯醇、修飾劑、離子交換試劑與做為溶劑之水,而且前述四者的含量分別為100重量份(parts by weight)、10-100重量份、10-100重量份與100-2,500重量份。
上述聚乙烯醇的重量平均分子量可為15,000-
120,000,例如50,000-55,000、75,000-80,000、89,000-95,000、107,000-112,000、112,000-120,000。選擇聚乙烯醇為離子交換膜的主要材料,是因為聚乙烯醇具有耐藥性高、造膜性佳、耐光性佳與無毒性等優點。
上述修飾劑的功用為與聚乙烯醇的部分氫氧基進行反應,減少聚乙烯醇之氫氧基的密度,以解決聚乙烯醇容易吸收水氣,並因而分解的問題。而且,由於所使用的溶劑為水,所以修飾劑要能溶解於水中,或是能均勻地分散於水中。
此外,由於為了要讓自靜電紡絲機台的紡嘴紡出來之聚乙烯醇奈米纖維能快乾而不會沾黏在一起,在電紡過程中溫度都保持在50-60℃。因此,修飾劑必須在電紡溫度下不會與聚乙烯醇反應,直到所得聚乙烯醇奈米纖維在100-200℃下加熱烘乾時,修飾劑才能與聚乙烯醇反應,以免紡絲液凝固而阻塞靜電紡絲機台內部的管路。
修飾劑需具有可與聚乙烯醇氫氧基反應的反應基(reactive group)數目至少為1,例如可為1、2或3。當修飾劑具有2個以上的反應基時,修飾劑的作用與交聯劑的作用相同,可讓聚乙烯醇的分子鏈之間產生鍵結。上述之可與聚乙烯醇氫氧基反應的反應基,常見的例如有異氰酸基(-NCO)、羧基(-COO-)或硝基(-NO2-)。
符合上述條件的修飾劑舉例如下:、、
或,其中R1為、或。
上述之離子交換試劑,為一種水溶無毒的有機陰離子,其具有可以與聚乙烯醇之氫氧基形成氫鍵的極性官能基,常見的例如有-OH、-NH2、-COOH、-CHO、-F或前述之任意組合等等。在離子交換試劑中陰離子基的部分,常見的例如有-SO3 -、-COO-或-NO2 -。符合上述條件的離子交換試劑舉例如下:間苯二甲酸-5-磺酸鈉(5-sodium sulfoisophthalate;5-SSIPA)、間苯二甲酸二甲酯-5-磺酸鈉(Sodium dimethyl 5-sulphonatoisophthalate;SIPM)或間苯二甲酸二乙酯-5-磺酸鈉(Dimethyl 5-sulfoisophthalate sodium salt hydrate;SIPE)、2-羥基-1,2,3-丙三羧酸三鈉、乙二胺四乙酸二鉀、2.3-二羥基丁二酸鈉、海藻酸鈉、亞硝酸鈉等其中之一者。
由於做為離子交換試劑的有機陰離子具有可與聚乙烯醇之氫氧基形成氫鍵的極性官能基,因此可以與聚乙烯醇藉由氫鍵結合在一起,形成穩定的混合物。又,由於做為離子交換試劑的有機陰離子具有陰離子基,所以其具有陽離子的交換能力。此外,由於離子交換試劑所帶
的電荷,還可以加強靜電紡絲的電場效應,使得電紡產率增加約2-4倍。
先製備上述之聚乙烯醇靜電紡絲液,然後進行靜電紡絲的步驟,可以得到直徑為50-300nm的奈米纖維。在靜電紡絲時,溫度是維持在50-60℃,讓奈米纖維自紡嘴噴出後能較快乾燥,避免沾黏在一起無法分開,而變成微米纖維。
奈米纖維自紡嘴噴出後,可直接以收集板收集,在收集板上形成多孔的纖維膜。接著,讓纖維膜進入烘箱中,在100-200℃下,讓纖維中之聚乙烯醇與修飾劑進行反應,讓纖維膜可以耐水解,而得到耐水解的離子交換膜。
為了更詳細說明上述離子交換膜的製作方法與優點,以下將以實例的製作流程及各項實驗結果來說明之。
在以下實驗例中,所用聚乙烯醇(PVA)的重量平均分子量包括50,000-55,000 Da(PVA1)、75,000-80,000 Da(PVA2)、89,000-95,000(PVA3)、107,000-112,000 Da(PVA4)以及112,000-120,000 Da(PVA5),所用
的修飾劑包括、、以及,其中R1為及,所用的離子交換試劑可為間苯二甲酸-5-磺酸鈉(5-sodium sulfoisophthalate;5-SSIPA)、間苯二甲酸二甲酯-5-磺酸鈉(Sodium dimethyl 5-sulphonatoisophthalate;SIPM)或間苯二甲酸二乙酯-5-磺酸鈉(Dimethyl 5-sulfoisophthalate sodium salt hydrate;SIPE)、2-羥基-1,2,3-丙三羧酸三鈉、乙二胺四乙酸二鉀、2.3-二羥基丁二酸鈉、海藻酸鈉或亞硝酸鈉。再讓聚乙烯醇、修飾劑、離子交換試劑與水以不同的重量比例來配製紡絲液。接著,讓紡絲液進行靜電紡絲,在收集板上形成纖維膜,再於110-150℃下進行烘乾的步驟,得到成品做為離子交換膜。對照例的紡絲液組成及製備步驟與實驗例相同,但是在紡絲液中沒有添加離子交換試劑。上述之對照例與各實驗例之各組成的重量比都列在下面的表1-a至1-g中。
表1-a:紡絲液的組成
*修飾劑為。
#離子交換試劑為間苯二甲酸二乙酯-5-磺酸鈉(SIPE)。
#離子交換試劑為間苯二甲酸二乙酯-5-磺酸鈉(SIPE)。
接著,讓上述各種組成的紡絲液,分別進行靜電紡絲,得到不同的纖維樣品。
接下來,針對各實驗例所得之纖維,測量其直徑的相關數值。所得數據列在下面的表2-a至2-g中。
在直徑量測面,利用低真空掃描式電子顯微鏡(LV-SEM)來記錄纖維膜的表面影像,再利用影像分析軟體Image-J來分析SEM影像中奈米纖維的纖維直徑,以獲得平均纖維直徑與纖維直徑分佈結果。
從表2-a至2-e實驗例的數據可知,紡絲液中PVA的添加量越多,或修飾劑添加量較多,都會增加PVA奈米纖維直徑的平均值。分別比較對照例A至E與實驗例1A至1E可知,在紡絲液中添加離子交換試劑,會減少PVA奈米纖維直徑的平均值。從表2-f的數據可知,不同修飾劑因添加的比例很少因此對於纖維膜特性影響不大。從表2-g的數據可知,不同離子交換試劑因添加的比例很少因此對於纖維膜特性影響不大。而根據表2-a至2-f,纖維的細度集中率則都相當一致,顯示靜電紡絲可以得到粗細相當均勻的PVA奈米纖維。
將實施例二中得到的不同的PVA奈米纖維在收集板上形成PVA奈米纖維膜。
在PVA奈米纖維膜的性質方面,測試了PVA奈米纖維膜的一些基本性質(如厚度、基重、拉伸強度)以及一些其他性質(如孔隙率、通氣度、離子交換量、氨氣去除率與耐水解試驗)。所得數據分別列在下面的表3-a至3-g與表4-a至4-g中。
先測量PVA奈米纖維膜的基本性質。其中,PVA奈米纖維膜的厚度係使用厚度測定器來測量。取樣時,在正方形PVA奈米纖維膜的四角落、四邊中間與中央共取樣9個點,然後取平均值為其厚度值。
PVA奈米纖維膜的基重的測量法如下。先將PVA奈米纖維膜剪下30cm×40cm的一塊樣品,然後在樣品的四邊各取一塊10cm×10cm的樣品,再於中間區域取出兩塊10cm×10cm的樣品。將六塊樣品稱重後,取平均值,計算出PVA奈米纖維膜的基重。
在拉伸強度的測量方面,是利用拉力測試分析儀來進行分析的。測試前先將PVA奈米纖維膜剪裁成16cm×10cm大小的樣品,再放入拉力測試分析儀的夾具中,進行拉力測試,紀錄樣品斷裂時拉力測試分析儀的施力大小,再計算而得拉伸強度。
從表3-a至3-e的數據來看,PVA奈米纖維膜
的厚度分佈在257-249nm的範圍內,膜基重分佈在2.13-2.53g/m2的範圍內,顯示PVA奈米纖維膜的規格相當均勻。從表3-f的數據可知,不同修飾劑因添加的比例很少因此對於纖維膜基本特性影響不大。從表3-g的數據可知,不同離子交換試劑因添加的比例很少因此對於纖維膜基本特性影響不大。比較實驗例1A-6A、1B-6B、1C-6C、1D-6D及1E-6E的拉伸強度可知,紡絲液中修飾劑/PVA的重量比越高時,PVA奈米纖維膜的拉伸強度就越強。分別比較對照例A至E與實驗例1A至1E可知,在紡絲液中添加離子交換試劑,可以大幅增加PVA奈米纖維膜的拉伸強度。
接著,測量奈米纖維膜的其他性質。其中纖維膜的孔隙率與孔徑集中率的測量方法為將待測之PVA奈米纖維膜剪裁成適當尺寸,固定在孔徑分析儀(購自PM1)的夾具中來進行量測。接著,利用軟體分析所得數據,得到孔隙率與孔徑集中率的數據。
上述之通氣度是利用通氣度測試儀來測量。測量時,PVA奈米纖維膜剪裁成10cm×10cm的大小,再固定於通氣度測試儀的夾具中進行測量。
而PVA奈米纖維膜上磺酸根的含量是用甲苯胺藍(Toluidine Blue O,結構式如下)來測定。由於TBO溶解在NaOH的水溶液中時,是帶著正電荷的,所以TBO可以與PVA奈米纖維膜上帶著負電荷的磺酸根藉由靜電吸引力來互相作用而被吸附在PVA奈米纖維膜上。然後,再用醋酸溶液讓被吸附的TBO脫附下來,再測量其在633nm的
吸光值。在與TBO的濃度標準曲線對照後,可計算出TBO的脫附量,再換算出PVA奈米纖維膜上磺酸根的含量。
由表4-a至4-e的數據可知,各樣品的孔隙率與孔徑集中率都相當一致,孔隙率為80-87%,孔徑集中率皆為90-95%,顯示各樣品的PVA奈米纖維膜的品質相當穩定。從表4-f的數據可知,不同修飾劑因添加的比例很少因此對於纖維膜其他特性影響不大。從表4-g的數據可知,不同離子交換試劑因添加的比例很少因此對於纖維膜其他特性影響不大。比較通氣度的數據,可以發現紡絲液中沒有添加離子交換試劑所得之對照例樣品的通氣度最高,而紡絲液中添加離子交換試劑所得之實驗例樣品的通氣度較低。比較離子交換量的數據可知,紡絲液中離子交換試劑/PVA重量比越高,則離子交換量越高。而增加修飾劑的添加量,在實驗例1A-1E與2A-2E中會減少離子交換量,但是在實驗例3A-3E與4A-4E以及實驗例5A-5E與6A-6E中反而讓離子交換量略增。從表4-g的數據可知,不同種類的離子交換試劑的添加對於離子交換量有些許的不同,整體的離子交換量皆在1,500μeq/g以上。
然後,取用實驗例1B與對照例的樣品,使用氨氣模擬分析儀來測量實驗例1B樣品的氨氣去除率。測試的條件包括溫度為20-25℃,相對濕度為60-65%,氨氣濃度為10ppm,氨氣流速為1000mL/min。結果發現在4.5小時內,當氨氣通過實驗例1B的PVA奈米纖維膜之後,氨氣去除率始終維持100%。對照例B樣品的氨氣去除率則在測試期間內始終維持為0%。顯示實驗例1B的樣品具有優秀的氨氣去除能力。
此外,實驗例所得之PVA奈米纖維膜,在氣體通過前後的壓損十分小,只有8mmH2O左右。但是,一般的HEPA濾材或是玻璃纖維的濾材的壓損至少為15-30mmH2O,顯示上述之PVA奈米纖維膜具有很好的過濾效能,可以達到高效濾網(high-efficiency particulate air;HEPA)的過濾等級。
將實施例三中所得到PVA奈米纖維膜置入烘箱中烘乾,讓該PVA奈米纖維膜中的聚乙烯醇與修飾劑進行反應,以使得該PVA奈米纖維膜獲得耐水解性,而得到耐水解的離子交換膜。
對離子交換膜進行耐水解試驗。將上述之各實驗例1B-6B的靜電紡絲液制得的離子交換膜樣品放在水中浸置2個月後,取出乾燥之。然後使用掃描電子顯微鏡(SEM)來觀察其纖維型態。第1圖顯示的為實驗例3B之離子交換
膜在水解前的SEM影像,第2圖為實驗例3B之離子交換膜在水解後的SEM影像。比較第1圖與第2圖,完全看不出在進行水解試驗2個月後,PVA奈米纖維的外型有任何改變。而且重複測試實施例二與實施例三的所有試驗,各項試驗的結果也都與水解前的實驗數據一樣。因此可知使用修飾劑可以讓PVA奈米纖維具有良好的耐水解能力。
因此,從上面的內容可知,在PVA的靜電紡絲液中添加修飾劑以及離子交換試劑之後,可以改善PVA奈米纖維的耐水解特性,並使本案的離子交換膜具有優異的陽離子交換特性,能快速地吸附陽離子污染物,讓陽離子污染物不再釋放出來。此外,也由於其優異的陽離子交換特性,讓離子交換膜可以處理低濃度的極性氣體,如氨氣。因此,上述離子交換膜可以應用於空氣過濾、水過濾與電池隔離膜等等不同用途上。
雖然本發明已以實施方式揭露如上,然其並非用以限定本發明,任何熟習此技藝者,在不脫離本發明之精神和範圍內,當可作各種之更動與潤飾,因此本發明之保護範圍當視後附之申請專利範圍所界定者為準。
Claims (10)
- 一種靜電紡絲液,其組成包括:100重量份的聚乙烯醇;10-100重量份的修飾劑,該修飾劑具有至少一個反應基,該反應基與該聚乙烯醇的氫氧基在100-200℃下進行反應;10-100重量份的離子交換試劑,該離子交換試劑具有一極性官能基與一陰離子基,該極性官能基能與該聚乙烯醇的氫氧基形成氫鍵;以及100-2,500重量份的水。
- 如請求項1所述之靜電紡絲液,其中該聚乙烯醇的重量平均分子量為15,000-120,000。
- 如請求項1所述之靜電紡絲液,其中該修飾劑的反應基包括異氰酸基(-NCO)、羧基(-COO-)或硝基(-NO2-)。
- 如請求項1所述之靜電紡絲液,其中該修飾劑為、、或,其中R1為、或。
- 如請求項1所述之靜電紡絲液,其中該離子交換試劑的極性官能基包括-OH、-NH2、-COOH、-CHO、-F或前述之任意組合。
- 如請求項1所述之靜電紡絲液,其中該離子交換試劑的陰離子基包括-SO3 -、-COO-或-NO2 -。
- 如請求項1所述之靜電紡絲液,其中該離子交換試劑包括間苯二甲酸-5-磺酸鈉(5-sodium sulfoisophthalate;5-SSIPA)、間苯二甲酸二甲酯-5-磺酸鈉(Sodium dimethyl 5-sulphonatoisophthalate;SIPM)或間苯二甲酸二乙酯-5-磺酸鈉(Dimethyl 5-sulfoisophthalate sodium salt hydrate;SIPE)、2-羥基-1,2,3-丙三羧酸三鈉、乙二胺四乙酸二鉀、2.3-二羥基丁二酸鈉、海藻酸鈉、亞硝酸鈉等其中之一者。
- 一種聚乙烯醇奈米纖維,其係使用如請求項1-7任一項的靜電紡絲液經由靜電紡絲而得。
- 如請求項8所述之聚乙烯醇奈米纖維,其中該聚乙烯醇奈米纖維的直徑為50-300nm。
- 一種離子交換膜,其包括如請求項8所述之聚乙烯醇奈米纖維。
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