• 한국기계연구소 소보
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• s.15
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• pp.37-46
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• 1985

Properties of Precursor pitch derived from petroleum residue were studied physical and chemical analysis method for investigation of production of pitch fiber. For preparing of those precursor pitches it was carried out a temperature and time variation experiment i reactor. It was demonstrated the precursor pitch prepared in this study to have a similar properties to Ashland precursor pitch capable of bulk mesophase formation from the results of the basic analysis, that is, molecular weight distribution, coking yield, carbon content, chemical composition, etc.

• Journal of the Korean Ceramic Society
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• v.33 no.12
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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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• v.15 no.4
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• pp.247-254
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• 2014

In this work, thermal treatment accompanied with different acid treatments was applied to a commercial coal tar pitch (CTP) to obtain a spinnable precursor pitch for carbon fiber. In the case of thermal treatment only, a relatively high reaction temperature of between $380^{\circ}C$ and $400^{\circ}C$ was required to obtain a softening point (SP) range of $220^{\circ}C-260^{\circ}C$ and many meso-phase particles were created during the application of high reaction temperature. When nitric acid or sulfuric acid treatment was conducted before the thermal treatment, the precursor pitch with a proper SP range could be obtained at reaction temperatures of $280^{\circ}C-300^{\circ}C$, which were about $100^{\circ}C$ lower than those for the case of thermal treatment only. With the acid treatments, the yield and SP of the precursor pitch increased dramatically and the formation of meso-phase was suppressed due to the lower reaction temperatures. Since the precursor pitches with acid and thermal treatment were not spinnable due to the inhomogeneity of properties such as molecular weight distribution and viscosity, the CTP was mixed with ethanol before the consecutive nitric acid and thermal treatments. The precursor pitches with ethanol, nitric acid, and thermal treatments were easily spinnable, and their spinning and carbon fiber properties were compared to those of air blowing and thermal treated CTP.

• Carbon letters
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• v.6 no.3
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• pp.173-180
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• 2005

In this study, AR (aromatic resin) pitch was employed as the matrix-precursor for carbon/carbon composite because it exhibits much higher coke yield than coal tar pitch. As a result, a fabrication process of carbon/carbon composites can be shortened. It has been known that the pitches may cause swolling problem during the carbonization process. In order to restrain the swelling occurrence, a small quantity of carbon black was added to the AR pitch. Due to addition of carbon black the swelling was decreased largely and the perform can be infiltrated with the AR pitch. The densification efficiency of the performs was compared with various matrix-precursors. The coke yield of matrixprecursors, the morphology and the degree of graphitization of carbon matrix were analyzed.

• Carbon letters
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• v.2 no.2
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• pp.99-104
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• 2001

Partial mesophase (PM) pitch precursor was prepared from fluidized catalytic cracking-decant oils (FCC-DO) by chemical reaction in the presence of $Br_2$. The PM pitch heated-treatment at $420^{\circ}C$ for 9 h exhibited the softening point of $297^{\circ}C$ with 23% yield, and 55% anisotropic content. The PM pitch precursor was melt-spun through circular nozzle by pressurized $N_2$, stabilized at $310^{\circ}C$, carbonized at $700^{\circ}C$, $1000^{\circ}C$, and $1200^{\circ}C$. The enough stabilization introduced 16.4% of the oxygen approximately. The stacking height ($L_{c002}$) and interlayer spacing ($d_{002}$) of the as-spun fibers were 4.58 nm and $3.45{\AA}$ and the value became minimum and maximum at $700^{\circ}C$ respectively in the carbonization procedure. The tensile strength increased with an increase in the heat treatment temperature exhibiting highest value of 750 MPa at $1200^{\circ}C$ carbonization.

• Journal of Industrial and Engineering Chemistry
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• v.67
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• pp.276-283
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• 2018

For the first time, polyvinyl chloride (PVC) was used as an easily-handled chlorine source for preparation of isotropic pitch-based carbon fiber (IPCF) incorporating ethylene bottom oil (EO) as a raw material. Pitch precursors were prepared by the chlorination-dehydrochlorination triggered by chlorine radicals originated from PVC; aromatization and poly-condensation reactions occurred by polyene-type radicals from PVC. Radical production and co-carbonization were facilitated by pretreatments of EO through vacuum distillation, bromination, and additional heat treatment. Pitches were prepared by the co-carbonization of pretreated EO and EO containing 20 wt% PVC, and had higher yields and better spinnability than those by simple distillation.

• Journal of the Korean Ceramic Society
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• v.34 no.9
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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.

• Carbon letters
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• v.10 no.3
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• pp.198-201
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• 2009

Among other filters such as light filter, wave filter, air filter, ultra filter and filter paper, a novel adsorption filter from thermostable polyester nonwoven fabrics immobilized with functional super activated carbon by means of quinoline soluble, activateable isotropic pitch binder were developed in this study. The activated carbon precursor is available in the market branded as coconut shell based activated carbon(CCS-AC) produced by Dongyang Carbon Co. Ltd. BET-surface area of this precursor was $1,355\;m^2/g$, after KOH-activation it increased over $2,970\;m^2/g$ and was named as super activated carbon. In the preliminary research, this precursor was impregnated with $PdCl_2$(0.188 wt%) $KMnO_4$(3 wt%) and redox-agent(CuCl2, 0.577 wt%) in order to promote TOF up to 100/h and Selectivity up 99% and patented as a functional AC for the ethylene adsorption. The enhancement of the isotropic pitch binder to the AC-immobilized adsorption filter was BET-surface area upgraded by $266\;m^2/g$ and promoted the Iodine- and MB-adsorption by 1.4 times, respectively and also micro pore wide ranges < $5{\AA}{\sim}30\;{\AA}$ >.

• Korean Chemical Engineering Research
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• v.43 no.6
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• pp.745-750
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• 2005

Naphtha cracking bottoms(NCB) oil was reformed by varying the heat treatment temperature, treatment time, and nitrogen flow rate in preparation of precursor pitch for isotropic pitch-based carbon fibers and activated carbon fibers. The reformed pitches were investigated in the yield, softening point, elementary analysis, and molecular weight distribution, and then the precursors reformed were melt spun to certify the optimum reforming conditions. The optimum precursor pitch was prepared when the NCB oil was reformed at $380^{\circ}C$, 3 h and 1.25 vvm $N_2$, and it's the softening point was around $240^{\circ}C$. The reforming resulted in product yield of 21 wt％. The C/H mole ratio of the precursor pitch increased from 1.07 to 1.34, the aromaticity increased from 0.85 to 0.88. The insolubles in benzene and quinoline were 30.0 wt％ and 1.5 wt％, respectively. The spinning temperature was about $50^{\circ}C$ higher than the softening point. The molecular weights of the precursor components were distributed from 250 to 1250, and 80％ of them were in the range of 250 to 700.

• Fibers and Polymers
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• v.2 no.4
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• pp.178-183
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• 2001

A pitch precursor for a general purpose carbon fiber was prepared by condensation of pyrolized fuel oil (petroleum residual oil) with bromine under nitrogen blowing. such a condensation raised the softening point of the pitch from 4$0^{\circ}C$ to $265^{\circ}$ with a yield of 43%. The pitch precurosr showed an enhanced aromaticity and enlarged molecular size, which led to a reduction in molecular mobility and optical isotropy. The precursor was spun into fibers of $20\mu\textrm{m}$ diameter at a take-up speed of 700m/min. The fiber was stepwise stabilized in air and carbonized in Ar gas to obtain an isotropic carbon fiber. The carbon fiber exhibited tensile strengths of 500-800 ㎫though the fiber was formed via a crude method. The electric conductivity of the carbon fiber was relatively high, 2.2$\times$$10^2$S/cm, sufficient to be used as electrode materials.