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隨著經(jīng)濟(jì)的快速發(fā)展以及人們對(duì)環(huán)境重視程度的提高，聚砜膜分離技術(shù)以其高效、節(jié)能、環(huán)保、選擇性高、裝置靈活等特點(diǎn)，在工農(nóng)業(yè)水處理、海水淡化、生物醫(yī)學(xué)等方面有著廣泛的應(yīng)用。聚砜由于其耐酸堿腐蝕，抗氧化能力強(qiáng)，具有優(yōu)良的力學(xué)性能，適合在壓力環(huán)境下使用，常被用于膜分離材料。但由于聚砜材料自身親水性差，膜分離過程中，生物懸浮物或大分子/膠體沉積易在膜表面和膜孔內(nèi)部造成膜污染。此外，聚砜質(zhì)脆，柔韌性較差的缺點(diǎn)也限制了其在其他領(lǐng)域的應(yīng)用。 本文針對(duì)聚砜樹脂柔韌性不足、親水性差的問題，通過羥基封端的聚砜和異氰酸酯基封端的聚氨酯預(yù)聚體共聚制備聚氨酯改性聚砜樹脂，結(jié)合聚氨酯的結(jié)構(gòu)特性，改善聚砜樹脂柔韌性和親水性。論文主要包括以下內(nèi)容：制備了以羥基封端的聚砜，得到一系列不同分子量聚砜，研究了該合成方法的最佳合成條件及影響因素；合成了以異氰酸酯（NCO）基團(tuán)封端的聚氨酯預(yù)聚體；用羥基封端的聚砜和聚氨酯預(yù)聚體共聚，合成了聚氨酯改性聚砜（PSF-PU）樹脂，研究了其制備的最佳條件；利用 ATR-IR、1HNMR、GPC手段對(duì)聚氨酯改性聚砜樹脂的結(jié)構(gòu)進(jìn)行了表征；將改性的聚砜樹脂制備成膜，測(cè)試該膜材料的斷裂伸長率、抗張強(qiáng)度、表面接觸角，玻璃化轉(zhuǎn)變溫度等物理性能；將改性的聚砜樹脂制備成平板超濾膜，測(cè)定超濾膜的純水通量以及對(duì)PEG-10000分子的截留率等分離性能。再用牛血清蛋白模擬動(dòng)態(tài)吸附，測(cè)試超濾膜在使用過程中的抗污染性。 通過調(diào)節(jié)聚砜以及聚氨酯改性聚砜樹脂的制備條件，研究各因素的影響，確定聚砜的合成最佳條件為：反應(yīng)單體濃度40%，甲苯用量35 mL，帶水時(shí)間2 h，縮聚反應(yīng)溫度160℃，時(shí)間4 h。聚氨酯改性聚砜樹脂的最佳合成條件為：反應(yīng)溫度80℃，時(shí)間6 h；反應(yīng)物濃度25%。 ATR-IR、1HNMR、GPC分析表明，聚砜的端羥基與聚氨酯預(yù)聚體的端異氰酸酯基發(fā)生了反應(yīng)，聚氨酯預(yù)聚體與聚砜發(fā)生反應(yīng)，具有聚氨酯特性的鏈段成功引入到聚砜上。 聚氨酯改性聚砜樹脂膜的玻璃化轉(zhuǎn)變溫度為188.33℃，比聚砜高2.75℃；斷裂伸長率為18.62%，比聚砜膜高4.38%；水接觸角比聚砜小21.5° ~ 22.3°，親水性得到提高。 聚氨酯改性聚砜樹脂超濾膜的純水通量增加4.36 mL•cm-2•h-1，對(duì)于PEG-10000分子的截留率提高4%，分離性能提高；對(duì)牛血清蛋白的總污染度減小0.18389，不可逆污染減小減少0.12243，抗污染性能提高。 將聚氨酯改性聚砜樹脂超濾膜和聚砜超濾膜處理皮革脫毛廢水測(cè)定超濾膜對(duì)廢水中的硫化物、COD、色度、懸浮物及灰分的截留率。測(cè)定結(jié)果表明聚氨酯改性聚砜樹脂超濾膜相比聚砜超濾膜對(duì)于皮革脫毛廢水中的各項(xiàng)指標(biāo)均有較高的截留率。 Because of the rapid economic development and the continuous improvement of people's attention to the environment, polysulfone separation membrane technology, depending on its high efficiency, energy saving, environmental protection, high selectivity and device flexibility, has been widely used in the industrial and agricultural water treatment, desalination, biomedical applications and so on. Due to its acid and base resistance, anti-oxidation ability, excellent mechanical properties, adaptability for using under pressure, polysulfone was always selected for membrane material. However, hydrophilicity of polysulfone was poor, which could easily result in the membrane fouling from biological suspended solids or macromolecules/colloids deposited on the membrane surface and membrane inner holes. Besides, the application of polysulfone material in other fields is limited as its brittleness and poor flexibility. In this thesis, in order to improve hydrophilicity and flexibility of polysulfone resin, firstly, the synthesis of hydrophilic isocyanate group ended polyurethane and the hydroxyl ended polysulfone was carried out. Then the copolymerization of the hydroxyl ended polysulfone and the isocyanate group ended polyurethane was carried out. The preparation method, the optimum preparation conditions and influence factors of polysulfone and polyurethane modified polysulfone resin were studied by comparing the viscosity of the products. The structures of polyurethane modified polysulfone resin was characterized with ATR-IR, 1HNMR and GPC. The polyurethane modified polysulfone membrane resin membrane was prepared through L-S phase inversion method. The elongation at break, tensile strength contact angle, the glass transition temperature and other physical properties of modified membrane was tested. The polyurethane modified polysulfone resin ultrafiltration membrane was prepared. The pure water flux and the reject rate of the PPG-10000 of the ultrafiltration membrane were tested through the ultrafiltration cup. The antifouling property was tested by assessing the flux loss of bovine serum albumin in the process of dynamic adsorption. We studied the preparation conditions of polysulfone . Finally, we found that the monomer concentration was 40%, the dosage of toluene was 35 mL, the dewater time was 2 h, condensation reaction temperature was 160℃ and condensation reaction time was 4 h. The best copolymerization temperature of polysulfone and polyurethane copolymerization was 80℃; The best copolymerization time was 6 h; The best copolymerization concentration was 25%. Tg of polyurethane modified polysulfone resin membrane was 188.33℃, which was 2.75℃ higher than the polysulfone. Elongation at break of polyurethane modified polysulfone membrane was 18.62%, 4.38% higher than the polysulfone membrane. The water contact angle of polyurethane modified polysulfone membrane are 21.5°~22.3° lower than polysulfone membrane. The pure water flux of polyurethane modified polysulfone resin ultrafiltration membrane was 4.36 mL•cm-2•h-1 higher than polysulfone membrane and the reject rate was 4% higher than polysulfone membrane. The pollution resistance performance of polyurethane modified polysulfone ultrafiltration membrane was better than polysulfone ultrafiltration membrane. Total pollution reduced by 0.18389, irreversible pollution reduced by 0.12243. When we used the flat ultrafiltration membrane for treating laboratory leather unhairing waste-water, the application performance of the flat ultrafiltration membrane was assessed by comparing the chroma, ash content, sulfide, suspended solids, chemical oxygen demand (COD) between influent and effluent. We found that the reject rate of COD, sulfide, chroma, suspended solids and ash treated by polyurethane modified polysulfone resin ultrafiltration membrane were higher than by polysulfone ultrafiltration membrane. |
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修改后的文章： 第一段： With the rapid development of economy and the increasing attention people pay on the environment, the separation technology of polysulfone membrane depending on its high efficiency, energy saving, environmental protection, high selectivity and device flexibility, has been widely used in the water treatment of the industrial and agricultural, desalination, biomedical applications and so on. Due to its acid and alkali resistance, anti-oxidation ability, excellent mechanical properties, fitness for using under pressure, polysulfone is always selected as the material of membrane. However, the poor hydrophilicity of polysulfone could easily result in the membrane fouling from biological suspended solids or macromolecules/colloids deposited on the membrane surface and membrane inner holes. Besides, the brittleness and poor flexibility of polysulfone material has limited its application in other fields. |
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