• Title/Summary/Keyword: reaction crystallization

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Densification and Crystallization Characteristics of LAS Gels Prepared by the Hydrolysis-Condensation Reaction and the Mixed Colloidal Processing Route (가수분해-축합반응 및 콜로이드 혼합법으로 유도된 LAS gel의 치밀화와 결정화 특성)

  • 김광수;장현명;정창주
    • Journal of the Korean Ceramic Society
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    • v.28 no.11
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    • pp.865-872
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    • 1991
  • LAS (lithium aluminosilicate) sol was synthesized using the hydrolysis-condensation reaction of TEOS, chelated Al(OBus)3 and LiNO3 with H2O in alcohol (ethanol+2-propanol) medium. Lowering Li content by a factor of 1/2 significantly enhanced densification and retarded the crystallization of LAS gel by ~30$0^{\circ}C$. Dense LAS specimen with essentially pore-free microstructure was obtained by sintering the sol-gel derived gel at 80$0^{\circ}C$ for 4 h and annealing at 120$0^{\circ}C$ for 2 h. Similary, a mixed colloidal processing was attempted as a convenient, alternative route for the fabrication of dense LAS sintered body. The $\beta$-spodumene seeding (~0.8 ${\mu}{\textrm}{m}$) in the sol-gel derived LAS modified the sequence of phase transformations and lowered the temperature of crystallization by ~12$0^{\circ}C$. Combining the epitaxial seeding with the sol-gel process, we could lower the crystallization temperature to the sintering temperature range (~80$0^{\circ}C$) and, demonstrate a possibility of making the viscous sintering/crystallization as a continuous as a continuous unit process.

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Feasibility of Powdered MSWI Ash Melted Slag as a Seed Crystal of crystallization reaction for the Removal of Phosphorus from Sewage (하수중 인제거를 위한 정석탈인반응의 정석재로서 소각분말 용융슬래그의 이용 가능성 평가)

  • Kim, Choong Gon;Shin, Hyun Gon;Kim, Seung Won
    • Journal of the Korea Organic Resources Recycling Association
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    • v.21 no.1
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    • pp.69-75
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    • 2013
  • This study is a fundamental research to test the applicability of powdered MSWI(Municipal Solid Waste Incinerator) ash melted slag as a seed Crystal for crystallization reaction. Powdered ash melted slag was melted at $1100^{\circ}C$ and ground to lesser than 0.35mm. According to the result of the tests, calcium, enough for crystallization reaction, was eluted from powdered ash melted slag. Moreover, sample(Phosphorus concentration is under 10 mg/L), more than 90% of Phosphorus can be removed. So we rectify the Phosphorus concentration to 100 mg/L. Alkalinity, being well known that it interferes crystallization reaction, effect was studied for synthetic solution(100 mg/L initial Phosphorus concentration, 50 mg/L calcium, pH 8, 1% powdered ash melted slag dosage). For this result, we know that Phosphorus removal is hindered by alkalinity. In addition, the effect of reaction temperature was performed at the same method. The reaction velocity was increased through raising the reaction temperature.

Effect of Reaction Conditions on Crystals in the Reaction Crystallization of Lanthanum Oxalate (란타늄 옥살레이트 반응성 결정화에서 반응조건에 따른 결정입자 연구)

  • Kim, Hong-Ju;Kim, Woon-Soo;Kim, Woo-Sik
    • Applied Chemistry for Engineering
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    • v.9 no.7
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    • pp.1004-1010
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    • 1998
  • Effects of reaction conditions such as power input and feeding time and feeding mode of reactants on the reaction crystallization of lanthanum oxalate in semi-batch reactor were investigated experimentally. Even though the crystal size distribution of lanthanum oxalate was always monomodal, its mean crystal size was significantly varied with the reaction conditions. As the power input and reactant feeding rate increased, the mean crystal size was reduced and the relative induction time was prolonged. The mean crystal size produced in oxalic acid feeding mode was smaller than that in lanthanum chloride feeding mode, but the trend of the relative induction time with the feeding mode was reverse to that of the mean crystal size. The crystal morphology of lanthanum oxalate, which was produced within the ranges of the reaction conditions in our experiment, was maintained as a needle shape.

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Chain extension effects of para-phenylene diisocyanate on crystallization behavior and biodegradability of poly(lactic acid)/poly(butylene terephthalate) blends (파라-페닐렌 다이이소시아네이트의 사슬 연장이 PLA/PBT 블렌드의 결정화 거동과 생분해성에 미치는 영향)

  • Kim, Myung-Wook;Hong, Sung-Min;Lee, Doo-Jin;Park, Kwang-Seok;Youn, Jae-Ryoun
    • Composites Research
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    • v.22 no.3
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    • pp.18-28
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    • 2009
  • Blends of poly(lactic acid) (PLA) and poly(butylene terephthalate) (PBT) were prepared by reaction extrusion with para-phenylene diisocyanate (PPDI). The crystallization behavior and biodegradability were investigated by using a differential scanning calorimeter (DSC), a wide angle X-ray diffractometer (WAXD), a contact angle goniometer, and a buffer solution containing esterase. The addition of PBT into PLA polymer matrix induced the cold crystallization of PLA phase, and the crystallization rate of PLA phase was significantly accelerated when both PBT and PPDI participated in the reaction with PLA simultaneously. But the chain extension caused by PPDI decreased the crystallinity and hydrophilicity of PLA and PBT phases. The crystallinity and hydrophilicity did not affect the biodegradability of PLA/PBT blends. However, phase separation between PLA and PBT in PLA/PBT blends increased the interfacial area exposed to the hydrolysis of enzyme, resulting in the improved degradability rate of PLA phase. In contrast, the improved interfacial adhesion between PLA and PBT matrices by the reaction with PPDI reduced the area exposed to the enzyme to decrease the degradation rate of PLA phase.

Synthesis of kaolinite by hydrothermal reaction using pseudoboehmite as starting material (Pseudoboehmite를 출발물질로한 kaolinite의 수열 합성)

  • 고태석
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.11 no.1
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    • pp.33-37
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    • 2001
  • Kaolinite was synthesized through th acid treatment of mixture which consisted of psudoboehmite and colloidal silica in hydrothermal reaction at $213^{\circ}C$ under autogeneous vapor pressure. Crystallization process was characterized by X-ray powder diffraction pattern, IR spectra and Hinckley index was calculated. The synthesis in acidic solution promotes the dissolution of the starting materials and leads to crystallization of kaolinite. The rate of crystallization to kaolinite and stacking defect were found to e affected by kind of anion, acidity and starting materials.

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Preparation of $TiO_2-SiO_2$ by Sol-Gel Method and Their Photocatalytic Activities (졸-겔법에 의한 $TiO_2-SiO_2$합성 및 광촉매활성)

  • 류완호;양천희
    • Journal of the Korean Society of Safety
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    • v.14 no.1
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    • pp.101-107
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    • 1999
  • $TiO_2$ and $xTiO_2-ySiO_2$ system photocatalysts were developed by sol-gel method based on the change of production parameters, and their structure of crystallization and the specific surface area was measured. Considering the efficiency of the ethanol decomposition using the catalyst, the conclusion was made as follows: 1) By means of X-ray analysis of $TiO_2$ powder that is obtained from water and Titanium alkoxide with various molar ratios, it is shown that structure of crystallization is a dominating structure and, on the other hand, the crystallization of rutile also partly exists. The specific surface area is at its maximum value at R=6, which is the molar ratio of water vs. alkoxide, whereas its value goes down as the molar ratio increases. In the reaction of using $TiO_2$ catalyst, the ethanol is decomposed into the extent of 15 ~30% in an hour and three hours are necessitated for 70% decomposition. 2) $TiO_2/SiO_2$ powder is developed from Titanium and Silicon alkoxide by a hetero-condensation process. The increase of SiO$_2$ contents causes the decrease of the degree of crystallization of the gel, whereas the specific surface area preferentially increases. In the decomposition reaction of the ethanol, the decomposition efficiency represents 25~60% in an hour. It is, however, examined that the efficiency inactively increases corresponding to the duration of reaction time. It is shown that more than 90% of ethanol is decomposed when reaction time is about three hours and the efficiency illustrates the maximum value for 60-$TiO_2/4O-SiO_2$ catalyst.

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Crystallization of Poly(vinylidene fluoride)-SiO2 Hybrid Composites Prepared by a Sol-gel Process

  • Cho, Jae Whan;Sul, Kyun Il
    • Fibers and Polymers
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    • v.2 no.3
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    • pp.135-140
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    • 2001
  • Organic-inorganic hybrid composites consisting of poly(vinylidene fluoride) (PVDF) and SiO$_2$ were prepared through a sol-gel process and the crystallization behavior of PVDF in the presence of $SiO_2$ networks was investigated by spectroscopic, thermal and x-ray diffraction measurements. The hybrid composites obtained were relatively transparent, and brittleness increased with increasing content of tetraethoxysilane (TEOS). It was regarded from FT-lR and DSC thermal analyses that at least a certain interaction existed between PVDF molecules and the $SiO_2$ networks. X-ray diffraction measurements showed that all of the hybrid samples had a crystal structure of PVDF ${\gamma}$-phase. Fresh gel prepared from the sol-gel reaction showed a very weak x-ray diffraction peak near 2$\theta$=$21^{\circ}$ due to PVDF crystallization, and Intensity increased grade-ally with time after gelation. The crystallization behavior of PVDF was strongly affected by the amount of $SiO_2$ networks. That is, $SiO_2$ content directly influenced preference and disturbance fur crystallization. In polymer-rich hybrids, $SiO_2$ networks had a favorable effect on the extent of PVDF crystallization. In particular, the maximum portent crystallinity of PVDF occurred at the content of 3.7 wt% $SiO_2$ and was higher than that of pure PVDF. However. beyond about 10 wt% $SiO_2$, the crystallization of PVDF was strongly confined.

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Preparation of Ferroelectric PZT Thin Film by Sol-Gel Processing; (II) Effect of Catalysts on Densification and Crystallization (솔-젤법에 의한 강유전성 PZT 박막의 제조;(II) 치밀화 및 결정화에 미치는 촉매의 영향)

  • 김병호;박성호;김병호
    • Journal of the Korean Ceramic Society
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    • v.32 no.7
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    • pp.783-792
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    • 1995
  • Sol-Gel derived ferroelectric PZT thin films were fabricated on ITO/Glass and Si/SiO2 substrates. In order to investigate the effect of catalysts on the densification and crystallization of PZT thin films, a nitric acid or ammonium hydroxide was added to the PZT stock solution at the state of partial hydrolysis reaction. The measured pH for a stable PZT sol was 5.2~9.3. In case of an acid-catalyzed PZT sol, a highly condensed particulate PZT sol was formed by accelerating the hydrolysis reaction. But weakly branched polymeric PZT sol was formed with a base-catalyzed condition. The difference in densification behavior was not found in the pH range of added catalyst, but the refractive index of PZT thin film was increased rapidly as the annealing temperature increased. The PZT thin film annealed at 54$0^{\circ}C$ for 10 min was fully densified and its refractive index was above 2.4. When the annealing temperature increased, the transition from the pyrochlore phase to perovskite appeared at 54$0^{\circ}C$. The base-catalyzed PZT thin film suppressed to form the pyrochlore phase and proceeded effectively to convert the perovskite phase. This was due to the formation of polymeric molecular structure by controlling the hydrolysis and condensation reaction through the additiion of the ammonium hydroxide.

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Study on the reaction crystallization of silver chloride in Rushton type semi-batch reactor (Rushton type 반회분식 반응기에서 염화은 반응성 결정화에 관한 연구)

  • 이종석;김우식
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.6 no.4
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    • pp.609-619
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    • 1996
  • Experimental study on effects of factors on the reaction crystallization of silver chloride in rushton type reactor. The size and size distributions of the silver chloride crystals were observed to be markedly affected by the agitation speed of solution, and feeding rate, feeding mode and concentration of reactants. From experimental data it was inferred that in the reaction crystallization of silver chloride the supersaturation level of silver chloride and concentration of excess ions in the solution, and mass transfer rate around the crystals were implicitly interrelated with factors and directly affected on the crystal nucleation and grwoth processes. However, the morphology of the silver chloride crystal was not changed by factors.

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Effect of Ionic Liquid on Increased Surface Area Crystallization Process for Vancomycin (표면적이 증가된 반코마이신 결정화 공정에서 이온성 액체의 영향)

  • Kim, Sung-Jae;Kim, Jin-Hyun
    • Microbiology and Biotechnology Letters
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    • v.42 no.3
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    • pp.297-301
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    • 2014
  • We examined the effect of ionic liquid on the crystallization efficiency of vancomycin in an increased surface area crystallization with silica gel. The crystallization efficiency was improved by the addition of ionic liquid, [BMIm][$BF_4$]. The addition of ionic liquid (20%, v/v) on the increased surface area crystallization with silica gel dramatically reduced the crystallization time by 6 folds (4 h), compared with the results of the case where the surface area-increasing material and ionic liquid had not been added. In addition, the crystal size of vancomycin was decreased and the crystal quality of vancomycin was improved by increasing the addition of ionic liquid.