本文選題：納濾膜 + 表面接枝��； 參考：《浙江理工大學(xué)》2017年碩士論文

【摘要】：納濾膜具有高效率、低能耗等優(yōu)點(diǎn),被廣泛用于地表水有機(jī)物、地下水硬度、部分溶解性鹽的去除和染料分離濃縮等領(lǐng)域,但膜污染則是目前制約納濾膜規(guī)�；瘧�(yīng)用的關(guān)鍵因素。因而,提高納濾膜的抗污染性能對(duì)于納濾膜技術(shù)的發(fā)展具有重要意義。本課題選用3-氨基丙基三乙氧基硅烷(APTES)作為改性材料,利用初生態(tài)聚酰胺復(fù)合納濾膜表面的殘留酰氯基團(tuán)與APTES之間的反應(yīng),對(duì)聚哌嗪酰胺納濾膜進(jìn)行表面接枝改性,研究表面改性對(duì)復(fù)合膜表面性質(zhì)、分離性能及抗污染性能的影響規(guī)律。采用ATR-FTIR、XPS、FE-SEM、AFM、接觸角和Zeta電位等手段對(duì)復(fù)合膜表面性質(zhì)和形貌結(jié)構(gòu)進(jìn)行表征。采用錯(cuò)流分離裝置系統(tǒng)地研究了復(fù)合膜的切割分子量及膜對(duì)不同無(wú)機(jī)鹽和有機(jī)染料的分離性能。以腐殖酸(HA)、陽(yáng)離子表面活性劑(DTAB)和牛血清蛋白(BSA)作為特征污染物,考察復(fù)合膜的抗污染性能。結(jié)論如下:(1)ATR-FTIR和XPS結(jié)果表明,初生態(tài)復(fù)合膜表面未反應(yīng)的酰氯基團(tuán)和APTES發(fā)生了酰胺化或酯化反應(yīng),利用表面二次反應(yīng)技術(shù)可以成功地將APTES接枝到復(fù)合膜的表面;分離層孔徑由0.88 nm變?yōu)?.84 nm,復(fù)合膜表面變得更加的致密,復(fù)合膜的切割分子量由290 Da降至260 Da。改性使粗糙度略微上升,均在20 nm以下,表面改性并未對(duì)其表面粗糙度造成很大的影響。靜態(tài)接觸角測(cè)試表明,復(fù)合膜接觸角由58°下降至46°,復(fù)合膜的親水性有所增加。Zeta測(cè)試顯示復(fù)合膜表面的電負(fù)性下降,且接枝的濃度越大,電負(fù)性下降的越多。(2)APTES的濃度及反應(yīng)時(shí)間影響改性膜的表面性質(zhì)和分離性能。增加APTES濃度和延長(zhǎng)反應(yīng)時(shí)間可增強(qiáng)接枝效果,但酰胺化反應(yīng)或酯化反應(yīng)與酰氯的水解反應(yīng)為競(jìng)爭(zhēng)關(guān)系,繼續(xù)增大反應(yīng)濃度或延長(zhǎng)反應(yīng)時(shí)間改性效果變化不大。為了得到綜合分離性能最優(yōu)的復(fù)合膜,最終確定APTES改性濃度為0.4 wt%,反應(yīng)時(shí)間為4 min,在此條件下,根據(jù)XPS分析可知,初生態(tài)膜表面的殘留酰氯基團(tuán)發(fā)生酰胺化、酯化和水解反應(yīng)的比例為13.2%、17.6%和69.2%。(3)聚酰胺復(fù)合納濾膜表面接枝APTES以后,在25℃、0.5 MPa的操作條件下,復(fù)合膜的水通量由67.9 LMH上升至73.3 LMH,脫鹽率由97.83%下降至96.08%,二者之間存在著Trade-off效應(yīng);復(fù)合納濾膜對(duì)無(wú)機(jī)鹽的截留順序?yàn)镹a2SO4MgSO4NaClMgCl2,符合一般荷負(fù)電納濾膜對(duì)無(wú)機(jī)鹽的截留規(guī)律;染料分離試驗(yàn)發(fā)現(xiàn),復(fù)合膜對(duì)染料的截留順序?yàn)?結(jié)晶紫㧐玫瑰紅B㧐甲酚紅㧐亞甲基藍(lán)㧐中性紅,改性膜對(duì)染料的脫除率、通量皆優(yōu)于原膜;染料的分離提純實(shí)驗(yàn)表明,經(jīng)過(guò)10 h的染料提純?cè)囼?yàn),料液中的鹽含量分別降至起始濃度的5.53%和0.62%,提純時(shí)間縮短,提純通量較原膜高出7.0%。(4)聚酰胺復(fù)合納濾膜表面接枝APTES可提高復(fù)合膜的抗污染性能。對(duì)于DTAB、HA和BSA水溶液,改性膜的通量下降速率明顯低于原膜,原膜與改性膜過(guò)濾DTAB溶液的平衡通量下降率分別為39.6%和29.7%、過(guò)濾HA溶液的平衡通量下降率分別為28.0%和25.8%、過(guò)濾BSA溶液的平衡通量下降率分別為33.7%和26.8%。經(jīng)過(guò)原位清洗以后,改性膜的通量恢復(fù)率高于原膜,DTAB污染膜的通量恢復(fù)率由原始膜的90.6%提高到改性膜的96.0%、HA污染膜的通量恢復(fù)率由原始膜的88.0%提高到改性膜的93.0%、BSA污染膜的通量恢復(fù)率由原始膜的82.5%提高到改性膜的91.3%。
[Abstract]:Nanofiltration membrane has many advantages, such as high efficiency, low energy consumption and so on. It is widely used in the fields of surface water organic matter, groundwater hardness, removal of partial dissolved salt and dye separation and concentration, but membrane pollution is the key factor restricting the large-scale application of nanofiltration membrane. Therefore, the improvement of the anti pollution performance of nanofiltration membrane has been developed for nanofiltration membrane technology. It is important to use 3- amino propyl triethoxy silane (APTES) as a modified material. The surface grafting of polypiazine amide nanofiltration membrane was modified by the reaction between the residual acyl chloride group and APTES on the surface of the membrane surface of the first ecological polyamide composite nanofiltration membrane. The surface properties, separation properties and pollution resistance of the surface modification on the composite membrane were studied. The surface properties and morphology of the composite films were characterized by means of ATR-FTIR, XPS, FE-SEM, AFM, contact angle and Zeta potential. The cutting molecular weight of the composite membrane and the separation performance of the membrane to different inorganic salts and organic dyes were systematically studied. Humic acid (HA) and cationic surfactant (D) were used. TAB) and bovine serum protein (BSA) as the characteristic pollutants to investigate the anti pollution properties of the composite membrane. Conclusions as follows: (1) the results of ATR-FTIR and XPS showed that the acyl chloride group and APTES of the surface of the first ecological composite membrane were amidation or esterification, and the surface of the composite membrane could be successfully grafted on the surface of the composite membrane by using the surface two reaction techniques. The pore size of the separation layer changed from 0.88 nm to 0.84 nm, and the surface of the composite membrane became more compact. The cutting molecular weight of the composite membrane was reduced from 290 Da to 260 Da., and the roughness slightly increased, all of which were below 20 nm. The surface modification did not greatly influence the surface roughness. The static contact angle test showed that the contact angle of the composite film decreased from 58 to 46. The hydrophilicity of the composite film increased by.Zeta test. The electronegativity of the surface of the composite membrane decreased, and the greater the concentration of the graft, the more electronegativity decreased. (2) the concentration and reaction time of APTES influence the surface properties and separation properties of the modified membrane. Increasing the APTES concentration and prolonging the reaction time can enhance the graft effect, but the acylation reaction or ester The reaction was competitive with the hydrolysis reaction of acyl chloride, and the effect of the reaction time was not changed. In order to obtain the composite membrane with the best comprehensive separation performance, the APTES modified concentration was determined to be 0.4 wt% and the reaction time was 4 min. Under this condition, the residual acylation of the surface of the first ecological membrane could be found. After the chlorination of the chlorine group, the proportion of the esterification and hydrolysis reaction is 13.2%, 17.6% and 69.2%. (3) polyamide composite nanofiltration membrane graft APTES. Under the conditions of 25 C and 0.5 MPa, the water flux of the composite film rises from 67.9 LMH to 73.3 LMH, the desalination rate decreases from 97.83% to 96.08%, and there is a Trade-off effect between the two. The retention order of the membrane to inorganic salts is Na2SO4MgSO4NaClMgCl2, which conforms to the rule of the retention of inorganic salts in the general negative electric nanofiltration membrane. The dye separation test found that the retention order of the dyes by the composite membrane is crystal violet, rose red B, cresol red, methylene blue, neutral red, and the flux of the modified membrane is superior to the original film; the separation and extraction of the dye The pure experiment showed that after 10 h dye purification test, the salt content in the liquid was reduced to 5.53% and 0.62% of the initial concentration, the purification time was shortened, and the surface grafting APTES of 7.0%. (4) polyamide composite nanofiltration membrane higher than the original membrane could improve the anti pollution performance of the composite membrane. For DTAB, HA and BSA aqueous solutions, the flux decline rate of the modified membrane was reduced. The rate of balance flux of the original film and modified membrane filtration DTAB solution was 39.6% and 29.7%, respectively, and the balance flux decreased by 28% and 25.8% in the filtered HA solution, respectively, and the decrease rate of the equilibrium flux of the filtered BSA solution was 33.7% and 26.8%. after the in-situ cleaning, and the flux recovery rate of the modified membrane was higher than that of the original film and DTAB. The flux recovery rate of the dyed membrane is increased from 90.6% of the original film to 96% of the modified membrane. The flux recovery rate of the HA fouling film is increased from 88% of the original film to 93% of the modified membrane. The flux recovery rate of the BSA fouling film is increased from 82.5% of the original film to the 91.3%. of the modified membrane.
【學(xué)位授予單位】：浙江理工大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2017
【分類號(hào)】：TQ051.893

【共引文獻(xiàn)】

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5 張s，

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