本课题以沥青基炭纤维为原料制备分子筛型沥青基活性炭纤维。详细开展了分子筛型活性炭纤维的炭化、空气氧化及二氧化碳活化法、空气氧化及水蒸气活化法、水蒸气和二氧化碳两步活化法这三种复合活化工艺的研究，并以甲烷/二氧化碳分离体系为研究对象，考察了沥青基活性炭纤维的筛分性能。 对于通用级沥青基炭纤维，炭化可以较为显著地提高其物理活化产品的收率、比表面积以及吸附性能。炭化明显降低了炭纤维及活性炭纤维的结晶有序度，有利于类石墨晶层堆积的无序化和大量微孔的形成。 空气氧化处理使得沥青基炭纤维形成了大量极微孔和反应活性点，这有利于活化剂在更温和的反应条件下与炭纤维表面无定形碳或边缘碳原子反应从而形成大量微孔，使得孔径分布变窄，空气氧化及二氧化碳活化法所制备的沥青基活性炭纤维不仅收率提高而且比表面积也得到一定提高。由于空气和水蒸气的反应性都很强，容易与炭纤维表面更稳定的微晶发生反应，使表面已有的微孔孔壁塌陷从而刻蚀出大孔，所以空气氧化及水蒸气活化法不适于制备孔径分布窄的沥青基活性炭纤维。水蒸气与沥青基炭纤维的反应活性高于二氧化碳，水蒸气和二氧化碳两步活化法可以制备出高比表面积的沥青基活性炭纤维。 对所制备的沥青基活性炭纤维进行氮气等温吸附线表征表明其吸附行为属于代表微孔型吸附剂吸附行为的I型吸附。甲烷/二氧化碳分离实验表明空气氧化及二氧化碳活化法制备的沥青基活性炭纤维筛分性能最好，空气氧化及水蒸气活化法不适于制备孔径分布窄的沥青基活性炭纤维。空气氧化处理、二氧化碳850℃活化60min制备的沥青基活性炭纤维以及在活化温度850℃水蒸气活化30min、二氧化碳活化80min条件下制备的沥青基活性炭纤维通过孔径分布测试表明其微孔孔径集中在0.90～0.98nm之间，分子筛特征显著。

In this work, pitch-based activated carbon fibers (PACF) were prepared from pitch-based carbon fiber (PCF) through oxidation, carbonization and activation. The activation process and reaction mechanism of PACF with narrow pore size distributions and highly selective adsorption were studied. The preparation conditions, microstructure, adsorption ability and the effect of microstructure on separation ability of PACF were discussed. In this paper the work mainly contains the studies on carbonization and three kind multiplex activation processes, the tests on adsorption ability of PACF and investigation on separation ability of PACF with CH4/CO2 separation system as study object. The mainly results as follows: The results from the study of carbonization influences on the properties of PACF indicate that carbonization can improve the yield, surface area and adsorption ability of PACF evidently. Carbonization can reduce the crystal order degree of PCF and PACF evidently. So carbonization is propitious to disorder of graphite-like crystal layer and formation of a great deal micropores. The experiment studies on the three multiplex activation methods indicate that air oxidation makes PCF to form a great deal micropores and active points of reaction. This is propitious to that active agents react with amorphism carbon or fringe carbon atoms under the more mild reaction condition and pore size distribution becomes narrow. Meanwhile, the yield and surface area of PACF are increased at a certain extent. Because air and vapor all have high reactivity and they are so easy to react with more steady crystallite that make the pore wall falls in and bring some big pore, so this makes against producing PACF with narrow pore distribution. The reactivity of vapor with PCF is higher than carbon dioxide. The multiplex activation method about vapor and carbon dioxide can prepare PACF with high surface area. The characterization about physisorption isotherm of prepared PACF indicates that the adsorption behavior of PACF belongs to the type I adsorption that represented micropore sorbents. The results of CH4/CO2 separation experiment indicate that the PACFs prepared by the multiplex method of air oxidation and carbon dioxide activation have the best separation ability. The multiplex method of air oxidation and vapor activation is unfit for preparing PACF with narrow pore size distribution. The pore size of PACFs that prepared under the conditions with air oxidation and carbon dioxide activated in 60 minutes at the temperature 850℃, vapor activated in 30 minutes and carbon oxidation activated in 80 minutes at the temperature 850℃ is concentrated on the range among 0.90~0.98 nm. The character about molecular sieve is evident.