本文選題：軟模板法 + 酚醛樹脂��； 參考：《大連理工大學(xué)》2016年碩士論文

【摘要】：膜分離技術(shù)作為一種新型氣體分離技術(shù),因其高性能、低成本、操作簡單等優(yōu)點(diǎn)而備受矚目。炭膜是一種由含碳物質(zhì)經(jīng)高溫?zé)峤馓炕傻男滦吞炕げ牧?具有耐高溫、抗腐蝕、耐酸堿、生物相容性好、孔徑可調(diào)且氣體分離性能優(yōu)異等特點(diǎn),因此應(yīng)用前景十分廣闊。均質(zhì)炭膜因質(zhì)脆、強(qiáng)度低無實(shí)用價(jià)值。為了實(shí)現(xiàn)其實(shí)際應(yīng)用,通常制備成具有一定強(qiáng)度的復(fù)合炭膜,即在具有一定機(jī)械強(qiáng)度的支撐體上復(fù)合一層炭膜前驅(qū)體,經(jīng)高溫?zé)峤庑纬蓮?fù)合炭膜。然而,作為支撐體的多孔材料通�？讖捷^大,表面存在針眼或缺陷,容易轉(zhuǎn)移到分離層表面,影響復(fù)合炭膜的分離性能。所以,對支撐體表面進(jìn)行修飾是制備高性能復(fù)合炭膜的關(guān)鍵。介孔炭材料是一種具有較高比表面積,均一孔徑結(jié)構(gòu)的功能型材料,是修飾炭膜支撐體缺陷的理想材料。本論文利用軟模板法,分別采用酸、堿催化劑合成介觀相酚醛樹脂,修飾支撐體,并在此基礎(chǔ)上涂覆分離層,制備復(fù)合炭膜。主要探討了介觀相酚醛樹脂的合成反應(yīng)溫度、時間以及炭化工藝等對介孔炭結(jié)構(gòu)的影響。通過XRD、N2吸附、TEM及氣體滲透裝置等手段,對所制備的介孔炭的孔結(jié)構(gòu)特性、微觀形貌及氣體滲透分離性能進(jìn)行表征。得到如下結(jié)果：1、在酸性催化劑下,當(dāng)合成時間為3 h,老化時間為72h,炭化溫度為6000C,恒溫時間為2h,制備得到的介孔炭為蠕蟲狀孔結(jié)構(gòu),其孔容和比表面積分別為0.613cm3/g和685.75m2/g,平均孔徑為2.2 nm。用其制備介孔炭膜,其氧氣通量為77390 barrer,氧氮選擇性為0.99。在堿性催化劑參與下,當(dāng)反應(yīng)溫度為70℃,合成時間為1 h,炭化溫度為600 ℃,恒溫時間為4 h,制備得到的介孔炭有序度良好,其平均孔徑為4.0 nm;制備的介孔炭膜,其氧氣通量為24850 barrer,氧氮選擇性為1.11。2、采用介觀相酚醛樹脂聚合物修飾炭膜支撐體,得到的支撐體孔徑均一,表面更加平整,滲透通量維持在2000GPU左右。3、采用旋涂法在修飾后的支撐體上涂覆分離層,制備得到了具有一定的氣體分離性能的復(fù)合炭膜。發(fā)現(xiàn)介觀相酚醛樹脂的合成方法對所制備的復(fù)合炭膜的氣體分離性能有一定的影響。以酸性催化劑合成的介觀相酚醛樹脂修飾的支撐體制備的復(fù)合炭膜其氧氣通量為1615 GPU,氧氮選擇性為2.07。以堿酸性催化劑合成的介觀相酚醛樹脂修飾的支撐體制備的復(fù)合炭膜其氧氣通量為1193 GPU,氧氮選擇性為1.53。
[Abstract]:As a new gas separation technology, membrane separation technology has attracted much attention because of its high performance, low cost and simple operation. Carbon film is a kind of new carbon base membrane material which is prepared by pyrolysis and carbonization of carbonaceous material at high temperature. It has the characteristics of high temperature resistance, corrosion resistance, acid and alkali resistance, good biocompatibility, adjustable pore size and excellent gas separation performance. Therefore, the application prospect is very broad. Homogeneous carbon film has no practical value because of its brittleness and low strength. In order to realize its practical application, the composite carbon film with a certain strength is usually prepared, that is, the composite carbon film is formed by pyrolysis at high temperature on the support with a certain mechanical strength. However, porous materials, which are usually used as supports, usually have large pore size and have pinhole or defects on the surface, which can easily be transferred to the surface of the separation layer and affect the separation performance of the composite carbon membrane. Therefore, the surface modification of the support is the key to the preparation of high performance composite carbon film. Mesoporous carbon is a functional material with high specific surface area and homogeneous pore structure. It is an ideal material for modifying the defects of carbon membrane support. In this paper, mesoscopic phenolic resin was synthesized with acid and alkali catalyst by soft template method, and modified with support, and then coated with separation layer to prepare composite carbon membrane. The effects of reaction temperature, reaction time and carbonization process on the structure of mesoporous carbon were investigated. The pore structure, micromorphology and gas permeation performance of the prepared mesoporous carbon were characterized by means of XRDN _ 2 adsorption TEM and gas permeation apparatus. The results are as follows: 1. Under acidic catalyst, the mesoporous carbon is worm-like structure when the synthesis time is 3 h, the aging time is 72 h, the carbonization temperature is 6 000 C, and the constant temperature time is 2 h. The pore volume and specific surface area are 0.613cm3/g and 685.75m2 / g, respectively. The average pore size is 2.2 nm. The oxygen flux and oxygen nitrogen selectivity of mesoporous carbon membrane were 77390 barrer and 0.99, respectively. When the reaction temperature was 70 鈩，

本文編號：1936647