• Carbon letters
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• 제16권3호
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• pp.171-182
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• 2015

Mesophase pitch is an important starting material for making a wide spectrum of industrial and advanced carbon products. It is produced by pyrolysis of petroleum residues. In this work, mesophase formation behavior in petroleum residues was studied to prepare environmentally-benign mesophase pitches, and the composition of petroleum residues and its influence on the mesophase formation was investigated. Two petroleum residues, i.e., clarified oil s (CLO-1, CLO-2) obtained from fluid catalytic cracking units of different Indian petroleum refineries, were taken as feed stocks. A third petroleum residue, aromatic extract (AE), was produced by extraction of one of the CLO-1 by using N-methyl pyrrolidone solvent. These petroleum residues were thermally treated at 380℃ to examine their mesophase formation behavior. Mesophase pitches produced as a result of thermal treatment were characterized physico-chemically, as well as by instrumental techniques such as Fourier-transform infrared spectroscopy, nuclear magnetic resonance, X-ray diffraction and thermogravimetry/derivative thermogravimetry. Thermal treatment of these petroleum residues led to formation of a liquid-crystalline phase (mesophase). The mesophase formation behavior in the petroleum residues was analyzed by optical microscopy. Mesophase pitch prepared from CLO-2 exhibited the highest mesophase content (53 vol%) as compared to other mesophase pitches prepared from CLO-1 and AE.

• 한국세라믹학회지
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• 제34권8호
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• pp.817-824
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• 1997

Stabilization is a key stage in the production of advanced carbon/carbon composites (ACC) from mesophase pitch, to render the mesophase infusible and the prevention of puffing during the subsequent carbonization. It is generally known that stabilization process as well as properties of mesophase pitch has a great deal of influence on the properties of the resultant ACC. Hence, it is possible to infer the properties of ACC by examing the stabilized mesophase pitch. In this study, extractions by solvents or acidified solvents extraction were carried out from the A-240 petroleum pitch. The extracted pitches were made into mesophase by heat treatments. Oxidative stabilization by air and non-oxidative stabilization by a chemical free radical initiator were performed. When a soluble polymer is fully stabilized, it should become insoluble in solvents. This phenomenon was used to estimated the degree of stabilization. The non-oxygen stabilized mesophase pitch powder was compared with the air stabilized mesophase pitch powder. FTIR provided additional information on the functional groups.

• 한국세라믹학회지
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• 제33권12호
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• pp.1387-1393
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• 1996

A study on mesophase pitch as a matrix precursor of carbon fiber reinforced carbon (C/C) composite has been recently presented. This study is concerned with the production of mesophase pitch as matrix precursors for C/C composite from coal tar pitch. A commercial coal tar pitch was heat-treated at 25$0^{\circ}C$ for 2 hours to remove low molecular weight fraction from the pitch then increasing the temperature of the pitch to between 350~45$0^{\circ}C$ to produce mesophase pitch. The pitch was continuously stirred during this time and nitrogen gas was continuously bubbled through the pitch. Spherical and bulk mesophases were formed in the pitch after heat-treatment,. Parent and mesophae pitches were characterized by elemental analysis coke yield solubi-lity in tetrahydrofuran and hexane and an optical microscopy to measure the mesiophase content. It was neces-sary to produce C/C composite that a mesophase pitch with about 30-40 vol% mesophase spherulites can be infiltrated into a fiber preform without a filter effect as a matrix precursor conditions. This condition was satisfied with mesophase pitch heat treated at 40$0^{\circ}C$ for 2 hours. The other heat treatment conditions showed the nuclei of mesophase or bulk mesophae which were not satisfied with the matix precursor condition.

• Carbon letters
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• 제5권3호
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• pp.113-117
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• 2004

The mesophase pitch was prepared by adding 1~10 wt% of the borane-pyridine complex (BPC) to decant oil. It was prepared in a reactor held at $450^{\circ}C$ for 2 h in $N_2$ atmosphere. The mesophase pitches were analyzed using thermogravimetric analyzer (TGA), melting point apparatus, X-ray diffraction (XRD) and polarized optical microscope. The coke yield, softening point, toluene insoluble, density and content of anisotropy in the mesophase pitches were increased with BPC contents. The XRD profiles did not show any effect of addition of BPC on the formation of mesophase pitch, while the crystallinity of mesophase pitches was increased when the materials were heat treated with boron compound.

• 한국세라믹학회지
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• 제34권9호
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• pp.963-968
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• 1997

Coal tar pitch was used to study the effect of the pyrolysis conditions to produce mesophase pitch used as a matrix precursor for carbon/carbon composites. The pyrolysis conditions were presented in all cases that the total pressure was 1 atm and the first stage temperature was changed from 25$0^{\circ}C$ to 34$0^{\circ}C$ to remove the low molecular weight compounds in the pitch, and then, heated to 40$0^{\circ}C$ to form anisotropic mesophase as the second stage temperature. The first stage temperature was very affected to form resulting anisotropic mesophase pitch. The resulting mesophase pitches show a significantly increased anisotropic contents upto 30$0^{\circ}C$. However, the contents of mesophase were decreased above 30$0^{\circ}C$. It was the reason that the first stage temperature had been control the number of free radicals to react the aromatic compounds in the pitch to form high molecular weight compound. Therefore, the two stage pyrolysis method could be very effectively used to control various contents of anisotropic polyaromatic mesophase compared to continuous to continuous heating method.

• Bulletin of the Korean Chemical Society
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• 제26권3호
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• pp.418-422
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• 2005

By introducing spin-coating method to the evaporation induced self-assembly (EISA) process, a simple and reproducible route in controlling the mesophase of silica thin films has been developed for the first time in this work. When a comparatively solvent-rich Si-sol (The atomic ratio of TEOS : F127 : HCl : $H_2O$ : EtOH = 1 : 0.006 : 0.2 : 9.2 : 30) was used as coating solution, the mesophase of resultant silica films was selectively controlled by adjusting the spin-on speed. The cubic mesophase has been obtained from the coating at a low rpm, such as 600 rpm, while the 2-D hexagonal mesophase is formed at a high rpm, such as 2,500 rpm. At a medium coating speed, a mixture of cubic and hexagonal mesophase has been found in the fabricated films. The present results confirm that the evaporation rate of volatile components at initial step is critical for the determination of mesopore structures during the EISA process.

• Carbon letters
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• 제24권
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• pp.28-35
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• 2017

We demonstrated an effective way of preparing melt spinnable mesophase pitches via catalytic hydrogenation of petroleum residue (fluidized catalytic cracking-decant oil) and their subsequent thermal soaking. The mesophase pitches thus obtained were analyzed in terms of their viscosity, elemental composition, solubility, molecular weight, softening point and optical texture. We found that zeolite-induced catalytic hydrogenation under high hydrogen pressure contributed to a large variation in the properties of the pitches. As the hydrogen pressure increased, the C/H ratio decreased, and the solubility in n-hexane increased. The mesophase pitch with entirely anisotropic domains of flow texture exhibited good meltspinnability. The mesophase carbon fibers obtained from the catalytically hydrogenated petroleum residue showed moderate mechanical properties.

• Carbon letters
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• 제1권3_4호
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• pp.165-169
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• 2001

The C-type mesophase pitch-based carbon fiber (C-MPCF) was prepared throuch C-type spinnerette and compared the mechanical properties to those of round type mesophase pitch fiber (R-MPCF) and C-type isotropic pitch fiber (C-iPCF). The tensile strength and modulus of C-MPCF were about 18.6% and 35.7% higher than those of R-MPCF. The tensile strength of C-MPCF was 62% higher than that of C-iPCF of the same $8{\mu}m$ thickness because of more linear transverse texture, which could be easily converted to graphitic crystallinity during heat treatment. The torsional rigidity of C-MPCF was 2.37 times higher than that of R-MPCF. The electrical resistivity of C-MPCF was $8{\mu}{\Omega}{\cdot}m$. The C-iPCF shows far lower electrical resistivity than R-iPCF as well as the mesophase carbon fiber because of better alignment of texture to the fiber axis.

• 공업화학
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• 제10권5호
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• pp.690-695
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• 1999

석탄핏치로부터 제조된 메조페이스 핏치의 실험적 연구가 용융상태에서의 유변학적 거동을 알아보고자 수행되었다. 겉보기 점도, 전단변형율, 전단응력, 퀴놀린 불용분(QI), 연화점(SP) 변화 등을 조사하여 다음과 같은 결론을 얻었다. 중합시에 메조페이스의 적당한 함량을 증가시키기 위한 조건으로는 열처리 시간이 5시간, 촉매농도는 3%, 반응온도는 $420^{\circ}C$로 나타났다. 온도상승에 따른 겉보기 점도 변화는 핏치의 열처리 조건에 따라 달라지는데 열처리 온도가 높을수록, 열처리 시간이 길어질수록, 메조페이스 함량이 증가할수록 커지며, 유동도는 작아진다. $270^{\circ}C$ 이후의 용융 메조페이스 핏치의 유변학적 거동은 $375^{\circ}C$ 이하에서는 Newtonian fluid의 성질을 띠며 그 이상에서는 Non Newtonian fluid의 거동을 보이며 Casson 모델에 잘 일치됨을 알 수 있었다.

• 한국수소및신에너지학회논문집
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• 제27권4호
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• pp.421-430
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• 2016

To prepare mesophase pitches through low energy process, pyrolysis fuel oil with $AlCl_3$ has been modified using two-step heat treatment which is heat-treated at $330^{\circ}C$ for 3~5 h after pre-treatment at $250^{\circ}C$. The result of polarized optical microscope observation, mesophase is not observed in pitches carried out only pre-heat treatment. While mesophase content is significantly increased from 9% to 100% according to increasing secondary heat treatment time from 3 h to 5 h. Synthesizing of the mesophase pitch at low temperature of $330^{\circ}C$ is attributed to decrease of viscosity of the pitches carried out first heat treatment with $AlCl_3$. The result of Fourier-transform infrared spectroscopic analysis, it is expected that aromatization of aliphatic compounds is dominant at early secondary heat treatment, on the other hand, polycondensation reaction becomes dominant as secondary heat treatment time increases. Aromaticity and stacking height of the pitches secondary heat treated for 5 hours are more increased about 25% and 107%, respectively, than that of pitches carried out only first heat treatment.