• Title/Summary/Keyword: Residual solvents

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Synthesis and Characterization of Chelated Polymers of Polyhydrazones (폴리히드라존계 킬레이트 고분자의 합성과 특성)

  • Kong Soo Kim;Yong Woo Lee;Doo Hee Lee
    • Journal of the Korean Chemical Society
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    • v.29 no.5
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    • pp.543-551
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    • 1985
  • A new class of polyhydrazones has been synthesized by the solution polycondensation from equimolecular amounts of aromatic dialdehydes such as para, meta, ortho-phthal aldehyde, 5,5'-methylene-bis-salicyl aldehyde (PPTA, MPTA, OPTA, MBSA) and dihydrazides, 5,5'-methylene-bis-salicylic dihydrazide (MBSDH), terephthalic dihydrazide (TDH), sebacic dihydrazide (SDH) in DMF-$CH_3COOH$ solution. The solubility characteristics, spectral, and thermal properties of the synthesized polyhydrazones and their metal chelates were also studied. These polyhydrazones and their metal chelates except the polyhydrazone prepared from OPTA-MBSDH were generally insoluble in common organic solvents. The thermogravimetric analysis of polyhydrazones showed 10% weight losses at 250∼350$^{\circ}$C and residual weight at 500$^{\circ}$C were 32.5∼62.5%. The decomposition temperature of higher relatively, and the metal chelates decrease in the following orders; Zn(II)-IIa > Ni(II)-IIa > Co(II)-IIa > Cu(II)-IIa.

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Filling and Wiping Properties of Silver Nano Paste in Trench Layer of Metal Mesh Type Transparent Conducting Electrode Films for Touch Screen Panel Application (실버 나노분말을 이용한 메탈메쉬용 페이스트의 충전 및 와이핑 특성)

  • Kim, Gi-Dong;Nam, Hyun-Min;Yang, Sangsun;Park, Lee-Soon;Nam, Su-Yong
    • Journal of Powder Materials
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    • v.24 no.6
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    • pp.464-471
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    • 2017
  • A metal mesh TCE film is fabricated using a series of processes such as UV imprinting of a transparent trench pattern (with a width of $2-5{\mu}m$) onto a PET film, filling it with silver paste, wiping of the surface, and heat-curing the silver paste. In this work nanosized (40-50 nm) silver particles are synthesized and mixed with submicron (250-300 nm)-sized silver particles to prepare silver paste for the fabrication of metal mesh-type TCE films. The filling of these silver pastes into the patterned trench layer is examined using a specially designed filling machine and the rheological testing of the silver pastes. The wiping of the trench layer surface to remove any residual silver paste or particles is tested with various mixture solvents, and ethyl cellosolve acetate (ECA):DI water = 90:10 wt% is found to give the best result. The silver paste with 40-50 nm Ag:250-300 nm Ag in a 10:90 wt% mixture gives the highest electrical conductance. The metal mesh TCE film obtained with this silver paste in an optimized process exhibits a light transmittance of 90.4% and haze at 1.2%, which is suitable for TSP application.

Cloning, Expression, and Characterization of a Cold-Active and Organic Solvent-Tolerant Lipase from Aeromicrobium sp. SCSIO 25071

  • Su, Hongfei;Mai, Zhimao;Yang, Jian;Xiao, Yunzhu;Tian, Xinpeng;Zhang, Si
    • Journal of Microbiology and Biotechnology
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    • v.26 no.6
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    • pp.1067-1076
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    • 2016
  • The gene encoding lipase (Lip98) from Aeromicrobium sp. SCSIO 25071 was cloned and functionally expressed in Escherichia coli. Lip98 amino acid sequence shares the highest (49%) identity to Rhodococcus jostii RHA1 lipase and contains a novel motif (GHSEG), which is different from other clusters in the lipase superfamily. The recombinant lipase was purified to homogeneity with Ni-NTA affinity chromatography. Lip98 showed an apparent molecular mass of 30 kDa on SDS gel. The optimal temperature and pH value for enzymatic activity were recorded at 30℃ and 7.5, respectively. Lip98 exhibited high activity at low temperatures with 35% maximum activity at 0℃ and good stability at temperatures below 35℃. Its calculated activation energy was 4.12 kcal/mol at the low temperature range of 15-30℃. Its activity was slightly affected by some metal ions such as K+, Ca2+, and Na+. The activity of Lip98 was increased by various organic solvents such as DMSO, ethanol, acetone, and hexane with the concentration of 30% (v/v) and retained more than 30% residual activity in neat organic solvent. The unique characteristics of Lip98 imply that it is a promising candidate for industrial application as a nonaqueous biocatalyst and food additive.

A Study on Development of Alternative Non-aqueous Cleaning Agents to Ozone Depletion Substances and its Field Application (오존파괴물질 대체 비수계세정제 개발 및 현장 적용 연구)

  • Park, Yong-Bae;Bae, Jae-Heum;Lee, Min-Jae;Lee, Jong-Gi;Lee, Ho-Yeoul;Bae, Soo-Jung;Lee, Dong-Kee
    • Clean Technology
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    • v.17 no.4
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    • pp.306-313
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    • 2011
  • Flux or solder is used in soldering process for manufacturing electronic parts such as printed circuit boards (PCB). After soldering process, residual flux and solder paste on the parts should be removed since their residuals could cause performance degradation or failure of parts due to their corrosion and electric leakage. Ozone depletion substances such as 1,1,1- trichloroethane (TCE) and HCFC-141b have widely been using for removal of residual flux and solder paste after soldering process In manufacturing of electronic parts until now. In this study, non-aqueous cleaning agents without flash point were developed and applied to industrial field for replacement of cleaning agents with ozone depletion. In order to develop non-aqueous cleaning agents without ethers, esters, fluoride- type solvents. And their physical properties and cleaning abilities were evaluated, and they were applied to industrial fields for cleaning of flux and solder on the PCB. And vacuum distillation apparatus were operated to determine their operating conditions and recycling yields for recycling of used cleaning agents formulated in this study. As a result of physical properties measurement of our formulated cleaning agents, they were expected to have good wetting and penetrating power since their surface tensions were relatively low as 18.0~20.4 dyne/$cm^2$ and their wetting indices are relatively large. And some cleaning agents holding fluoride-type solvents as their components did not have any flash point and they seemed to be safe in their handling and storage. The cleaning experimental results showed that some cleaning agents were better in their cleaning of flux and solder paste than 1,1,1-TCE and HCFC-141b. And industrial application results of the formulated cleaning agents for cleaning PCB indicated that they can be applicable to industry due to their good cleaning capability in comparison with HCFC-141b. The recycling experiments of the used formulated cleaning agents through a vacuum distillation apparatus also showed that their 91.9~97.5% could be recycled with its proper operating conditions.

A Study on the Extraction of Monasil PCA using Liquid CO2 (액체 이산화탄소 이용한 Monasil PCA 추출에 대한 연구)

  • Cho, Dong Woo;Oh, Kyoung Shil;Bae, Won;Kim, Hwayong;Lee, Kab-Soo
    • Korean Chemical Engineering Research
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    • v.50 no.4
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    • pp.684-689
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    • 2012
  • Poly(acrylic acid) (PAA) microspheres is one of the widely-used polymeric materials for the bio-field application and the electric materials. For the synthesis of PAA microspheres, the polymerization technique using surfactants is applied. After the synthesis, the purification and separation processes are required for the removal of surfactant. When general organic solvents were used, many problems, such as huge amount of waste solvent, additional separation processes, and the possibility of residual media, were occurred. Thus, High-pressure Soxhlet extraction using liquid $CO_2$ was developed to solve these problems. In this study, High-pressure Soxhlet extraction of the synthesized PAA microspheres using liquid $CO_2$ was conducted for the removal of Monasil PCA which is used for the dispersion polymerization of acrylic acid in compressed liquid Dimethyl ether (DME). The morphology of the extracted PAA particles was checked by field emission scanning electron microscopy (FE-SEM) and the residual concentration of Monasil PCA was analyzed by inductively coupled plasma - Optical Emission Spectrometer (ICP-OES). For studying the effect of the solvent effect, Soxhlet extraction was conducted using n-hexane, liquid DME, and liquid $CO_2$. In case of n-hexane, some extracted PAA microspheres were produced. However, deformation was also occurred due to the high thermal energy of n-hexane vapor. Liquid DME could not remove Monasil PCA. When using liquid $CO_2$, the extracted PAA microspheres which were free for the residual solvent were produced without deformation. For finding the optimum operating condition, high-pressure Soxhlet extraction was conducted for 8 hours with changing the temperature of reboiler and condenser. When the extractor temperature is $19.6{\pm}0.2^{\circ}C$ and the pressure is $51.5{\pm}0.5$ bar, the best removal efficiency was obtained.

Study on Long-Term Preservation of Hwangnyunhaedok-Tang Pharmacopuncture (황련해독탕 약침의 장기보존시험에 관한 연구)

  • Lee, Jin-Ho;Ha, In-Hyuk;Kim, Me-Riong;Chung, Hwa-Jin;Lee, Jae-Woong;Kim, Min-Jeong;Kim, Eun-Jee;Lee, In-Hee
    • Journal of Korean Medicine Rehabilitation
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    • v.26 no.2
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    • pp.51-59
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    • 2016
  • Objectives We studied long-term preservation in stability of a mixed preparation of distilled and 70% alcohol extracted Hwangnyunhaedok-tang pharmacopuncture to establish standards for expiration date and quality control. Methods Three lots of consecutively prepared Hwangnyunhaedok-tang pharmacopuncture were each tested in triplicate to a total 5 tests at 3 month intervals over a period of 12 months for analysis of appearance, pH, specific gravity, index component content, endotoxins, microbial sterility, residual organic solvents, heavy metals, and pesticides. Items with no difference by elapsed time were tested at the initial and final timepoints, and data of items with potential difference by elapsed time were analyzed for trends to establish individual quality control standards. Results All tested items were stable over the study period, and therefore the expiration date was set as 12 months. pH quality control standards were set as 3.66~5.69, and that of specific gravity as 0.802~1.203, respectively. In index component content standards, berberine was set at $4.96{\sim}8.98{\mu}g/vial$, baicalin at $6.47{\sim}10.31{\mu}g/vial$, and geniposide at $116.03{\sim}189.55{\mu}g/vial$, respectively. Standards for other items with no difference by elapsed time were set according to general Korean herbal medicine standards in the Korean Pharmacopoeia. Conclusions Manageable expiration date and quality control standards were established through long-term preservation testing of Hwangnyunhaedok-tang pharmacopuncture, furthering standardization of Korean medicine pharmacopuncture.

Evaluation of Stability in the Purified Wood Vinegar and Its Hair Growth Effect (목초액의 안정성 및 모발 성장 촉진 효과)

  • Cho, Young-Ho;Lee, Ju-Yeon;Lee, Jong-Hwa;Cho, Jae-Su;Lee, Gye-Won
    • Journal of Life Science
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    • v.19 no.10
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    • pp.1389-1395
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    • 2009
  • Generally, it takes a long time to purify wood vinegar, and it contains toxic compounds such as tar, methanol, phenol and benzopyrene. To reduce the toxicity of wood vinegar itself, we have developed a new purification method of wood vinegar using an oxidation-cohesion reaction and distillation with an active carbon. We have investigated the physico-chemical change (pH, specific gravity, refractive index and dissolved tar), the change of amount of toxic compounds (carbonyl group, phenol, benzopyrene and residual solvents) and organic acids (formic acid (FA), acetic acid (AA), propionic acid (PA)) of the purified wood vinegar under the long term and accelerated storage conditions. Also, we have evaluated the effect of the purified wood vinegar on hair growth using an alopecia model of C57BL/6 mice. As a result, we could find out that the purified wood vinegar was stable and remained without decay under the storage conditions and benzopyrene, a carcinogenic agent, was not detected in the purified wood vinegar. After topical treatment of the purified wood vinegar solution or minoxidil (MXD) for 2 weeks to dorsal skin, the hair regrowth of the mice accelerated faster than that of the control, with no clinical signs. In conclusion, we could suggest a guideline for quality control of process to reduce the toxic compounds in wood vinegar and it might be a useful hair growth promoter in the treatment of baldness or alopecia.

The effect of solvent evaporation of dentin adhesive on bonding efficacy (상아질 접착제의 용매 증발이 접착 효율에 미치는 영향)

  • Cho, Min-Woo;Kim, Ji-Yeon;Kim, Duck-Su;Choi, Kyoung-Kyu
    • Restorative Dentistry and Endodontics
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    • v.35 no.5
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    • pp.321-334
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    • 2010
  • Objectives: The purpose of this study is to evaluate bonding efficacy by means of measuring the effect of remained solvent on Degree of conversion(DC) and ${\mu}TBS$ and FE-SEM examination. Materials and Methods: Two 2-step total etching adhesives and two single-step self etching adhesives were used in this study. First, volume weight loss of 4 dentin adhesives were measured using weighting machine in process of time in normal conditions and calculate degree of evaporation (DE). Reaction/reference intensity ratio were measured using micro-Raman spectroscopy and calculate DC according to DE. Then 2 experimental groups were prepared according to air-drying methods (under, over) and control group was prepared to manufacturer's instruction. Total 12 groups were evaluated by means of micro tensile bond strength and FE-SEM examination. Results: Degree of evaporation (DE) was increased as time elapsed but different features were observed according to the kind of solvents. Acetone based adhesive showed higher DE than ethanol and butanol based adhesive. Degree of conversion (DC) was increased according to DE except for $S^3$ bond. In ${\mu}TBS$ evaluation, bond strength was increased by additional air-drying. Large gaps and droplets were observed in acetone based adhesives by FE-SEM pictures. Conclusions: Additional air-drying is recommended for single-step self etching adhesive but careful consideration is required for 2-step total etching adhesive because of oxygen inhibition layer. Evaporation method is carefully chose and applied according to the solvent type.

Quantitative Determination of Marker Compounds in the Extracts of Camellia sinensis L. Sub-branches (Residual Products) by HPLC (HPLC에 의한 차나무 잔가지(부산물)의 추출물 내 지표 성분의 정량분석)

  • Lee, Min Sung;Im, Hyeon Jeong;Jeong, Hea Seok;Cho, Hae Jin;Woo, Hyun Sim;Oh, Yu Jin;Lee, Soo In;Kim, Hyun Chul;Ahn, Kyung Wan;Kim, Yeong Su;Kim, Dae Wook
    • Korean Journal of Medicinal Crop Science
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    • v.27 no.1
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    • pp.24-29
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    • 2019
  • Background: Camellia sinensis L.(CS) is a perennial evergreen species of plant whose leaves are used to produce tea. In this plant species, the parts used are the leaves, sub-branch parts are thrown out. Methods and Results: Ethanol extract of sub-branch parts was used for isolation of major compounds by column chromatography. Structures were identified as caffeine (1), (-)-epicatechin (2) and (-)-epicatechin gallate (3) by interpretation of spectroscopic analysis, including $^1H$- and $^{13}C$-NMR. High-performance liquid chromatography (HPLC) method was used to compare the quantitative level of marker compounds in various extraction solvents of sub-branch parts of CS. The content of caffeine, (-)-epicatechin, and (-)-epicatechin gallate in 30% ethanol extract showed higher value with $3.28{\pm}0.57mg/g$, $5.53{\pm}0.88mg/g$, and $1.29{\pm}0.24mg/g$, respectively. Conclusions: These results indicated that not only leaves parts but also sub-branch, could be a good source for the functional material and pharmaceutical industry.

A Study on the Preparation and Purification Characteristics of Graphene Oxide by Graphite Type (흑연 종류에 따른 산화 그래핀의 제조 및 정제를 통한 특성연구)

  • Jeong, Kyeom;Kim, Young-Ho
    • Clean Technology
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    • v.27 no.2
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    • pp.132-138
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    • 2021
  • Research is being conducted on graphene to provide graphene having both excellent physical as well as electrical properties in addition to unique physical properties. In this study, Hummer's method, which is a representative method for chemical exfoliation, was applied in order to investigate the possibility of the mass production of high-quality graphene oxide. Three types of graphite (graphite, crystalline graphite, and expanded graphite) were used in the preparation of graphene oxide with variations in the amount of potassium permanganate added, reaction temperature, and reaction time. Then a Fourier transform infrared spectroscopy (FT-IR), a Raman spectrometer, and a transmission electron microscope (TEM) were used to measure the quality of the prepared graphene oxide. Of the three types of graphite used in this experiment, crystalline graphite showed the highest quality. The prepared graphene oxide was then purified with an organic solvent, and an analysis conducted using energy dispersive X-ray spectroscopy (EDS). From the results of the residual values, we were able to confirm that both acid wastewater and wastewater were best purified using cyclohexane. The method for manufacturing graphene oxide as well as the method of purification using organic solvents that are presented in this study are expected to have less of an environmental impact, making them environmentally friendly. This makes them suitable for use in various industrial fields such as the film industry and for heat dissipation and as coating agents.